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Enhancement of docosahexaenoic acid production by

ORIGIN AL ARTI CLEEnhancement of docosahexaenoic acid production by Schizochytrium ing a two-stage oxygen supply control strategy based on oxygen transfer coefﬁcientL.Qu,X.-J.Ji,L.-J.Ren,Z.-K.Nie,Y.Feng,W.-J.Wu,P.-K.Ouyang and H.HuangState Key Laboratory of Materials-Oriented Chemical Engineering,College of Biotechnology and Pharmaceutical Engineering,Nanjing University of Technology,Nanjing,ChinaIntroductionDocosahexaenoic acid[DHA;22:6(n-3)]is a long-chain polyunsaturated fatty acid(PUFA)which belongs to the omega-3group.In recent years,DHA has attracted much attention because of its beneﬁts to human health includ-ing both infants and adults(Lauritzen et al.2001;Nordoy et al.2001;Ratledge2004;Sijtsma and de Swaaf2004). Microbial oils(single cell oils)are currently being devel-oped because they have many superiorities:possibility to obtain oils with high and speciﬁc PUFAs content,with higher oxidative stability,production from sustainable raw materials,lower puriﬁcation costs,the disappearance of environmental man-made pollutants and a more constant product quality is possible(Ratledge2004;Sijtsma and de Swaaf2004).Strains from the marine protists Traustochy-trid and dinoﬂagellate Crypthecodinium cohnii have tradi-tionally been considered to have the most potential in a commercial setting,especially the former,which belongs to the genus Thraustochytrium and Schizochytrium(Chi et al.2007).Schizochytrium sp.possesses a PUFA synthase complex which has an O2-independent,polyketide syn-thase-like mode of action(Jakobsen et al.2008). Jakobsen et al.(2008)found that the lipid content of Aurantiochytrium sp.T66,which was also a genus of Schizochytrium,could be increased under oxygen limita-tion condition.A two-stage growth of Schizochytrium limacinum SR21with shifting dissolved oxygen level in shakeﬂask scale was also investigated and DHA content increased from3Æ65to6Æ56g l)1(Chi et al.2009).These studies used dissolved oxygen to show the oxygen supply during fermentation process,which could not be easily used for scale-up process.The two-stage growth in Chi’s study was not carried out as a constant process,so this method needs further investigation before its application in large-scale process.Keywordsdocosahexaenoic acid,oxygen transfer, Schizochytrium sp.,two-stage strategy.CorrespondenceHe Huang,State Key Laboratory of Materials-Oriented Chemical Engineering,College of Biotechnology and Pharmaceutical Engineering,Nanjing University of Technology,No.5Xinmofan Road,Nanjing 210009,China.E-mail:biotech@2010⁄1112:received29June2010,revised 17October2010and accepted18October 2010doi:10.1111/j.1472-765X.2010.02960.x AbstractAims:To improve the yield and productivity of docosahexaenoic acid(DHA) by Schizochytrium sp.in terms of the analysis of microbial physiology. Methods and Results:A two-stage oxygen supply control strategy,aimed at achieving high concentration and high productivity of DHA,was proposed.At theﬁrst40h,K L a was controlled at150Æ1h)1to obtain high l for cell growth, subsequently K L a was controlled at88Æ5h)1to maintain high q p for high DHA accumulation.Finally,the maximum lipid,DHA content and DHA productiv-ity reached46Æ6,17Æ7g l)1and111mg l)1h)1,which were43Æ83%,63Æ88% and32Æ14%over the best results controlled by constant K L a.Conclusions:This paper described a two-stage oxygen supply control strategy based on the kinetic analysis for efﬁcient DHA fermentation by Schizo-chytrium sp.Signiﬁcance and Impact of the study:This study showed the advantage of two-stage control strategy in terms of microbial physiology.As K L a is a scaling-up parameter,the idea developed in this paper could be scaled-up to industrial process and applied to other industrial biotechnological processes to achieve both high product concentration and high productivity.Letters in Applied Microbiology ISSN0266-8254In our previous study(Ren et al.2010),a stepwise aer-ation control strategy was developed for efﬁcient DHA production in a1,500-l bioreactor using fed-batch fer-mentation.However,this work only studied the effect of aeration condition,and the agitation condition,which also affects the oxygen supply greatly,was not discussed. In the present study,the effect of different oxygen supply conditions,as measured by the volumetric oxygen mass transfer coefﬁcient(K L a),which was a scaling-up parame-ter,was investigated in a50-l bioreactor using fed-batch fermentation.Subsequently,a two-stage oxygen supply control strategy was designed based on the kinetic analysis of fed-batch processes controlled by single oxygen supply and was conﬁrmed experimentally.Materials and methodsMicro-organismSchizochytrium sp.HX–308(CCTCC M209059),which was isolated from seawater in our previous work and stored in China Center for Type Culture Collection (CCTCC)(Huang et al.2009),was used in the present study.This strain was preserved in20%(v⁄v)glycerol at )80°C.Culture conditionsThe seed culture medium and the conditions were as indi-cated in our previous study(Ren et al.2009).The culture preserved in the glycerine tube was inoculated into a250-mlﬂask with50ml medium and cultivated for24h.After three generation cultivation,the preculture was inoculated into a10-l seed fermentor with an inoculum size of1% (v⁄v)and cultivated for24h,and the seed culture(20%, v⁄v)was then transferred to a50-l fermentor with a work-ing volume of35l.The bioreactor was equipped with three impellers and a frit sparger with an average pore diameter of40l m.Dissolved oxygen concentration of cultures was measured using a polarographic electrode and was expressed as percentage of O2saturation.The oxygen transfer rate was studied as the volumetric oxygen mass transfer coefﬁcient(K L a).The agitation and aeration rates wereﬁrst set at different values,characterizing differ-ent oxygen transfer conditions:27Æ3h)1(100rev min)1, 1vvm),88Æ5h)1(200rev min)1,1vvm)and150Æ1h)1 (250rev min)1,1Æ4vvm).During the fermentation pro-cess,in addition to adding glucose at the initial fermenta-tion stage,intermittent glucose feeding was also supplied to keep its concentration above15g l)1.The fed-batch fermentation was performed at25°C until the glucose concentration did not change.The bioreactor had agita-tion and temperature controlled by a computer system,while pH was not controlled in this study.All fermenta-tions were inoculated with the same culture.Analytical methodsTen millilitres broth was used to determine cell dry weight by gravimetric method.The methods of lipid extraction and fatty acid methyl esters(FAMEs)prepara-tion were according to our previous study(Ren et al. 2009).The measurements of individual FAMEs,glucose, glutamate and pH used the same method as our previous study(Ren et al.2010).Calculation of kinetic parametersThe speciﬁc cell growth rate(l,h)1),speciﬁc glucose consumption rate(q s,h)1)and speciﬁc lipid accumula-tion rate(q p,h)1)were estimated from experimental data of cell growth(x,g l)1),residual glucose concentration(s, g l)1)and lipid accumulation(p,g l)1)according to the method mentioned in our previous study(Ji et al.2009). The measurement of oxygen transfer coefﬁcients,K L a,in bioreactorThe sulﬁte method(Na2SO3method)is proposed for the measurement of oxygen transfer coefﬁcients,K L a,in bior-eactors(Puskeiler and Weuster-Botz2005).ResultsEffect of different K L a on DHA fermentationEffects of different K L a(27Æ3,88Æ5and150Æ1h)1)on DHA fermentation were investigated,respectively.The results indicated that K L a played a vital role in lipid and DHA production.As shown in Fig.1,the relative high ﬁnal lipid and DHA concentration up to32Æ4and 10Æ8g l)1were obtained at the K L a of88Æ5h)1.While when the K L a was higher or lower,theﬁnal lipid and DHA concentration decreased(21Æ8and8Æ5g l)1at 27Æ3h)1,24Æ8and8Æ25g l)1at150Æ1h)1).This indicated that either lower K L a(27Æ3h)1)or higher K L a(150Æ1h)1) was not beneﬁcial for lipid and DHA accumulation. However,although theﬁnal DHA concentration at the K L a of88Æ5h)1was higher compared with the K L a of 150Æ1h)1,the former DHA productivity was lower than the latter(75mg l)1h)1at88Æ5h)1,84mg l)1h)1at 150Æ1h)1).The above-mentioned observations indicated that the K L a for obtaining high concentration and high yield of DHA was not suitable for ensuring high DHA productivity.It can therefore be concluded that high con-centration,high yield and high productivity of DHAL.Qu et al.Enhancement of docosahexaenoic acid productioncould not be achieved simultaneously by controlling a constant K L a throughout the whole culture process. Kinetic analysis of DHA fermentation at different K L a To analyse the kinetic characteristics of the above-mentioned processes at different K L a,three kinetic parameters,including l,q s and q p,were calculated based on the data of Fig.1.As shown in Fig.2,compared with the K L a of88Æ5h)1,l and q s were higher at the K L a of 150Æ1h)1at the early stage of DHA fermentation(before 40h).It showed that the K L a of150Æ1h)1was better for cell growth and glucose consumption during theﬁrst 40h.But after40h,the K L a of88Æ5h)1was beneﬁcial for DHA accumulation with a high value of q bin-ing this result with that obtained in the experiments of constant K L a fermentation,it could be concluded that the lower K L a was beneﬁcial for high DHA accumulation in the later stage of cultivation.Based on the analysis of l, q s and q p,a two-stage oxygen supply control strategy based on oxygen transfer coefﬁcient was therefore pro-posed.In this strategy,the K L a was controlled at 150Æ1h)1in theﬁrst40h to maintain high l and q s for fast cell growth and glucose consumption and then switched to88Æ5h)1after40h to maintain high q p for high DHA production.DHA production with two-stage oxygen control strategy Time course of two-stage oxygen supply control strategy for DHA fermentation was shown in Fig.3.Table1listed the results of constant and two-stage oxygen supply con-trolling experiments.It was observed that by using the two-stage oxygen supply control strategy,the maximum concentration of lipid and DHA reached46Æ6and 17Æ7g l)1with the productivity of111mg l)1h)1.The results were both higher than that of constant K L a pro-cesses(10Æ8g l)1of DHA concentration at the K L a of 88Æ5h)1and85mg l)1h)1of DHA productivity at the K L a of150Æ1h)1).It can be concluded that this two-stage oxygen supply control strategy could not only consider-ably improve lipid and DHA concentration but also increase DHA productivity.The proposed two-stage oxy-gen supply control strategy was therefore proved to be effective for efﬁcient DHA production.Enhancement of docosahexaenoic acid production L.Qu et al.DiscussionIn this paper,the uniﬁcation of relatively high concentra-tion and high productivity of DHA was achieved by applying a two-stage oxygen supply control strategy,com-bining the advantages of high DHA concentration under lower K L a and high DHA productivity under higher K L a. Theﬁnal concentration and productivity of DHA reached 17Æ7g l)1and111mg l)1h)1,respectively,which approaches the highest published value of134mg l)1h)1 by Schizochytrium sp.SR21(Yaguchi et al.1997), 115mg l)1h)1for Schizochytrium mangrovei Sk-02(Una-gul et al.2006),and117mg l)1h)1for strain12B,(Perveen et al.2006)and much higher than93mg l)1h)1by using Aurantiochytrium sp.T66(Jakobsen et al.2008).A two-stage growth of Schizochytrium limacinum SR21 with shifting dissolved oxygen level in shakeﬂask scale was studied in the previous work(Chi et al.2009).In our previous study(Ren et al.2010),a stepwise aeration con-trol strategy was developed for efﬁcient DHA production in a1,500-l bioreactor using fed-batch fermentation.In this study,we investigated the characteristics of DHA fermentation under different oxygen supply conditions, and it was interesting toﬁnd that signiﬁcant differences occurred in l,q s and q p in fed-batch fermentation experi-ments using Schizochytrium sp.HX-308under different K L a conditions.And a proper oxygen supply method using a two-stage oxygen supply control strategy was therefore developed from a kinetic stand point.Finally, 43Æ83,63Æ89and32Æ14%improvements in lipid concen-tration,DHA concentration and productivity of DHA over the best results controlled by constant K L a were observed under this two-stage oxygen supply control strategy.And this might be attributed by the following reasons.The two-stage growth is common in oleaginous micro-organisms.Theﬁrst stage can be considered as a cell growth stage in which cell density increased rapidly,while the cell accumulated a low content of lipids.The second stage can be considered as a product accumulation stage in which cell number increased little,but lipid content in the cell,cell body weight and cell size was all increased, leading to a high biomass concentration(Chi et al.2009). In terms of oxygen demand in the fermentation process, a high oxygen consumption rate is preferred for theﬁrst stage,because cell growth requires a large amount of pri-mary metabolites such as enzymes,nucleic acids and other proteins.In this study,kinetic analysis of DHA fer-mentation at different K L a values showed that the K L a of 150Æ1h)1was better for cell growth and glucose con-sumption during theﬁrst40h.This might be caused by the fact that in theﬁrst40h during the fermentation,the relatively high K L a led to a relatively high dissolved oxy-gen concentration(Fig.4),so in this two-stage fermenta-tion process,high oxygen supply in theﬁrst stageTable1Comparison of parameters infed-batch production of docosahexaenoic acid(DHA)by Schizochytrium sp.HX-308at differ-ent oxygen supply control strategies Parameters K L a(h)1)Increment(%)* 27Æ388Æ5150Æ1150Æ1(0–40h),88Æ5(after40h)Cell dry weight(g l)1)72Æ0273Æ1074Æ0292Æ7225Æ3Total lipids(g l)1)21Æ832Æ424Æ846Æ643Æ83DHA content(g l)1)8Æ510Æ88Æ2517Æ763Æ88DHA productivity(mg l)1h)1)42Æ5758411132Æ14Total lipids content in celldry weight(%)30Æ2744Æ3233Æ5050Æ2613Æ4Fermentation time(h) 20014498160–DHA⁄TFA(%)48Æ3942Æ7035Æ7841Æ96–TFA,total fatty acids.*Compared with the best result controlled by constant K L a.Fermentation time was deﬁned as the time when the glucose concentration did not change. L.Qu et al.Enhancement of docosahexaenoic acid productionbrought about faster cell growth and glucose consump-tion,which is favourable for high cell density considered as theﬁrst concern for high production of intracellular products.Furthermore,in the lipids’accumulation stage,how-ever,low oxygen supply is more favourable.Chi et al. (2009)found that high dissolved oxygen concentration set at50%level during the later phase of fermentation proved to have an adverse effect on lipid production, because cell size remained small and no improvement in dry cell weight was noted.Bailey et al.(2003)showed a similar result in their study,in which a high dissolved oxygen level of40%produced18Æ2%lipids in the bio-mass,but low dissolved oxygen at5%produced24Æ4%. Both of these results prove that lower oxygen is more beneﬁcial for lipids production in Schizochytrium sp.Our study showed the similar results,lipid and DHA concen-tration up to32Æ4and10Æ8g l)1were obtained at the K L a of88Æ5h)1while when the K L a was higher,theﬁnal lipid concentration and DHA concentration decreased to24Æ8 and8Æ25g l)1at the K L a of150Æ1h)1.These results may be explained by two facts:First,high oxygen supply in the lipid accumulation stage may lead to more carbon source used for cell respiration and energy metabolism rather than lipid synthesis.Therefore,the decrease in oxy-gen supply in the lipid accumulation stage could promote the carbon source utilization efﬁciency and increase the lipid accumulation.In addition,Schizochytrium species synthesize long-chain PUFAs via a kind of PUFA synthase (Metz et al.2001),which is O2-independent.So low oxy-gen supply in the lipids’accumulation stage is more favourable for DHA and other long-chain PUFAs accumulation.In our study,the DHA concentrations in the total fatty acids under different oxygen supply condi-tions showed that lower oxygen supply led to higher DHA concentration(Table1).This result proved that low oxygen supply is more favourable for DHA accumulation. In conclusion,this paper described a two-stage oxygen supply control strategy based on the kinetic analysis for efﬁcient DHA fermentation by Schizochytrium sp.Finally, the maximum concentration of lipid and DHA reached 46Æ6and17Æ7g l)1with the productivity of111mg l)1h)1.This is another example to showing the advantage of two-stage control strategy in terms of microbial physi-ology.As K L a is a scaling-up parameter,the idea devel-oped in this paper could be scaled-up to industrial process and applied to other industrial biotechnological processes to achieve both high product concentration and high productivity.AcknowledgementsThis work wasﬁnancially supported by the Key Program of National Natural Science Foundation of China(no. 20936002),the National Basic Research Program of China (nos.2007CB707805and2009CB724700),the Scientiﬁc Research Project for Postgraduate in Jiangsu Province (no.CX07s_032z),the Fifth of Six Projects Sponsoring Talent Summits of Jiangsu Province(no.2008-D-63),the College Industrialization Project of Jiangsu Province(no. JH09-30),the Fok Ying Tung Education Foundation(no. 123014)and the Program for Century Excellent Talents in University from the Ministry of Education of China (no.NCET–09–0157).We also thank both managerial and technical staff of Jiangsu TianKai Biotechnology Co., Ltd.(Nanjing,P.R.China)for providing the manufactur-ing facilities and technical assistance.ReferencesBailey,R.B.,DiMasi,D.,Hansen,J.M.,Mirrasoul,P.J., Ruecker,C.M.,Veeder,G.T.III,Kaneko,T.and Barclay,W.R.(2003)Enhanced production of lipids containingpolyenoic fatty acid by very high density cultures ofeukaryotic microbes in Patent6607900. Chi,Z.Y.,Hu,B.,Liu,Y.,Frear,C.,Wen,Z.Y.and Chen,S.L.(2007)Production of x-3Polyunsaturated Fatty AcidsFrom Cull Potato Using an Algae Culture Process.ApplMicrobiol Biotechnol134-140,805–815.Chi,Z.Y.,Liu,Y.,Frear,C.and Chen,S.L.(2009)Study of a two-stage growth of DHA-producing marine algae Schizo-chytrium limacinum SR21with shifting dissolved oxygenlevel.Appl Microbiol Biotechnol81,1141–1148.Huang,H.,Ren,L.J.,Xiao,A.H.,Jin,L.J.and Li,J.(2009)A kind of Schizotrium sp.and the method for DHA-rich oilEnhancement of docosahexaenoic acid production L.Qu et al.production using thereof.Chinese Patent(in Chinese),200910033869.5.Jakobsen,A.N.,Aasen,I.M.,Josefsen,K.D.and Strom,A.R.(2008)Accumulation of docosahexaenoic acid-rich lipid in thraustochytrid Aurantiochytrium sp.strain T66:effects of N and P starvation and O2limitation.Appl MicrobiolBiotechnol80,297–306.Ji,X.J.,Huang,H.,Du,J.,Zhu,J.G.,Ren,L.J.,Hu,N.and Li, S.(2009)Enhanced2,3-butanediol production by Klebsiel-la oxytoca using a two-stage agitation speed control strat-egy.Bioresour Technol100,3410–3414.Lauritzen,L.,Hansen,H.S.,Jorgensen,M.H.and Michaelsen, K.F.(2001)The essentiality of long chain n-3fatty acids in relation to development and function of the brain andretina.Prog Lipid Res40,1–94.Metz,J.G.,Roessler,P.,Facciotti,D.,Levering,C.,Dittrich,F., Lassner,M.,Valentine,R.,Lardizabal,K.et al.(2001)Production of polyunsaturated fatty acids by polyketidesynthases in both prokaryotes and eukaryotes.Science293, 290–293.Nordoy,A.,Marchioli,R.,Arnesen,H.and Videbaek,J.(2001) n-3polyunsaturated fatty acids and cardiovascular diseases.Lipids36,127–129.Perveen,Z.,Ando,H.,Ueno,A.,Ito,Y.,Yamamoto,Y., Yamada,Y.,Takagi,T.,Kaneko,T.et al.(2006)Isolation and characterization of a novel thraustochytrid-like micro-organism that efﬁciently produces docosahexaenoic acid.Biotechnol Lett28,197–202.Puskeiler,R.and Weuster-Botz,D.(2005)Combined sulﬁte method for the measurement of the oxygen transfer coefﬁ-cient KLa in bioreactors.J Biotechnol120,438. Ratledge,C.(2004)Fatty acid biosynthesis in microorganisms being used for Single Cell Oil production.Biochimie86,807–815.Ren,L.J.,Huang,H.,Xiao,A.H.,Lian,M.and Ji,X.J.(2009) Enhanced docosahexaenoic acid production by reinforcing acetyl-CoA and NADPH supply in Schizochytrium sp.HX-308.Bioprocess Biosyst Eng32,837–843.Ren,L.J.,Ji,X.J.,Huang,H.,Feng,Y.,Qu,L.,Tong,Q.Q.and Ouyang,P.K.(2010)Development of a stepwise aerationcontrol strategy for efﬁcient docosahexaenoic acid produc-tion by Schizochytrium sp.Appl Microbiol Biotechnol87,1649–1656.Sijtsma,L.and de Swaaf,M.E.(2004)Biotechnological pro-duction and applications of the x-3polyunsaturated fatty acid docosahexaenoic acid.Appl Microbiol Biotechnol64,146–153.Unagul,P.,Assantachai,C.,Phadungruengluij,S.,Pongsuteera-gul,T.,Suphantharika,M.and Verduyn,C.(2006)Bio-mass and docosahexaenoic acid formation bySchizochytrium mangrovei Sk-02at low salt concentrations.Bot Mar49,182–190.Yaguchi,T.,Tanaka,S.,Yokochi,T.,Nakahara,T.and Higashihara,T.(1997)Production of high yields ofdocosahexaenoic acid by Schizochytrium sp.strain SR21.J Am Oil Chem Soc74,1431–1434.L.Qu et al.Enhancement of docosahexaenoic acid production。

