化学溶液沉积法制备Bi4Ti3O12铁电薄膜及其性质的研究

报道了用化学溶液沉积法采用价格低廉的原料在电阻率为6～9Ω·cm的n型Si(100)衬底上生长Bi4Ti3O12铁电薄膜,并对薄膜的性质进行了研究。结果表明此制膜工艺简单,成本低,制备的Bi4Ti3O12铁电薄膜具有较低的结晶温度,且薄膜均匀,致密,无裂纹。在650℃下退火30min时得到的Bi4Ti3O12铁电薄膜具有良好的绝缘性和铁电性,薄膜的剩余极化Pr＝4.9μC/cm2,矫顽电场Ec＝87kV/cm。     

La/Nb掺杂对Bi_4Ti_3O_(12)薄膜铁电性能和疲劳特性的影响

采用溶胶–凝胶工艺(sol–gel)在Pt/Ti/SiO2/p-Si衬底上分别制备Bi4–xLaxTi3O12和Bi4Ti3–yNbyO12铁电薄膜,研究La/Nb掺杂对Bi4Ti3O12薄膜铁电性能和疲劳特性的影响。结果表明:La/Nb掺杂均能有效改善Bi4Ti3O12薄膜的铁电性能和疲劳特性。当La摩尔(下同)掺量在0.5～0.75时,La掺杂对Bi4Ti3O12薄膜的性能改善作用最好,而且在明显提高薄膜铁电性能的同时,对薄膜疲劳特性的改善更加显著,薄膜经1010极化反转后,其剩余极化强度(Pr)仅下降5.1%。Nb掺杂对提高薄膜铁电性能的作用更加明显,Nb掺量为0.06时,Bi4Ti3–yNbyO12薄膜的Pr高达18.7μC/cm2,但Nb掺量不宜过多,当Nb掺量超过0.06以后,薄膜的铁电性能和疲劳特性均反而有所下降。     

A位掺杂Bi_4Ti_3O_(12)薄膜的制备及铁电性能研究

采用溶胶-凝胶法制A位掺杂Bi4Ti3O12(BTO)的铁电薄膜Bi3.25La0.75Ti3O12(BLT)、Bi3.15Nd0.85Ti3O12(BNT)及Bi3.15(La0.5Nd0.5)0.85Ti3O12(BLNT);XRD结果表明制备的薄膜具有(117)和(00l)的混合取向;在10V电压下,BLT、BLNT和BNT薄膜的Pr分别为13.14μC/cm2、20.65μC/cm2和21.23μC/cm2;FE-SEM显示BNT薄膜表面光滑致密,颗粒均匀,薄膜厚度约为300nm。     

Li_(1-x)Bi_(4+x)Ti_4O_(15)薄膜制备与表征

在LiNO_3/SiO_2/Si基板上制备了Li_(1-x)Bi_(4+x)Ti_4O_(15)系列薄膜(x=0.3、0.4、0.5、0.6),并系统分析了这些薄膜的微观结构以及铁电、介电及漏电等电学特性。研究结果表明,在氮气气氛中以600℃持温30 min制备的单一相薄膜中Li0.5Bi4.5Ti4O15薄膜的结晶效果最好,且在其表面可成长出独立晶粒分布状态;x为0.5时薄膜的剩余极化强度2Pr=53.5μC/cm2、矫顽场2Ec=144.2 k V/cm,此时薄膜的铁电性能相对最佳;该系列薄膜的介电常数介于37~100,介电损失相对偏高,介于0.7~1.0;所有薄膜的漏电流均随外加电压的增加而逐渐增大,其中Li0.5Bi4.5Ti4O15薄膜漏电流最小,外加电压为10 V时其值约为3.88×10-6A。     

Nd和Mg共掺杂钛酸铋铁电薄膜的电性能研究

利用化学溶液沉积法在Pt/Ti/Si O2/Si(100)基底和700℃条件下分别制备了Nd和Mg(不同浓度)共掺杂的钛酸铋薄膜Bi3.15Nd0.85Ti(3-x)Mg2xO12(BNTM)(x=0.00,0.06,0.10和0.14),并进行了这一系列薄膜的包括微结构、介电、铁电和漏电流等特性的研究和对比。发现当Mg含量为x=0.10时,薄膜具有较高的剩余极化强度(2Pr=33.40μC/cm2)和介电常数(ε=538,频率为1k Hz),其漏电流密度为10-8A/cm2。讨论了相关的物理机制。     