铝合金车身客车蒙皮接缝处理工艺方法研究

2020年第8期一、研究背景随着客车车身轻量化的不断推广，客车制造越来越多地采用铝合金作为车身材料。

蒙皮接缝处理不当会造成明显的油漆开裂，影响产品质量，因此，如何有效处理铝合金蒙皮的接缝，降低蒙皮接缝对后续油漆工序的影响尤为重要。

目前经过生产实践，总结出四种接缝处理方法，包括原子灰处理法、聚氨酯胶填充法、贴胶带纸补偿法、丢缝处理+打胶处理法等。

本文主要从操作方法、优点、缺陷及应用范围等几方面进行研究。

二、原子灰处理法原子灰又称腻子，是由大量的填充颜料、树脂和溶剂组成的一种粘稠的浆状涂料，用来填嵌工件表面的凹陷、气孔、擦伤、接缝等缺陷，干燥打磨后可以获得均匀平整的表面。

根据不同的用途，原子灰可分为钣金原子灰、塑料原子灰和幼滑原子灰（快干原子灰）。

鉴于铝合金基材较为敏感，选用合金原子灰作为填嵌铝合金蒙皮接缝的实验产品。

操作方法：铝合金车身蒙皮粘接完成后，整车经过高压冲洗，彻底除去容器的灰尘、油污等；将合金灰主剂及固化剂进行搅拌混合，充分搅拌均匀，使其颜色一致，混合率应按其重量比例计算；原子灰的可用时间受到温度和湿度的影响，配制后要在7～10min 以内使用；嵌油灰必须用刮刀彻底捋平以防泡沫；腻子彻底硬化之后才可以打磨(20℃时，需经1h 以上才硬化，雨季及湿度较高时，原子灰硬化时间要稍延长)。

原子灰处理法具有灰质细腻、易刮涂、易填平、易打磨、干燥速度快、附着力强、硬度高、不易划伤、柔韧性好、耐温变、成本低等优点。

但原子灰及配套固化剂在灌装后，存在溶剂、树脂、矫顽力，对磁体的室温剩磁几乎没有影响；扩散热处理提高了磁体的高温矫顽力，对高温剩磁也几乎没有影响。

这是因为扩散热处理后，Dy 元素主要存在于晶粒表层，改善了晶粒表层的各向异性场，相应地提高了室温和高温矫顽力。

然而，磁体的剩磁温度稳定性主要由主相晶粒控制，扩散热处理对主相晶粒的影响较小，因而扩散热处理前后磁体的高温剩磁基本一致。

四、结论通过Dy 元素的晶界扩散，可以在一定程度上提高烧结钕铁硼磁体的矫顽力。

基于约瑟夫森效应的交流电压标准研究_朱珠

表1 交流电压标准特性对照表波形合成法约瑟夫森结类型输出电压（ max）输出信号输出频率（ max）测量不确定度二进制结 10V 离散信号 2kHz 脉冲调制法脉冲可编程结几百毫伏连续信号 30MHz［3］
［ 2］ Ralf Behr． Synthesis of Precision Waveforms Using a SINIS Josephson Junction Array ［ J］． IEEE Transactions on Instrumentation and Measurement， 2005 ， 54 （ 2 ）．［ 3］ Samuel P． Benz． Pulse － Driven Josephson Digital / Analog Converter ［ J］． IEEE Transactions on Applied Superconductivity， 1998 ， 8 （ 2）．［ 4］ Clark A． Hamilton． AC Josephson Voltage Standard： Progress Report ［ J］． IEEE Transactions on Instrumentation and Measurement， 1997 ， 46 （ 2 ）．［ 5］ Charles J． Burroughs，AC Josephson Voltage Standard Error Measurements and Analysis ［J］． IEEE Transactions on Instrumentation and Measurement， 2003 ， 52 （ 2）．［ 6］ C． A． Hamilton． Josephson D / A Converter with Fundamental Accuracy ［ J］． IEEE Transactions on Instrumentation and Measurement， 1995 ， 44 （ 2 ）．［ 7］ S． P． Benz，P． D． Dresselhaus，C． J． Burroughs et al． Precision measurements using a 300 mV Josephson arbitrary waveform synthesizer ［ J］． IEEE Trans． Appl． Supercond．， 2007．［ 8］ J． M． Williams，D． Henderson，P． Patel et al． Achieving sub － 100 － ns switching of programmable Josephson arrays ［J］． IEEE Trans． Instrum． Meas．，2007 ，56 （ 2 ）： 651 ～ 654．［ 9］ L． Palafox，G． Ramm，R． Behr et al． Primary ac power standard based on programmable Josephson junction arrays ［ J］． IEEE Trans． Instrum． Meas．， 2007 ， 56 （ 2 ）： 534 ～ 537．［ 10］ C． J． Burroughs，P． D． Dresselhaus，et al． Design of the NIST 10V programmable Josephson voltage standard system ［ C］． Conf． Digest CPEM2010 ， 2010．

ISO7637-2和ISO16750-2标准与对策

ISO7637-2和ISO16750-2标准与对策ISO 7637-2 和ISO 16750-2 标准与对策来源：雷卯电⼦在汽车电⼦中，电源瞬态浪涌可能对电⼦设备造成永久的损坏。

随着汽车上电⼦设备应⽤的逐年增多，各家汽车⼚商在实践中积累了宝贵的经验，发现在某些特定场景下的电源瞬态变化更易对设备造成损坏。

因此车⼚都制定相关的测试规范，重点测试在这些电源瞬态下，电⼦设备的抗⼲扰能⼒，硬件设计中必须预留⾜够的防护⼿段以抑制这些电源极端情况的影响。

表1列出在汽车电⼦系统中常见有害的电源瞬态情况。

表1. 汽车电⼦中常见有害的电源瞬态各家⼚商的测试标准也逐渐形成统⼀的国际标准，本⽂简要介绍ISO 标准中对汽车电⼦设备电源测试的要求，具体包括ISO 7637-2和ISO 16750-2中所阐述的汽车电源中可能遭遇的恶劣条件，如负载突变、电池反接和过压等场景下对应的电源测试要求。

ISO 7637-2ISO 7637 全称Road vehicles -- Electrical disturbances from conduction and coupling，是⼀项针对EMC的测试标准，标准分三⼤部分：ISO 7637-1:2015 -Definitions and general considerationsISO 7637-2:2011 -Electrical transient conduction along supply lines onlyISO 7637-3:2016 -Electrical transient transmission by capacitive and inductive coupling via lines other than supply lines尽管是EMC测试的标准，ISO 7637 也包含对电源测试的要求（ISO 7637-2）。

在2011年，ISO 7637 将其中与EMC不相关的电源测试，例如Load Dump 测试的Pulse 5a, 5b 移到ISO 16750-2，但标准中仍然保留着电源瞬态测试波形Pulse 1, 2a, 2b, 3a和3b。