溶胶-凝胶法制备掺钙钛酸锶铋铁电薄膜

利用溶胶-凝胶法在Pt/Ti/SiO2/Si衬底上制备了CaxSr1-xBi4Ti4O15(CxS1-xBT,x=0～1)铁电薄膜.研究了不同Ca2取代量对薄膜的微观结构、取向生长、铁电性能以及介电性能的影响.结果表明:当Ca2 取代量为x=0.4时,C0.4S0.6BT铁电薄膜样品在一定程度上沿a轴择优取向;样品致密性较好,晶粒呈球型,且大小均匀,尺寸约为100nm.C0.4S0.6BT薄膜的剩余极化强度为8.37μC/cm2,矫顽场强为72kWcm;在1 Hz～1 MHz频率范围内,相对介电常数为234～219,介电损耗为0.009～0.073.     

钽镁酸钡缓冲层对锆钛酸铅铁电薄膜性能的影响

采用溶胶–凝胶工艺在Pt/Ti/Si O2/Si基片上,通过引入钽镁酸钡[Ba(Mg1/3Ta2/3)O3,BMT]缓冲层,制备了锆钛酸铅[Pb(Zr0.52Ti0.48)O3,PZT]铁电薄膜。研究了BMT缓冲层对PZT铁电薄膜结晶和性能的影响。结果表明:引入BMT缓冲层利于PZT薄膜的生长;PZT薄膜具有钙钛矿结构,且没有裂纹、结晶良好、致密性好;缓冲层的厚度对PZT铁电薄膜的微观结构和铁电性能有重要影响。随BMT缓冲层厚度增加,PZT晶粒增大,介电损耗tanδ逐渐减少,介电常数εr和剩余极化强度Pr先增大后减少,矫顽场Ec先减少后增大。当BMT缓冲层厚约为10 nm时,PZT薄膜具有最优的铁电性能:εr=1 850,Pr=20.2μC/cm2,Ec=43.9 k V/mm。这与BMT与PZT具有相似的晶格常数、较小的晶格失配度和相近的禁带宽度有关。     

热处理工艺对钙锶铋钛铁电薄膜性能的影响

用溶胶-凝胶法和快速退火技术在带白金电极和钛过渡层的硅片(Pt/Ti/SiO2/Si)上制备了钙锶铋钛(Ca0.4Sr0.6Bi4Ti4O15,CsBT-0.4)铁电薄膜.结果表明:退火温度及保温时间对CSBT-0.4铁电薄膜的微观结构、晶粒取向以及铁电性能的影响较大.x射线衍射谱表明:退火温度为750℃、保温时间为5min,得到的CsBT-0.4铁电薄膜样品的晶粒大小较均匀且致密性好,而且晶粒以a轴取向的球状晶粒为主,剩余极化强度(2Pr)和矫顽场(2Ec)分别为16.2 μC/cm2和130kV/cm.     

射频磁控溅射制备PZT铁电薄膜的工艺研究

在SiO2/Si基片上采用直流对靶溅射技术制备出Pt/Ti底电极;应用射频磁控溅射方法,利用快速热处理(RTA)工艺,制备出了具有良好铁电性能的Pb(Zr0.52Ti0.48)O3铁电薄膜.将样品进行10min快速热退火处理,退火温度700℃.测试分析表明:薄膜厚度比较均匀、表面基本平整、没有裂纹和孔洞、致密性好、薄膜样品的矫顽场强(Ec)为28.6kV/cm,剩余极化强度(Pr)为18.7μC/cm2,自发极化强度(Ps)为37.5μC/cm2,是制备铁电薄膜存储器的优选材料.     

一种压电陶瓷降压变压器材料的研究

研制了一种新型的添加CaCO3,Bi(Cd1/2Ti1/2)O3,MnO2的改性PbTiO3压电陶瓷材料.从压电活性、压电各向异性、介电常数、介电损耗、机械品质因数及Curie点等综合参数看,该材料可用来开发压电陶瓷降压变压器.实验确定其典型配方为Pb0.73Ca0.27TiO3+4%(in mole)Bi(Cd1/2Ti1/2)O3+1%(in mole)MnO2;在优化后的制备工艺条件下,其主要参数为:εT33/ε0=187,d33=60×10-12 C.N-1,Kt=0.49,Kp=0.052,Qm=560,tan δ=0.7%,θC=317 ℃.     

Insect antifeedant properties of anthranoids from the genusVismia

Vismiones and ferruginins, representatives of a new class of lypophilic anthranoids from the genusVismia were found to inhibit feeding in larvae of species ofSpodoptera, Heliothis, and inLocusta migratoria.     