Enhanced magnetic performance of metal-organic nanowire arrays by

Enhanced magnetic performance of metal-organic nanowire arrays by FeCo/polypyrrole co-electrodepositionX. J. Luo, W. B. Xia, J. L. Gao, S. Y. Zhang, Y. L. Li et al.Citation: J. Appl. Phys. 113, 17B908 (2013); doi: 10.1063/1.4800835View online: /10.1063/1.4800835View Table of Contents: /resource/1/JAPIAU/v113/i17Published by the AIP Publishing LLC.Additional information on J. Appl. Phys.Journal Homepage: /Journal Information: /about/about_the_journalTop downloads: /features/most_downloadedInformation for Authors: /authorsDownloaded 04 Jul 2013 to 202.207.14.58. This article is copyrighted as indicated in the abstract. Reuse of AIP content is subject to the terms at: /about/rights_and_permissionsEnhanced magnetic performance of metal-organic nanowire arrays by FeCo/polypyrrole co-electrodepositionX.J.Luo,W.B.Xia,J.L.Gao,S.Y .Zhang,Y .L.Li,S.L.Tang,a)and Y .W.DuNanjing National Laboratory of Microstructures,Jiangsu Provincial Laboratory for Nanotechnology and Department of Physics,Nanjing University,Nanjing 210093,People’s Republic of China(Presented 16January 2013;received 20October 2012;accepted 29January 2013;published online 10April 2013)FeCo/polypyrrole (PPy)composite nanowire array,which shows enhanced magnetic remanence and coercivity along the nanowires,was fabricated by AC electrodeposition using anodic aluminum oxide templates.High resolution transmission electron microscopy shows that PPy grows on the surface of FeCo nanowires forming a coaxial nanowire structure,with a coating layer of about 4nm.It suggests that the decreased dipolar interaction due to the reduced nanowire diameters is responsible for the enhancement of magnetic performance.The possible mechanism of this coating may be that PPy is inclined to nucleate along the pore wall of thetemplates.VC 2013AIP Publishing LLC .[/10.1063/1.4800835]INTRODUCTIONMetal-organic composite nanostructures have attractedmuch interest due to their excellent properties on the catalyst,1biosensor,2optical,3and memory devices.4The polymer poly-pyrrole (PPy)is a good choice for the organic coating layer in the metal-organic composite,because it has good electrical and optical properties and stability.5,6However,most PPy coating has been synthesized by chemical reaction,7,8in which the product is usually in the form of powder,which is difﬁcult to purify.Also,the powder composites are unfavorable for applications in magnetic memory devices,which are strongly dependent on shape and size.In this work,arrays of PPy–magnetic metal composites were obtained by an eco-nomic and effective AC electrodeposition process into anodic aluminum oxide (AAO)templates,which show enhanced magnetic performance due to the reduced diameters after PPy coating.This offers great promise for magnetic memory devi-ces and spintronics applications.9EXPERIMENTSTwo types of AAO templates were prepared using 110l m thick aluminum foil (99.999%)at room temperature (about 25 C).One kind of template was oxidized in 0.3M oxalic acid at 40V for 3h.The another one was oxidized in 0.4M sulphuric acid at 25V for 6h,and then immersed in 0.3M H 3PO 4at 30 C for 20min,in order to increase the pore size.The resulting AAO templates had an average pore diameter of 45nm (35nm),and the center to center interpore distances about 110nm (60nm)in oxalic acid (sulphuric acid).FeCo/PPy composite nanowires were deposited from an electrolyte solution consisting of 0.02M CoSO 4Á7H 2O,0.016M FeSO 4Á7H 2O,1g/l ascorbic acid,and 0.021M pyr-role (Py)monomer,using 0.25M boric acid as buffer agent and 0.05M LiClO 4Á3H 2O as the oxidizer.In the electrolyteprepared for the growth of pure FeCo,we only removed the Py monomer.The wires were deposited in an AC electric ﬁeld of 13.3V at 50Hz.All nanowires were deposited for 30min.Magnetic properties were measured by vibrating sample magnetometer (VSM)at room temperature.X-Ray diffraction (XRD)was performed on the nanowire sheets where Al substrate was removed.The harvested nanowires prepared for TEM (Transmission Electron Microscopy)to-pography and HRTEM (High Resolution Transmission Electron Microscopy)measurements were rinsed in deion-ized water,and deposited onto the copper grid for the imag-ing.The topography of nanowires was characterized by TEM (JEOL–2010,Japan),and the HRTEM was character-ized by TEM (ARM200F,Japan).Both types of nanowires have the length more than 2l m,thus the inﬂuence of the lon-gitudinal demagnetizing factor for the magnetic performance can be ignored due to the large aspect ratio of the nanowires L =D w >50,10with L and D w the length and diameter of the nanowires,respectively.The nanowires were dried and pressed into pellets with KBr powder,in order to undergo the Fourier transform infrared (FT-IR)spectroscopic meas-urements using a Nexus 870spectrometer (Nicolet,USA).RESULT AND DISCUSSIONFig.1shows the XRD patterns of FeCo and FeCo-PPy co-deposition nanowires.Both nanowires have body-centered-cubic (bcc)structures with preferred (110)orientation along the axis of the wire.The Energy Dispersive Spectrometer (EDS)shows that the atomic ratio of Fe:Co in pure FeCo nanowires is close to 49:51and is 46:54in FeCo-PPy co-deposition nano-wires.Fig.2shows the FTIR absorption spectra of (a)pure FeCo and (b)FeCo-PPy co-deposition nanowires deposited in oxalic acid oxidized pared with pure FeCo nanowires,there are extra absorption peaks at 1161,1731,3426,3736cm À1,etc.,for FeCo-PPy co-deposition nanowires.The broad peak at 3426cm À1indicates a N–H,C–H stretch in the polypyrrole ring,11and the peak near 1161cm À1is attributed to the breathing vibration of the pyrrole ring.12a)Author to whom correspondence should be addressed.Electronic mail:tangsl@.0021-8979/2013/113(17)/17B908/3/$30.00VC 2013AIP Publishing LLC 113,17B908-1JOURNAL OF APPLIED PHYSICS 113,17B908(2013)The medium strong transmittance at 1731cm À1arises from the C ¼O stretching from the carboxylic group,which may attach to the AAO template wall before electrodeposition.Carboxylic group and PPy may form a covalent binding,which is favorable for the PPy nucleation on the AAO wall.However,pure FeCo nanowires do not show this peak.These results conﬁrm that PPy has grown into the nanowires in the FeCo-PPy co-deposition process,forming FeCo/PPy composite nanowires.Figure 3shows the room temperature magnetic hysteresis loops of nanowires deposited into two types of templates.The measurements were taken both with magnetic ﬁeld parallel (H k )and perpendicular (H ?)to the wire axis.Figs.3(a)and 3(b)show FeCo and FeCo/PPy composite nanowires grown in templates oxidized in oxalic acid.The remanence ratio and coercivity for pure FeCo is 89%and 2105Oe,and increased up to 97%and 2520Oe for FeCo/PPy composite nanowires.Similarly,for the nanowires deposited in the templates oxidized in sulfuric acid,the remanence ratio and coercivity reaches up to 94%and 2845Oe for FeCo/PPy composite nanowires (see Fig.3(d)),compared to the ones of 59%and 1961Oe for the pure FeCo nanowires.In both cases,the addition of PPy has effectively enhanced the magnetic remanence ratio and coerciv-ity.However,how the PPy grows into the nanowires and how it enhances the magnetic performance are still unclear.As the magnetocrystalline anisotropy of the ordered FeCo alloy is negligible,13we should mainly discuss the shape ani-sotropy,which is largely determined by the competition of demagnetization of the individual wires and magnetic dipolar interaction between the wires,due to the large aspect ratio of the nanowires.In the direction of magnetic ﬁeld perpendicular to the wire axis,the effective ﬁeld can be simpliﬁed as 10,14H ?k ¼H ?dem ÀH ?di ¼2p M s À2:1p M s D 2w L =ð4D 3i Þ:(1)In the direction of magnetic ﬁeld parallel to the wire axis (perpendicular to the ﬁlm),as the demagnetizationofFIG.1.The XRD spectra for FeCo and FeCo/PPy compositenanowires.FIG. 2.The FTIR spectra for (a)FeCo/PPy composite nanowires and(b)FeConanowires.FIG.3.(a)and (b)The magnetic hys-teric loops for FeCo and FeCo/PPy com-posite nanowires oxidized in oxalic acid.(c)and (d)The magnetic hysteric loops for FeCo and FeCo/PPy composite nano-wires oxidized in sulfuric acid.the individual wire is nearly zero,the effective anisotropic ﬁeld is mainly the dipolar interaction ﬁeldH kdi ¼4:2p M s D 2w L =ð4D 3i Þ(2)with D w the wire diameter,M s the saturation magnetizationof the nanowire array,and D i the interpore distance.Equations (1)and (2)suggest that the decrease of the dipole interaction ﬁeld can introduce the enhancement of magnetic remanence ratio and coercivity.If PPy grows on the surfaces as a coating layer of FeCo nanowires,a decreased nanowire diameter D w can be obtained,and then the weakened dipole interaction ﬁeld would bring a better permanent magnetic performance.The evidences are expected in the topography.Figure 4shows the TEM topography of (a)pure FeCo and FeCo/PPy composite nanowires deposited in the tem-plates oxidized in oxalic acid.The FeCo/PPy composite nanowire has a subtle coating layer (Fig.4(b)),which may be a very thin PPy coating.Figs.4(c)and 4(d)show the HRTEM images and electron diffraction (ED)patterns of pure FeCo and FeCo/PPy composite nanowires.There is a clear difference between the surfaces of these two kinds of nanowires.The FeCo/PPy composite shows a coating layer with subtle diffraction fringes (Fig.4(d)),while the pure FeCo nanowire (Fig.4(c))has none.The subtle diffraction fringes in the coating suggest a mixed crystal and amorphous phases.As the ED spots pattern (in a radius of 200nm area)show a single body centered FeCo pattern,we attribute the fringes to a small amount of FeCo,which was trapped in the amorphous PPy.The thin FeCo-PPy coexistence region is about 4nm in width,which will make a decrease of nanowire array diameter about 8nm.According to Eq.(1),the dipolar interaction will decrease by 40%,if the saturation magnet-ization and interpore distance are kept constant,which will largely enhance the magnetic remanence ratio and coercivity along the wire.Previous studies have shown that PPy is inclined to grow along the AAO and form PPy nanotubes,and the nano-tubes can be partially ﬁlled along the tube wall withincreasing deposition time.15The process indicates that PPy nucleates ﬁrst along the AAO wall.The reason may be the rich hydroxyl,carboxyl,and other hydrophilic radicals along the AAO wall.16These radicals may easily combine with the pyrrole ring,introducing nascent polypyrrole nucleate along the pore wall,At the same time,FeCo metal would nucleate at the pore base ﬁrst due to its ionic and polaron character,then grow along the electric ﬁeld in the negative half-period of electric ﬁeld.At last,PPy as a coating layer grows on the FeCo surface,forming a coaxial nanowire.CONCLUSIONIn conclusion,by a simple one-step AC electrodeposi-tion method,we had obtained FeCo/PPy composite nano-wires with PPy as the coating layer,with enhanced magnetic performance.The possible growth mechanism is that PPy is inclined to grow along the AAO wall because of the covalent hydrophilic radical on the wall,while FeCo prefers to nucle-ate in the centre of the AAO along the electric ﬁeld.The sim-ple one-step AC electrodeposition process presented here could be extended to other metals and polymers,which will has great application prospect.ACKNOWLEDGMENTSThis work was supported by the National Key Project of Fundamental Research of China (Grant Nos.2012CB932304and 2010CB923404),the Natural Science Foundation of China (Grant Nos.50971070and U1232210),and the Priority Academic Program Development of Jiangsu Higher Education Institutions.1K.Kwon,S.Jin,C.Pak,H.Chang,S.H.Joo,H.I.Lee,J.H.Kim,and J.M.Kim,Catal.Today 164(1),186(2011).2Y.Dan,Y.Cao,T.E.Mallouk,A.T.Johnson,and S.Evoy,Sens.Actuators B 125(1),55(2007);R.Dasari, F.J.Ibanez,and F.P.Zamborini,Langmuir 27(11),7285(2011).3L.J.Borthakur,S.Sharma,and S.K.Dolui,J.Mater.Sci.-Mater.Electron.22(8),949(2010).4J.A.Switzer,R.V.Gudavarthy,E.A.Kulp,G.Mu,Z.He,and A.J.Wessel,J.Am.Chem.Soc.132,1258(2010).5Y.Z.Long,M.M.Li,C.Gu,M.Wan,J.L.Duvail,Z.Liu,and Z.Fan,Prog.Polym.Sci.36(10),1415(2011).6L.Liu,C.Zhao,Y.Zhao,N.Jia,Q.Zhou,M.Yan,and Z.Jiang,Eur.Polym.J.41(9),2117(2005).7Y.Liu,Z.Liu,N.Lu,E.Preiss,S.Poyraz,M.J.Kim,and X.Zhang,mun.(Cambridge)48(20),2621(2012).8X.M.Feng,Z.Z.SunW.H.Hou,and J.J.Zhu,Nanotechnology 18,195603(2007);X.Li,Y.Gao,J.Gong,L.Zhang,and L.Y.Qu,J.Phys.Chem.C 113,69(2009).9K.R.Pirota,F.B e ron,D.Zanchet,T.C.R.Rocha,D.Navas,J.Torrej o n,M.Vazquez,and M.Knobel,J.Appl.Phys.109,083919(2011).10H.L.Su,G.B.Ji,S.L.Tang,W.Chen,Z.Li,B.X.Gu,and Y.W.Du,J.Appl.Phys.97(11),116104(2005).11K.Nam,G.Lee,H.Jung,J.Park,C.H.Kim,J.Seo,D.S.Yoon,S.W.Lee,and T.Kwon,Nanotechnology 22(22),225303(2011).12L.Goswami,N.S.Sarma,and D.Chowdhury,J.Phys.Chem.C 116,6446(2012).13D.H.Qin,Y.Peng,L.Cao,and H.L.Li,Chem.Phys.Lett.374,661(2003).14G.J.Strijkers,J.H.Dalderop,M.A.A.Broeksteeg,H.J.M.Swagten,and W.J.M.de Jonge,J.Appl.Phys.86,5141(1999).15Y.F.Chen,J.Liu,H.J.Yao,D.Mo,J.L.Duan,M.D.Hou,Y.M.Sun,L.Zhang,and K.Maaz,Physica B 405(10),2461(2010).16Y.Yamamoto,N.Baba,and S.Tajima,Nature (London)289,572(1981).FIG.4.(a)and (c)The TEM and HRTEM images,respectively,for FeCo nanowires,(b)and (d)the TEM and HRTEM images,respectively,for FeCo/PPy composite.。

The HRM organisational effectiveness link_ overview and the role of HR practitioners

Asia Pacific Human Resource Management and Organisational EffectivenessISBN 978-0-08-100643-6/10.1016/B978-0-08-100643-6.00011-7Copyright © 2016 Elsevier Ltd. All rights reserved.CHAPTER 11Conclusion: the human resource management–organisational effectiveness link: overviewand the role of HR practitionersC. Rowley, A. Nankervis, N.M. SallehINTRODUCTIONAs we stated in Chapter 1, the contributions of human resource (HR) func-tions and practitioners and HR management (HRM) systems and processes to organisational effectiveness has been less focused on Asia. Our book explores this subject and region both conceptually and empirically. Accordingly, our book adds to the literature and strategic HRM (SHRM) on this important topic and the differences and similarities between these linkages in Asian and W estern contexts using diverse countries, sectors and organisations, including multinational companies (MNCs).This chapter has twin aims. First we reiterate our individual contribu-tions, before exploring HRM more broadly and the developmental role of HR practitioners on organisational effectiveness more specifically.OVERVIEW OF CONTENTA quick reminder of the logic and content of our book follows. W e divided the chapters into three parts. The first part comprised two conceptual chap-ters and explored broad contextual issues impacting on the HRM and organisational effectiveness relationship in different regions and organisa-tions. Chapter 2 overviewed the challenges and opportunities associated with the formation of the new Asian Economic Community (AEC) to reveal ‘winner’ and ‘loser’ economies. Thus Singapore had significant attrac-tion and retention opportunities relative to Malaysia, Thailand, Indonesia and the Phillipines, but possibly struggled to retain its advantages against Australia and New Zealand due to their attractive employment conditions231232Asia Pacific HRM and Organisational Effectivenessand lifestyle issues. The HRM and organisational effectiveness relationship will be a crucial factor in the projected increases in labour mobility envis-aged by the AEC.Chapter 3 presented a different macro-perspective on HRM and organ-isational effectiveness. Through an intra-psychic lens it examined the trans-ference of W estern theories of emotional intelligence (EI), mindfulness and neurobiological science to Asian cultures and HRM practices given the significant cultural differences in emotional expression between them. It considered the application of these concepts to teamwork, job performance, productivity, leadership and overall organisational performance and found EI enabled better assessment and moderation of contingencies while mak-ing decisions.The second part had five chapters on HRM roles and competencies and organisational effectiveness in Asian countries. Chapter 4 took a broader approach, and analysed corporate social responsibility and unethical prac-tices during and after the 2008 global financial crisis in the Australian bank-ing sector. This showed how unethical behaviours eroded stakeholders’ (employees’ and customers’) commitment and engagement, with conse-quences for organisational effectiveness and how HRM practices could be enhanced through attention to and reinforcement of ethical behaviours.The next three chapters focused more on the relationship between HRM roles and competencies and organisational effectiveness. Chapter 5 explored the HRM ‘strategic business partner’ (SBP) role in Indian MNCs. It argued that SHRM was most productive when it encompassed the three key components of ‘strategic agility’ (external fit), ‘knowledge management’ and ‘management development’ (internal fit). It concluded that the SBP role was especially critical for MNCs operating in complex and dynamic busi-ness environments.Chapter 6 analysed HRM’s ‘evolution’ in stages from an administrative to a more strategic role and the associated contributions to organisational effec-tiveness in three Asian economies. It found that while there were differences in the forms and applications of SHRM across diverse ownership and sector types, overall most HR roles remained primarily the ‘functional HRM spe-cialist’, having progressed from purely ‘administrative expert’ roles but not yet developed fully as SBPs. It identified differences between countries, sectors and organisational types and concluded that HRM is in a transitional phase.Chapter 7 analysed the application of concepts of HRM devolution and social capital to the links between HRM, line managers andConclusion233 organisational effectiveness. Using the example of hospitality resorts in the Maldives, this chapter explored how these managerial relationships enhanced HRM practices and organisational effectiveness. It concluded that there was an ‘interaction effect’ between HR professionals and line managers.Chapter 8 focused on the relationships between SHRM and work qual-ity in Australian organisations. Using a four-dimensional analytical frame-work of job prospects, intrinsic job quality, extrinsic job quality and working time quality, it demonstrated that organisational effectiveness had both qual-itative and quantitative components and associated work quality with well-being from the employee perspective. Good work quality (on all four dimensions) was likely to result in higher productivity and organisational effectiveness, as seen in lower rates of employee turnover, absenteeism and tardiness and improved well-being.The third part contained two complementary chapters which analysed the influences of Asian employee relations and Islamic traditions on the HRM and organisational effectiveness link. Chapter 9 explored trade union relationships with members and the government in Malaysia. T o determine if trade union strength could be developed through its members relation-ship capital theory was used to identify if it could create a strong bond with members. It analysed the effectiveness of unions in relation to their repre-sentation of the collective ‘voice’ of members needs, particularly in negotia-tions over salary, security and safety and whether they assisted in the satisfaction of employees’ self-esteem and self-actualisation needs. It ques-tioned whether unions could be strengthened through the facilitation of expressions of member ‘voice’.Chapter 10 provided a conceptual framework for the analysis of job satisfaction from an Islamic perspective. Using W estern notions of extrinsic and intrinsic job satisfaction determinants the chapter explored how they were applied in Islamic organisations. Intrinsic determinants were the moti-vation to actively engage in learning activities out of curiosity, interest or enjoyment in order to achieve intellectual and personal goals. Intrinsic fac-tors focused on the non-materialistic goals. Examples of Islamic concepts and principles demonstrated the differences and similarities with W estern counterparts within and outside these countries. It concluded that Islamic organisations were more likely to favour intrinsic rather than extrinsic approaches towards job satisfaction, with emphases on religious values and personal and community services.234Asia Pacific HRM and Organisational EffectivenessOverall, our chapters indicated several important points in the HRM–organisational effectiveness relationship. One is the key issue of the role of HR practitioners themselves. W e now locate this in its HRM context.OVERVIEW OF THE ROLE OF HRM AND HR PRACTITIONERSMarchington (2008) argued that HRM’s key role was to ‘balance the com-peting needs of different constituents … and to solve problems’ (p. 4). He provided a categorisation of broad HRM competencies as ‘a sound under-standing of how institutions and markets shape people management and organisations; very strong technical knowledge of HR practice and pro-cesses’ (p. 16). Hall and Fourie (2007) similarly summarised overall HRM roles as ‘creators or drivers of the business’ which required an ‘understanding of the internal and external stakeholders’ (p. 54).Challenges to HRM include strategic decision-making, culture man-agement, fast change and market-driven connectivity (Brockbank and Ulrich, 2003) as well as clearly and robustly ‘proving’ the added-value of HRM practices and HR practitioners. Much HRM research focuses on establishing linkages between HRM and organisational performance, a key driver in competitive advantage. Competitive advantage can derive from the optimal utilisation of internal organisational resources (Wright et al., 2001), notably HR or human capital, ensured through the alignment of HRM strategies and processes and overall business strategies (Brockbank and Ulrich, 2003; Boudreau and Ramstad, 2003). This is the key assumption underlying taxonomies of HR roles and competencies, which together facilitate such successful alignments.However, not all organisational stakeholders are equally important in this pursuit and, therefore, diverse HR approaches and competencies may be required, not only for different countries, industries and organisations, but also for the ‘lifecycle’ stage within them. It might also be inferred that not all HR professionals will possess or require all of the designated compe-tencies and that sector and business development stages will demand differ-ent sets of HRM skills and competencies.VARIATIONS IN HR PRACTICE AND PROFESSIONALSOne key variable in the policies and practice of HRM is business strategy and its obvious organisational variations (see Rowley, 2003; Rowley andConclusion235 Harry, 2011; Rowley and Jackson, 2011). Many taxonomies have been dis-tinguished. These include those in so-called lifecycle models (such as K ochan and Barocci, 1985), with ‘Start-Up’, ‘Growth’, ‘Maturity’ and ‘Decline’ phases. Porter (1985) had ‘Cost Reduction’, ‘Quality Enhance-ment’ and ‘Innovation’ strategies. The earlier strategies of ‘Defender’ and ‘Prospector’ (Miles and Snow, 1978) were developed into ‘Internal’ and ‘Market T ype’ employment systems (Delery and Doty, 1996). Grubman (1998) aligned HRM practices to strategic styles labelled ‘Products’, ‘Oper-ations’ and ‘Customers’. Each of these strategy types have radically different implications for HRM and HR practitioners.HRM theorists have identified the key roles and competencies which define their strategic, policy and operational functions (Brockbank et al., 1997; Boudreau and Ramstad, 2003; Carroll, 1990; T yson and Fell, 1986; Wright et al., 2001). It can be seen that, on the one hand, HRM strategies and processes should represent an amalgam of responses to the chal-lenges of the external business environment and internal company imperatives, while on the other that all HRM functions should be inte-grated with each other (horizontally) and with HRM strategies (vertically).However, labels often cover a myriad of meanings and practices. In the area of people management and HRM this is certainly the case. So, what has often emerged are a range of titles and names to capture the radically different roles and jobs HR practitioners do. For example, Renwick (2003) suggested three HR manager roles of ‘Policy Makers’, ‘Advice Pro-viders’ and ‘Administrators’. One useful early schema to recall is the framework developed by T yson and Fell (1986) of different types of ‘people manager’. Using variations in simple variables such as ‘discretion’ (low to high) and ‘planning horizon’ (short to long term), a trio of prac-titioner types each with distinctly different roles were distinguished. These were ‘Clerk of the Works’ (services junior line managers; administrative support; follows routines; looks for leadership from others), ‘Contracts Manager’ (services and advises middle managers; provides knowledge of systems/practice; follows systems but modifies to some extent; gives lead-ership within existing structures) and ‘Architect’ (consultant to senior managers; conceptualiser, inventiveness, problem-solver; changes routines/ systems as necessary; copes rapidly with change; leads/participates with top management).Another example is Ulrich (1997), whose HRM roles were ‘Strategic Partner’, ‘Change Agent’, ‘Employee Champion’ and ‘Administrative236Asia Pacific HRM and Organisational EffectivenessExpert’. Iterations of his study, conducted in 2002, 2007 and 2012, led to extensive revisions. One study (2012) canvassed 20,000 respondents (HR and non-HR managers) in ten countries and resulted in HR roles of ‘Strategic Business Partner’, ‘Capability Builder’, ‘Change Champion’, ‘T echnology Proponent’, ‘HR Innovator and Integrator’ and ‘Credible Activist’ (Ulrich et al., 2013: 24).W e can add to this analysis of HR practitioner types by recalling and applying to HRM the seminal work of Katz (1955) with its useful 3 × 4 matrix/grid of skill requirements. T his had three broad, general skills labelled ‘T echnical’, ‘Human’ and ‘Conceptual’ and four job levels of ‘Individual Producer’, ‘Supervisor’, ‘Middle Manager’ and ‘Senior Executive’. Of course, while skills were listed independently, they are interrelated when applied to managerial problems. Nevertheless, the relative importance of these skill groups shifted between job levels and with seniority came, roughly, the need for more human skills, taken as the ability to work cooperatively and be a team player, communicate effectively and resolve conflicts.Variations in HR professionals may also occur due to the organisation’s operational context. We can illustrate this point by considering and apply-ing the underpinnings of the framework of leadership skills in Asia of Rowley and Ulrich (2012a, 2012b). They argued that being an effective leader was a mix of factors, the ‘3Cs’ (‘Context’, ‘Culture’, ‘Competence’) (see Figure 11.1). Some HR practitioners, as detailed in the above typolo-gies, will themselves be leaders of course, as well as, in the jargon, ‘followers’.The first factor, ‘Context’, is the philosophical country context that shapes how people think and act. Philosophical approaches which underlie behaviour and differences show up in W estern versus Asian approaches to business (see Table 11.1). Those from the W est assigned to work in Asian organisations need to be aware of their biases and to adapt to Asian phi-losophies. Similarly, those from Asia who only do things the ‘Asian way’ will be less able to respond to global pressures. Y et Asians who give into the ‘Western way’ will totally lose sight of their heritage and be inattentive to their cultural uniqueness.The second factor, ‘Culture’, is the unique company culture challenges faced in a particular context. An organisation’s culture can start with its strategic challenges. Organisations competing on price need to build cul-tures of efficiency and cost containment. Organisations competing on inno-vation need to build cultures of risk-taking and experimentation. Some Asian organisations are shifting from low-cost production of global goodsConclusion237Figure 11.1Factors affecting effective leadership. Source: Rowley and Ulrich (2012b).to innovative products and services and face demographic trends impacting on labour force supply. Given this, cultural dimensions to consider include the following six.1. P aternalism – Asian context and organisation cultures tend to be hierar-chical and the leaders paternalistic, accepting personal responsibility for the well-being of employees. Asians need to balance hierarchical control through paternalism with employee autonomy that comes from independence.2. T ime – Asian mindsets focus more on long- rather than short-term goals.Partly because of financing through debt (convincing a few investors to support them) over equity (showing profits to convince many unknown investors to invest), Asians take longer-term views. HRM systems also need to reflect these imperatives.3. B enevolence – Asian countries and companies have cultures of deferencewithin the hierarchy and an emphasis on teamwork and conformity to shared behavioural expectations. Outspoken employees rarely challenge seniors and such behaviour is discouraged. Such traditions may restrict organisational effectiveness, especially with respect to innovation. Hence,Asia Pacific HRM and Organisational Effectiveness238managers will need to design internal communication mechanisms by means of which employees are encouraged to share their ideas without compromising manager–employee relationships.4. C ollaboration – Asian culture encourages collaboration, mutual supportand banding together to achieve common goals. Differences of opinion are not encouraged and if voiced, are done so privately and respectfully . Public confrontations – including potentially constructive differences of opinion – are discouraged. Again, the advantages of these cultural fea-tures will need to be balanced with opportunities for individual endeav-our and recognition.5. R elationships – Asians learn the importance of ‘good connections’ (guanxi )as such relationships matter as much or more than technical expertise. Many of these relationships are forged through extended family ties, education or early in careers. In particular, relationships with govern-ment officials and agencies are crucial.Table 11.1 Differences in Western and Asian business approaches Western AsianTime horizonShort term – how Long term – future StrategyLeading to allocation of resources today Leading to positioning the firm for the future ManagementphilosophyManagement by objec-tives Management by shared mindset Decision-makingFast to decide, longer to sell and implement Slow to decide, quick to implement AccountabilityPersonalised and focused on ‘I’Shared and focused on ‘we’W orkLinear and focused on the task at hand Cyclical and focused on the context in which work is done Career orientationGeneralist Specialist Rewards High pay gap betweensenior executives andemployeesPay often based onperformanceLower pay gap between senior executives and employees Pay often based on tenure and position Leadership philosophy Hands on, walking aheadof peopleHands off, walking behind people Philosophical schoolsChristianity Buddhism, Confucianism,Hinduism, Islam, Taoism,Han Fei Adapted from Rowley and Ulrich (2012b).Conclusion239 6. O rganisation – the three archetypes with different requirements are asfollows:– P rivate owned enterprises – smaller start-ups commonly family run.Some have grown and shifted to professional management but they still have embedded family cultures.– S tate-owned enterprises – large, government-owned and dominating the infrastructure (construction, telecommunication, education, util-ities, finance). These need to adapt to changing conditions and make the bureaucracy more adaptable.– M ultinational corporations – large organisations headquartered outside of Asia and doing business in Asia and Asian organisations doing business globally. These face challenges of adapting practices from one Asian context to another.The third factor, ‘Competence’, relates to personal characteristics. There have been numerous studies about whether leaders are ‘born or bred’. These studies look at who leaders are, what they know and what they do as driven by their heritage versus their ability to learn. While some research implies leaders do have pre-dispositions that influence how they think and act, other research also implies leaders can learn to think and act differently if they consciously choose to do so. These findings give insights into what an individual needs to recognise to be effective in HRM. When people are self-aware of their predispositions, they are able to apply or adapt them to their required results. This can be applied to HR practitioners. This clearly indicates that even those managers with the same HR title may be radically different in what they do, what is expected and their skills. CONCLUSIONOur focus on the HRM and organisational effectiveness link and relation-ships and the influences on them in the Asia Pacific region has yielded three key themes. First, there are the implications of ongoing global and regional transformation, including changing governmental policies, demographic profiles, economic shifts and social perspectives. These will inevitably affect Asia Pacific organisations with respect to both their changing measures of and criteria for ‘effectiveness’ and the associated HRM strategies, roles and competencies required to deliver them. The studies in our book suggest that the latter are dynamic and transitional in all of the countries studied and that there are significant variations between countries and between organ-isational types.240Asia Pacific HRM and Organisational EffectivenessSecond, organisational effectiveness is a complex concept that contains both quantitative and qualitative components which are inexorably inter-twined and embrace multiple internal and external stakeholders. Hence, HRM researchers and professionals will need to develop more sophisticated modelling systems and measures which will enable more precise identifica-tion and subsequent justification of the links between HRM and organisa-tional effectiveness.The final theme is the importance of particular regional and country contexts on HRM theory and practice. It can no longer be assumed that US-biased and ethnocentric universalist HRM approaches are desirable or feasible in diverse economic, social, cultural or political environments. The debate over ‘convergence versus divergence’ in HRM has played an impor-tant part in reinforcing our understanding of this issue. However, we need to move further towards the recognition that HRM systems and practices need to be responsive to, and to be transformed by, local traditions as well as by global pressures and opportunities. Therefore, while we may use W estern HRM models and frameworks to analyse HRM strategies, systems and roles in Asia Pacific countries, we should also be prepared to amend them accord-ing to practical experience and growing empirical evidence such as we have presented in this book.REFERENCESBoudreau, J., Ramstad, P., 2003. From Professional Business Partner to Strategic Talent Leader: What’s Next for Human Resource Management? Cornell Center for Advanced Human Resource Studies, New Y ork.Brockbank, W., Ulrich, D., James, C., 1997. Trends in human resource competencies. Third Conference on HR Competencies, University of Michigan School of Business, Ann Arbor, MI.Brockbank, W., Ulrich, D., 2003. The New HR Agenda: 2002 HRCS Executive Summary.University of Michigan Business School, Ann Arbor, MI.Carroll, S.J., 1990. The new HRM roles, responsibilities and structures. In: Schuler, R.S.(Ed.), Managing Human Resources in the Information Age. Bureau of National Affairs, Washington, DC, pp. 204–226.Delery, J., Doty, H., 1996. Modes of theorizing in strategic HRM: tests of universalistic, contingency and configurational performance predictions. Academy of Management Journal 39 (4), 802–835.Grubman, E.L., 1998. The Talent Solution. McGraw-Hill, New Y ork.Hall, C., Fourie, L., 2007. Exploring the role of the human resource function in the South African IT industry. Journal of Human Resource Management 5 (1), 54–64.Katz, R., 1955. Skills of an effective administrator. Harvard Business Review, January–February 33–42.Kochan, T., Barocci, T., 1985. Human Resource Management and Industrial Relations. Little, Brown, Boston.Conclusion241 Marchington, M., 2008. Where Next for HRM? Rediscovering the Heart and Soul of Peo-ple Management. W orking Paper No 20. IES. Manchester Business School, University of Manchester.Miles, R., Snow, C., 1978. Organizational Strategy, Structure and Process. McGraw-Hill, New Y ork.Porter, M., 1985. Competitive Advantage: Creating and Sustaining Superior Performance.Free Press, New Y ork.Renwick, D., 2003. Line manager involvement in HRM: an inside view. Employee Relations 25, 262–280.Rowley, C., 2003. The Management of People: HRM in Context. Spiro, London. Rowley, C., Harry, W., 2011. Managing People Globally: An Asia Perspective. Chandos, Oxford.Rowley, C., Jackson, K., 2011. HRM: The Key Concepts. Routledge, London.Rowley, C., Ulrich, D., 2012a. Setting the scene for leadership in Asia. Asia Pacific Business Review 18 (4), 451–464.Rowley, C., Ulrich, D., 2012b. Lessons learned and insights derived from leadership in Asia.Asia Pacific Business Review 18 (4), 675–681.T yson, S., Fell, A., 1986. Evaluating the Personnel Function. Hutchinson, London. Ulrich, D., 1997. Human Resource Champions: The Next Agenda for Adding V alue to HR Practices. Harvard Business School Press, Boston.Ulrich, D., Brockbank, W., Y ounger, J., Ulrich, M., 2013. Global HR Competencies: Mastering Competitive Value from the Outside In. McGraw-Hill, New Y ork. Wright, P.M., Dunford, B.B., Snell, S.A., 2001. Human resources and the resource-based view of the firm. Journal of Management 27, 701–721.。

CONDUCTIVE METAL INK COMPOSITION, AND METHOD FOR P

专利名称：CONDUCTIVE METAL INK COMPOSITION, AND METHOD FOR PREPARING ACONDUCTIVE PATTERN发明人：Jiehyun Seong,Kyoung Su Jeon,Soo Yeon Heo,Jong Taik Lee,Ji Young Hwang,In-SeokHwang,Seung-Heon Lee申请号：US13819313申请日：20110826公开号：US20130277096A1公开日：20131024专利内容由知识产权出版社提供专利附图：摘要：The present invention relates to a conductive metal ink composition, comprising: a first metal powder having conductivity; a non-aqueous solvent; an attachment improving agent; and a polymer coating property improving agent, and a method for forming a conductive pattern by using the conductive metal ink composition, and the conductive metal ink composition can be appropriately applied to a roll printing process and a conductive pattern exhibiting more improved conductivity and excellent attachment ability with respect to a board can be formed.申请人：Jiehyun Seong,Kyoung Su Jeon,Soo Yeon Heo,Jong Taik Lee,Ji Young Hwang,In-Seok Hwang,Seung-Heon Lee地址：Daejeon KR,Seoul KR,Daejeon KR,Daejeon KR,Daejeon KR,Daejeon KR,Daejeon KR 国籍：KR,KR,KR,KR,KR,KR,KR更多信息请下载全文后查看。

沥青混合料介电特性温度-频率等效原理

第52卷第7期2021年7月中南大学学报(自然科学版)Journal of Central South University (Science and Technology)V ol.52No.7Jul.2021沥青混合料介电特性温度−频率等效原理于晓贺1,2，罗蓉1,2，王锦腾1,2，李冲1,2，束裕1,2(1.武汉理工大学交通学院，湖北武汉，430063；2.湖北省公路工程技术研究中心，湖北武汉，430063)摘要：为量化温度、频率对沥青混合料介电特性的影响，实现无损检测设备在不同温度、频率下的数据统一，通过理论推导建立基于温度、频率的沥青混合料介电模型和温度−频率等效原理，进行不同温度、频率条件下沥青混合料相对介电常数的测量试验。

试验采用介电常数测试平台测定2种沥青混合料在30~60℃温度范围、6种频率条件下的相对介电常数和介电损耗，用以验证沥青混合料介电模型和温度−频率等效原理的可靠性。

研究结果表明：在30~60℃温度范围内，沥青混合料相对介电常数随温度升高而增大，在1~1000kHz 频率范围内，沥青混合料相对介电常数随频率增大而减小；基于温度、频率的沥青混合料介电模型具有较强的适用性，对2组沥青混合料相对介电常数的拟合优度R 2均在0.95以上；温度−频率等效原理对2组沥青混合料相对介电常数的拟合优度R 2均在0.90以上，可以作为实现无损检测设备在不同温度、频率条件下数据统一的理论基础。

关键词：沥青混合料；介电特性；介电模型；温度；频率；等效原理中图分类号：U416.217文献标志码：A开放科学(资源服务)标识码(OSID)文章编号：1672-7207（2021）07-2268-08Development of temperature −frequency equivalence principle onasphalt mixturesYU Xiaohe 1,2,LUO Rong 1,2,WANG Jinteng 1,2,LI Chong 1,2,SHU Yu 1,2(1.School of Transportation,Wuhan University of Technology,Wuhan 430063,China;2.Hubei Provincial Highway Engineering Technology Research Center,Wuhan 430063,China)Abstract:In order to quantify the influence of temperature and frequency on the dielectric properties of asphalt mixtures,and unify the data of non-destructive testing equipment at different temperatures and frequencies,the dielectric model based on temperature and frequency and the temperature-frequency equivalence principle of收稿日期：2020−10−27；修回日期：2020−12−10基金项目(Foundation item)：国家重点基础研究发展规划(973计划)项目(2015CB060100)；湖北省科技厅重点研发计划项目(2020BCA085)(Project(2015CB060100)supported by the National Basic Research Development Program (973Program)of China;Project(2020BCA085)supported by the Key Research and Development Project of Science and Technology Department of Hubei Province of China)通信作者：于晓贺，博士研究生，从事沥青混合料性能及道路无损检测技术等研究；E-mail ：*****************.cnDOI:10.11817/j.issn.1672-7207.2021.07.014引用格式：于晓贺,罗蓉,王锦腾,等.沥青混合料介电特性温度−频率等效原理[J].中南大学学报(自然科学版),2021,52(7):2268−2275.Citation:YU Xiaohe,LUO Rong,WANG Jinteng,et al.Development of temperature −frequency equivalence principle on asphalt mixtures[J].Journal of Central South University(Science and Technology),2021,52(7):2268−2275.第7期于晓贺，等：沥青混合料介电特性温度−频率等效原理asphalt mixtures was established through theoretical derivation,and the relative dielectric constant measurement test of asphalt mixtures under different temperature and frequency conditions was carried out.The Dielectric Constant Testing Platform was used to determine the relative dielectric constant and dielectric loss of the two asphalt mixtures in the temperature range of30−60°C and6frequency conditions,and verified the reliability of the dielectric model and the temperature-frequency equivalence principle of the asphalt mixtures.The results show that the relative dielectric constant of asphalt mixtures increases with the increase of temperature in the temperature range of30−60℃,and the relative dielectric constant of asphalt mixtures decreases with the increase of frequency in the frequency range of1−1000kHz.The dielectric model of asphalt mixture based on temperature and frequency has great applicability,and the goodness of fit R2of the two groups of asphalt mixture samples is above0.95.The goodness of fit R2of the temperature−frequency equivalence principle for two types of asphalt mixtures is all above0.99,which can be used as a theoretical basis for the data unification of non-destructive testing equipment under different temperature and frequency conditions.Key words:asphalt mixture;dielectric properties;dielectric model;temperature;frequency;equivalence principle采用探地雷达等无损检测设备对沥青路面进行无损检测时，是基于某一路段不同位置处沥青路面材料的相对介电常数差异来进行质量评价的[1−2]。

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Conductivity enhancement of poly(3,4-ethylenedioxythiophene)-poly(styrenesulfonate) films post-spincastingAbdiaziz A. Farah, Steven A. Rutledge, Antje Schaarschmidt, Roger Lai, Justin P. Freedman et al. Citation: J. Appl. Phys. 112, 113709 (2012); doi: 10.1063/1.4768265View online: /10.1063/1.4768265View Table of Contents: /resource/1/JAPIAU/v112/i11Published by the American Institute of Physics.Related ArticlesSpace-charge-limited currents in polyimide filmsAppl. Phys. Lett. 101, 242905 (2012)Flexible cobalt-phthalocyanine thin films with high charge carrier mobilityAppl. Phys. Lett. 101, 222102 (2012)Analysis of mobile ionic impurities in polyvinylalcohol thin films by thermal discharge current and dielectric impedance spectroscopyAIP Advances 2, 042152 (2012)Dependence of contact electrification on the magnitude of strain in polymeric materialsJ. Appl. Phys. 112, 084909 (2012)Hole mobility characterization of DNA biopolymer by time-of-flight techniqueAppl. Phys. Lett. 101, 153701 (2012)Additional information on J. Appl. Phys.Journal Homepage: /Journal Information: /about/about_the_journalTop downloads: /features/most_downloadedInformation for Authors: /authorsDownloaded 08 Jan 2013 to 142.150.242.148. Redistribution subject to AIP license or copyright; see /about/rights_and_permissionsConductivity enhancement of poly(3,4-ethylenedioxythiophene)-poly(styrenesulfonate)films post-spincastingAbdiaziz A.Farah,Steven A.Rutledge,Antje Schaarschmidt,Roger Lai,Justin P .Freedman,and Amr S.Helmy a)Edward S.Rogers Sr.Department of Electrical and Computer Engineering,University of Toronto,10Kings College,Toronto,Ontario,Canada M5S 3G4(Received 17September 2012;accepted 1November 2012;published online 7December 2012)Poly(3,4-ethylenedioxythiophene)-poly(styrenesulfonate)(PEDOT:PSS)thin ﬁlms on indium tin oxide and glass substrates have been fabricated and subjected to a non-adiabatic annealing process.The ﬁlms showed subtle changes in their structure and optical properties as well as an increase in conductivity due to the effects of rapid thermal annealing.Through a combination of Raman spectroscopy,X-ray photoelectron spectroscopy and atomic force microscopy studies in conjunction with electrical characterization,and four-point probe measurements,material enrichment of conductive PEDOT domains at the polymer-metal interface have been demonstrated,which wellexplains the surface conductivity improvement of a thin ﬁlm of PEDOT:PSS after annealing.VC 2012American Institute of Physics .[/10.1063/1.4768265]INTRODUCTIONPlastic electronics offers a versatile platform for provid-ing transparent,ﬂexible,large scale circuits.For this to be more commercially viable,the attributes of the existing ele-ments that make up plastic electronics need to be enhanced.Materials’stability is one important example where improvements can be made.Another signiﬁcant example is the electrical transport properties of the organic semicon-ducting materials from which plastic electronics are made.1,2Several organic semiconducting compounds emerged recently with modiﬁed chemical architectures and physical properties that are tailored towards this aim.A great deal of research has been devoted to enhancing organic material transport properties through material processing that enables the optimization of their structural and molecular order.3,4Poly(3,4-ethylenedioxythiophene)-poly(styrenesulfonate)(PEDOT:PSS)has emerged to the forefront of these develop-ments in the last decade due to its promising physical,electrical,and chemical properties.5The advantage of PEDOT:PSS over its counterparts is that it is highly stable,with controllable morphology and relatively high conductiv-ity.As such,PEDOT:PSS has been utilized to enable highly stable optoelectronic devices including light-emitting diodes,solar cells,thin ﬁlms transistors,capacitors,smart windows,and sensors.6As PEDOT:PSS is being utilized in an increas-ing number of applications,more research has been directed towards developing techniques to further improve its attrib-utes without compromising its stability and other beneﬁcial properties.Carrier mobility and the associated layer conduc-tivity are of paramount importance for the aforementioned device applications.The relatively lower carrier mobility in organic materials such as PEDOT:PSS in comparison to inorganic crystalline materials poses stringent limitations on the carrier-photon conversion efﬁciency of organic light emitting devices.7Low mobility also impedes high carrierinjection and hence is partly responsible for making electri-cally pumped organic lasers an untenable aim.As such,sig-niﬁcant effort has been aimed at enhancing semiconductor polymer carrier mobility through the optimization of their structural and molecular order.8One of the techniques that has been previously exploited to improve these properties is thermal annealing in ovens.It has been demonstrated that the crystalline morphology and the orientation of spin cast conjugated polymers ﬁlms could be modestly improved through oven thermal annealing or melt crystallization approaches.9These processes are attractive as they offer a route to control the ﬁlm properties after casting on the substrate.The intra-and intermolecular structure inherent to PEDOT:PSS as well as the associated micro-phase behaviour are some of the chief properties that strongly impact the physical characteristics unique to this class of materials.Changes in this speciﬁc chemical architecture can lead to signiﬁcant variations in the physical properties of resultant structural forms.Modiﬁcations to the chemical architecture and morphology of spin cast PEDOT:PSS has been recently achieved through the use of non-adiabatic thermal process-ing;namely rapid thermal annealing approach (RTA).9Also,improvement to the crystalline morphology of water soluble CdTe polymer encapsulated quantum dots was achieved using the same annealing technique.8RTA is an attractive process,as it offers a route to control and manipulate thin ﬁlm properties after casting on the substrate beyond what is achievable using conventional oven-based annealing.10In this study,we examine the inﬂuence of the RTA annealing temperature on the optical and morphological properties of PEDOT:PSS ﬁlm.The conductivity changes in the annealed ﬁlms were studied using four point probe and transmission line measurements (TLMs),which were performed to ana-lyze the electrical effects of RTA on the sheet resistivity of the spincast ﬁlms on glass substrates.In addition,Raman spectroscopy,X-ray photoelectron spectroscopy (XPS),and atomic force microscopy (AFM)were carried out on thea)a.helmy@utoronto.ca.0021-8979/2012/112(11)/113709/8/$30.00VC 2012American Institute of Physics 112,113709-1JOURNAL OF APPLIED PHYSICS 112,113709(2012)samples undergoing the same annealing conditions.All these techniques shed light on the extent of which the main chain p-conjugation of PEDOT:PSS and structural phase morphol-ogy is directly inﬂuenced by the RTA.The spectroscopic properties of PEDOT:PSS were studied forﬁlms that are spincast on indium tin oxide(ITO)ﬁlms on glass.ITO was chosen due to its high conductivity and transparency over the visible spectrum.Also due to its widespread use as a con-tact layer in various optoelectronic applications including so-lar cell and organic light emitting diodes.11ELECTRICAL PERFORMANCE MODIFICATION WITH ANNEALINGThe inﬂuence of the RTA process on PEDOT:PSSﬁlms wasﬁrst investigated using electrical measurements.Insulat-ing glass substrates wereﬁrst cleaned in a Phantom RIE using oxygen plasma for5min to remove any trace organic mate-rial.For electrical characterization,PEDOT:PSS was spincast on the glass in a single cast at2000RPM for45s,and then soft baked at105 C for5min in ambient air.The resulting PEDOT:PSSﬁlm thickness was measured to be100nm.RTA was subsequently performed in an AnnealSys AS-One system. This system uses incoherent halogen bulbs to heat samples at greatly enhanced rates,as monitored by the system pyrometer. The rapid thermal annealing process investigated for electrical changes involved a temperature ramp rate of25 C/s before a 30s hold time at the maximum temperature in an inert Argon atmosphere.For electrical contacts,200nm of Al was then thermally evaporated directly onto the PEDOT:PSSﬁlm using a shadow mask technique that formed square contact pads with500l m sides at varying distance intervals on the slide for TLM.Electrical characterization of the conductivity of PEDOT:PSSﬁlm were obtained using both an HP4155semi-conductor parametric analyzer and also a4-point probe model 101C from four dimensions.To establish the highest temperature at which a device structure can be annealed,the lowest damage threshold of the material constituents of the structure has to be established. From prior work,it was established that the highest RTA processing temperature for PEDOT:PSS is300 C.Annealing at higher temperatures causes theﬁlm to demonstrate signs of damage.It was further established that of the materials uti-lized in this structure,ITO displayed the lowest damage threshold,which was found to exhibit signs of deterioration in its physical and electrical properties when annealed at temper-atures above200 C.The damage threshold for ITO was determined by analyzing current stability under consecutive biasing.These results can be seen in Figure1,which is a graph of25consecutive voltage sweeps fromÀ5to5V.The samples annealed at250 C and300 C show signiﬁcant varia-tion in conducted current through the ITOﬁlm and the expected linear relationship seen in the unprocessedﬁlm is destroyed as well.To properly adhere to all material con-straints for these and any future devices involving ITO/ PEDOT:PSS interfaces,RTA processing was subsequently limited to200 C.Initially,a linear TLM structure,utilizing thermally evaporated aluminum contacts was tested.The inset in Figure2is a schematic of the linear TLM structure used for analysis,with distances between pads ranging from650to 3550l m.In Figure2,the results of the TLM I-V measure-ments are displayed as a plot of the overall resistance change with respect to length following removing the effects of the contact resistance between the aluminum contacts and the PEDOT-PSSﬁlm.From these results,the reduction in slope, corresponding to a decrease in sheet resistivity of the PEDOT:PSS,with increased annealing temperature can be determined.By performing a linearﬁt to the data,a reduction in slope from0.075X/l m in the unannealed sample to0.054 X/l m in the200 C annealed sample was determined.To fur-ther elucidate and verify these results,4-point probe measure-ments of the PEDOT-PSSﬁlms spun on insulating glass were performed to compare the electrical properties of the as-spun and annealedﬁlms.The measurement results are given in Table I.They demonstrate the systematic reduction of sheet resistivity with increased RTA processing temperature,and a comparison between the unannealed sample and theﬁlm annealed at200 C shows a resistivity drop from7.60to2.54 X/ٗ.The reduction in the sheet resistance with annealing temperature corroborates the TLM results,which indicates that RTA increases the in-plane conductivity of spin cast PEDOT:PSSﬁlms.While RTA was limited to200 C to adhere to ITO constraints,previous spectroscopic results indi-cate that this trend persists up to annealing at300 C.9 In comparison to conventional oven annealing,this is a promising result as the anneal time is only30s at high tem-peratures as opposed to hours,preventing potentially de-structive heating effects,especially at temperatures greater than200 C.12While annealing up to300 C was not per-formed due to adherence with the conductive ITO layer, spectroscopic evidence from previous studies indicate the suitability of RTA for processing at temperatures where con-ventional annealing may cause degradation.PROBING THE ROOT CAUSES BEHINDTHE CONDUCTIVITY ENHANCEMENTTo investigate the root causes behind this sheet conduc-tivity increase,a variety of spectroscopic analyses were per-formed.Raman spectroscopy has been previously used to study doping mechanisms for electrochemically synthesized PEDOTﬁlms.13The Raman spectra of theseﬁlms revealed a signiﬁcant change in the position of C a¼C b stretching bands with various levels of different dopants.It has also been shown that the relative intensity of the symmetric C a¼C b stretching bands associate well with the doping level,and hence provided a valuable means for estimating the doping level of PEDOTﬁlms accurately from Raman spectra.Unlike conventional process monitoring techniques,such mass spec-troscopy,UV-Vis or near-infrared(NIR)spectroscopy,and other chromatography methods,Raman spectroscopy provides high chemical selectivity,requires no additional sample prep-aration procedures and more importantly is non-destructive and not affected by water.For optical characterization,high conductivity grade PEDOT:PSS aqueous dispersion from Sigma-Aldrich was spin coated onto pre-cleaned ITO substrates.The ITO was purchased from Delta Technologies Inc.and had a sheetresistivity in the range of 4-8X /ٗ.Average polymer ﬁlm thickness of 300nm was determined by ellipsometry.RTA was again performed in an AnnealSys AS-One system.The samples for optical analysis were heated in an inert argon atmosphere up to temperatures ranging between 200 C and 280 C with intervals of 20 C for a duration of 300s and with a ramp time of 15s.Raman spectroscopy was used ﬁrst to study the effects of the RTA on the PEDOT:PSS ﬁlms.Raman spectra were obtained using a HR 800Horiba Jobin Yvon with a 632nm excitation wavelength.A Gaussian/Lorentzian ﬁtting routine was applied across the entire spectrum to quantify the peaks.Samples with annealing tem-peratures above 300 C were not studied optically,astheFIG.2.A plot of the PEDOT:PSS sheet resistivity on a glass substrate obtained through I-V measurements on a linear TLM structure to remove the effects of the contact resistance.The distance between the Al contacts was varied from 650to 3550l m.Through a linear ﬁt of the data,the reduction in sheet resistance with increased annealing temperature is evident.The inset is an illustration of the structure fabricated for analysis.TABLE I.4-pt probe measurements of the annealed PEDOT:PSS ﬁlms on glass substrate.Annealing temperature ( C)Sheet Resistivity X /ٗUnannealed 7.60Â100150 3.30Â1002002.54Â10FIG.1.IV curves for ITO layers subjected to various annealing conditions,where the ITO was subjected to rapid thermal annealing at (B)200 C,(C)250 C,(D)300 C as well as no annealing (A).The graphs depict the current response to 25consecutive voltage sweeps from À5to 5V.At higher annealing tempera-tures,the variation in conduction over the 25sweeps due to material degradation is evident.polymer samples were degraded such that no peak assign-ment with any certainty could take place.Unannealed Raman spectrum of the spin coated PEDOT:PSS on ITO is shown in Figure 3(a).In order to achieve better accuracy when assigning the Raman modes,the Raman spectrum of PSS was obtained to serve as a reference.Due to the weak Raman scattering cross section of PSS,it was necessary to spin it on crystalline Si instead of ITO on glass in order to get an intelligible signal.The spectrum is shown in Figure 3(b).As can be seen in the spectrum,the PSS contributes very little to the Raman spectrum obtained from PEDOT:PSS.Raman mode frequencies and intensities for the PEDOT:PSS have been routinely correlated with the optical and electronic structures of poly and oligothiophenes with structures that con-tain p -conjugated backbone.Particularly,Raman modes in the 1100-1700cm À1range for PEDOT are not dispersive as no apparent shift of line positions were observed with the 632nm excitation laser line.14As such,the following bands are mainlyrelated to the PEDOT polymer structure and are strongly visible in the spectra:1563cm À1and 1532cm À1are assigned to the asymmetric C a ¼C b stretching,1421cm À1to symmetric C a ¼C b (ÀO)stretching,1368cm À1to C b -C b stretching,1256cm À1to C a -C a inter-ring stretching,1093cm À1to C-O-C deformation,989cm À1to oxyethylene ring deformation,701cm À1to symmetric C-S-C deformation,577cm À1to oxy-ethylene ring deformation,and 437cm À1to SO 2bending.The peak positions and their assignment are all in good agreement with reported literature data that are consistent with the invari-ant relative peak positions with excitation wavelengths.15,16From the Raman spectra,it was evident that annealed PEDOT-PSS ﬁlms exhibited signiﬁcant modiﬁcation of their electronic and vibrational properties as shown in Figure 3(c),which plots the Raman spectra of the annealed and unan-nealed samples.Notable differences between the Raman modes of the annealed and unannealed ﬁlms are evident in the region between 1100cm À1and 1700cm À1.New peak appearance,peak position shift,and changes in their shape are all observed in both the symmetric and asymmetric C a ¼C b band of the PEDOT.Curve ﬁtting of the C a ¼C b band proﬁles for one of the annealed PEDOT ﬁlms are shown in Figure 4(a).When monitoring the shift oftheseFIG.3.(A)Raman spectra of PEDOT:PSS ﬁlm as-formed ﬁlm.Key modes have been identiﬁed.(B)The Raman spectrum of PSS on a Si substrate.(C)Detailed Raman spectra of PEDOT:PSS ﬁlm having undergone rapid ther-mal annealing at different temperatures ranging from 220 C to 280C.FIG.4.(A)Curve ﬁtting analysis of relevant C a ¼C b stretching vibrations.(B)Relative ratios of relevant integrated intensities of C a ¼C b stretching vibrations from the annealing process in the range of 1100-1700cm À1in comparison to annealing temperature.With increased temperature,a signiﬁcant change in peak ratio can be observed correlating to changes in the PEDOT:PSS structure.modes as a function of annealing,it is found that the sym-metric C a¼C b(ÀO)stretching peak at1421cmÀ1for the unannealed sample shifts to a higher wavenumber and reaches1430cmÀ1for the sample annealed at280 C.Fur-thermore,amongst asymmetric modes,certain peaks become more dominant upon annealing.A new peak appears at 1478cmÀ1while the peak at1496cmÀ1increases its relative intensity until it becomes a distinct band in the sample annealed at280 C.Other noticeable modes also include peaks at1531cmÀ1and1563cmÀ1that are related to asym-metric C a¼C b stretching.15Relative peak intensities of these peaks as shown in Figure4(b)are indicative of the degree of PEDOT polymer chain doping,which monotonically increases with higher annealing temperature while the poly-mer microstructure remains intact.These changes in the band intensity ratio provide evidences that electronic struc-ture of the PEDOT is modiﬁed with RTA and the degree of modiﬁcation varies with annealing temperature.XPS was also used to examine the surface composition proﬁles of PEDOT-PSSﬁlm before and after annealing.For XPS,the samples were analyzed using a Thermo Scientiﬁc Theta Probe XPS spectrometer(ThermoFisher,E.Grinstead, UK).The samples were run in standard mode(i.e.,all angle collected(60 angular acceptance))for the survey spectra and the region spectra.A monochromatic Al K a X-ray source was used,with a spot area of300l m2.Charge compensation was provided utilising the combined eÀ/Arþﬂood gun.Posi-tion of the energy scale was adjusted to place the main C1s feature(C-C)at285.0eV.Peak areas were obtained from spectra run in low resolution mode(pass energy—200eV). Elements of interest(C,S,and O)were also run in high reso-lution mode(30eV pass energy).The instrument and all data processing were performed using the software(AVANTAGE) provided with the instrument.Peak areas,line shapes,and intensities of C1s,O1s,and S2p high resolution core levelspectra were monitored.Observed changes in relative signal ratios were analyzed to deduce,which elements are involved in the species generated.In all spectra reported here,small circles represent the data points whereas the solid lines repre-sentﬁts to the data used for analysis.The peakﬁtting of core level C1s spectra is shown in Figures5(a)and5(b)for the unannealed and the annealed ﬁlm at280 C,respectively.The spectrum for the unannealed ﬁlm displays three components with binding energies at 284.9eV,285.8eV,and286.7eV.This correspond to C-H/ C-C(curve1),C-C-O(curve2),and C-S(curve3)of the PEDOT:PSS,respectively.In comparison to the C1s spectra obtained for the unannealedﬁlms,theﬁlm annealed at 280 C develop some signiﬁcant changes in the C1s spectra, where the high-binding energy side of the main peak repre-senting the C-S and C-C-O exhibit reduction in intensity compared to the original peaks.This is indicative that the composition of the outermost surface of theﬁlm becomes rich in alkyl carbons due to the electronic charge gained by some of these carbon sites.More importantly,any sign of polymer photo thermal degradation, such as oxygen inter-diffusion into the polymer microstruc-ture was not observed by the XPS analysis in any of the ﬁlms.17This suggests that the quality of theﬁlms was maintained upon annealing at the temperatures used,in con-trast to the degradation induced by conventional oven annealing at these temperatures.The S2p core level spectra,as shown in Figures6(a) and6(b),for the unannealed sample and the sample annealed at280 C show,as expected,two signature peaks.Each peak involves contributions from a spin-split doublet,S2p3/2and S2p1/2,with1.2eV energy splitting and1:2intensity ra-tio.18,19The S2p contribution peaks at163.7eV(curve1) and164.9eV(curve2)corresponds to sulfur atoms of the PEDOT and those at higher binding energies at167.7eV (curve3)and168.9eV(curve4)belong to PSS because of the electronegative oxygen attached to sulfur atom in the sul-fonate fragment of the PSS.17As can be seen in Figure6,the intensity of S2p contri-bution from the PEDOT moiety signiﬁcantly increases and that of PSS decreases with increasing the annealing tempera-ture.This increase can be attributed the enhancement of the contribution of the PEDOT component to the signal.This in turn suggests the formation of aﬁlm with a PEDOT-accessible surface as the annealing temperature is increased. Such aﬁnding is remarkable as it is contrary to what is expected for PEDOT:PSS interfaces without anealing.20This can have implications on the control of the qualityof FIG. 5.Deconvolution of C1s core level from the XPS analysis of PEDOT:PSSﬁlm on ITO(A)as-formedﬁlm.(B)280 C thermally annealed ﬁlm.electrical contacts that can be formed on such ﬁlms.Despite of some intensity reduction in the S 2p peaks with annealing neither does the line shape of the S 2p contribution from the PSS changes form nor does the peak position shift to a lower binding energy.Equally signiﬁcant,signs of detachment of sulfonate group from the PSS polymer chain were not observed in the XPS analysis.16This is all indicative of the intact quality of the ﬁlms upon annealing at the temperatures used,which is unique to this annealing technique in compari-son to conventional oven annealing.XPS high resolution spectra for the O 1s deconvolved peaks for unannealed sample are shown in Figures 7(a)and 7(b).The spectra reveal three major components at 531.8eV (curve 1),533.1eV (curve 2),and 534.4eV (curve 3).In both the unannealed and 200 C annealed ﬁlms,the strongest intensities of O 1s peaks are centered at 533.1eV (curve 2)assigned to the (C-O-C)of the PEDOT and 531.8eV (curve 1)corresponding to (O ¼S)in the PSS.21For the 280 C annealed sample as in Figure 7(b),the peaks at 534.9eV (curve 4)and at 531.7eV (curve 1)remain almost invariant.A new peak emerges at 532.6eV (curve 2)while the peak at 533.7eV (curve 3)corresponding to C-O-C bond of the PEDOT increased in intensity.This suggests a modiﬁcation of electron charge distribution along the C-O-C bond of thePEDOT as a result of the annealing process,which sheds light on the mechanisms responsible for the changes in con-duction properties observed from electrical measurements.The interface between the PEDOT:PSS and ITO is also crucial in determining the electrical properties for future de-vice application of these materials.To better understand the nature of ITO/polymer interface and the morphological changes that may occur in the PEDOT:PSS ﬁlms as a result of thermal annealing,AFM images of PEDOT:PSS layer were taken before and after annealing at different tempera-tures.A Nanoscope IIIa AFM (Digital Instrument)was used to analyze the topography and the roughness of the ﬁlms before and after the annealing process.Images were acquired in tapping mode.The measurements were performed in air at 27 C,using a Si cantilever with a spring constant of ca.20-100N/m,a tip radius of 5–10nm,and resonance frequency of about 300KHz.As shown in Figure 8(a),unannealed PEDOT:PSS ﬁlms display smooth bundles of grain-like struc-tures that are attributed to molecularly phase separated PEDOT:PSS chains 19and with rms roughness of 7.20nm.Films annealed at 200 C and 280 C,the rms roughness become 11.50nm and 7.50nm,respectively.The surface roughness increases as the annealing temperature isincreasedFIG. 6.Deconvolution of S 2p core level from the XPS analysis of PEDOT:PSS ﬁlm on ITO (A)as-formed ﬁlm.(B)280 C thermally annealedﬁlm.FIG.7.Deconvolution of O 1s core level from the XPS analysis of PEDOT:PSS ﬁlm on ITO (A)as-formed ﬁlm.(B)280 C thermally annealed ﬁlm.from room temperature to 200 C,but further annealing tem-perature increase to 280 C,the surface becomes less rough compared to the ﬁlms annealed at 200 C.This roughness can be ascribed to the repulsion forces arising from enhanced con-ductivity of the ﬁlms.It is important to note that the PEDOT:PSS ﬁlms annealed at 200 C exhibit a coarse morphology and broad hill-like structures sticking vertically out from the planar ITO substrate as can be seen in Figure 8(b).These hill-like structures are indicative of the formation of PEDOT-rich domains,which are composed of time stable,molecularly doped PEDOT structures that are more readily accessible than those unannealed and annealed at 280 C.Moreover,the resulting spatial separations of the PEDOT-rich domains could diminish their electrostatic interaction with PSS chains.CONCLUSIONIn conclusion,through the application of RTA to thin ﬁlm PEDOT:PSS ﬁlms,the sheet conductivity has been increased by nearly a factor of three,demonstrating the im-portance and potential of RTA for post deposition processing to improve the characteristics of organic thin ﬁlms and devi-ces.The conductivity increase was measured through both TLM measurements and also 4-pt probing.Upon spectro-scopic investigation by Raman spectroscopy,XPS,and AFM,this conductivity enhancement has been attributed to microstructural variations and morphology of PEDOT:PSS ﬁlms.This study has clearly shown that annealing of PEDOT:PSS ﬁlms induces distinctive structural modiﬁca-tions of the PEDOT domains,which upon annealing emerge onto the ﬁlm interface.This can have a signiﬁcant impact on the contacts that can be achieved between this material sys-tem and metals amongst other materials.It also strongly sug-gests the formation of stable doped PEDOT 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