Direct observation of freeze-thaw instability of latex coatings via high pressure freezing and cryogenic SEM

Despite its industrial importance, the subject of freeze-thaw (F/T) stability of latex coatings has not been studied extensively. There is also a lack of fundamental understanding about the process and the mechanisms through which a coating becomes destabilized. High pressure (2100 bar) freezing fixes the state of water-suspended particles of polymer binder and inorganic pigments without the growth of ice crystals during freezing that produce artifacts in direct imaging scanning electron microscopy (SEM) of fracture surfaces of frozen coatings. We show that by incorporating copolymerizable functional monomers, it is possible to achieve F/T stability in polymer latexes and in low-VOC paints, as judged by the microstructures revealed by the cryogenic SEM technique. Particle coalescence as well as pigment segregation in F/T unstable systems are visualized. In order to achieve F/T stability in paints, latex particles must not flocculate and should provide protection to inorganic pigment and extender particles. Because of the unique capabilities of the cryogenic SEM, we are able to separate the effects of freezing and thawing, and study the influence of the rate of freezing and thawing on F/T stability. Destabilization can be caused by either freezing or thawing. A slow freezing process is more detrimental to F/T stability than a fast freezing process; the latter actually preserves suspension stability during freezing. Presented at the 82nd Annual Meeting of the Federation of Societies for Coatings Technology, October 27–29, 2004 in Chicago, IL. Tied for first place in The John A. Gordon Best Paper Competition.     

Ethanol and (−)-α-Pinene: Attractant Kairomones for Bark and Ambrosia Beetles in the Southeastern US

In 2002–2004, we examined the flight responses of 49 species of native and exotic bark and ambrosia beetles (Coleoptera: Scolytidae and Platypodidae) to traps baited with ethanol and/or (−)-α-pinene in the southeastern US. Eight field trials were conducted in mature pine stands in Alabama, Florida, Georgia, North Carolina, and South Carolina. Funnel traps baited with ethanol lures (release rate, about 0.6 g/day at 25–28°C) were attractive to ten species of ambrosia beetles (Ambrosiodmus tachygraphus, Anisandrus sayi, Dryoxylon onoharaensum, Monarthrum mali, Xyleborinus saxesenii, Xyleborus affinis, Xyleborus ferrugineus, Xylosandrus compactus, Xylosandrus crassiusculus, and Xylosandrus germanus) and two species of bark beetles (Cryptocarenus heveae and Hypothenemus sp.). Traps baited with (−)-α-pinene lures (release rate, 2–6 g/day at 25–28°C) were attractive to five bark beetle species (Dendroctonus terebrans, Hylastes porculus, Hylastes salebrosus, Hylastes tenuis, and Ips grandicollis) and one platypodid ambrosia beetle species (Myoplatypus flavicornis). Ethanol enhanced responses of some species (Xyleborus pubescens, H. porculus, H. salebrosus, H. tenuis, and Pityophthorus cariniceps) to traps baited with (−)-α-pinene in some locations. (−)-α-Pinene interrupted the response of some ambrosia beetle species to traps baited with ethanol, but only the response of D. onoharaensum was interrupted consistently at most locations. Of 23 species of ambrosia beetles captured in our field trials, nine were exotic and accounted for 70–97% of total catches of ambrosia beetles. Our results provide support for the continued use of separate traps baited with ethanol alone and ethanol with (−)-α-pinene to detect and monitor common bark and ambrosia beetles from the southeastern region of the US.     

Novel polyurethane coating technology through glycidyl carbamate chemistry

Glycidyl carbamate chemistry combines the excellent properties of polyurethanes with the crosslinking chemistry of epoxy resins. Glycidyl carbamate functional oligomers were synthesized by the reaction of polyfunctional isocyanate oligomers and glycidol. The oligomers were formulated into coatings with several amine functional crosslinkers at varying stoichiometric ratios and cured at different temperatures. Properties such as solvent resistance, hardness, and impact resistance were dependent on the composition and cure conditions. Most coatings had an excellent combination of properties. Studies were carried out to determine the kinetics of the curing reaction of the glycidyl carbamate functional oligomers with multifunctional and model amines. Detailed kinetic analysis of the curing reactions was also undertaken. The results indicated that the glycidyl carbamate functional group is more reactive than a glycidyl ether group. Presented at the 82nd Annual Meeting of the Federation of Societies for Coatings Technology, on October 27–29, 2004, in Chicago, IL.     

Highly moisture-proof polysilsesquioxane coating prepared via facile sol-gel process

A highly moisture-proof polysilsesquioxane coating was obtained from a new bis-silylated precursor, which was synthesized from 3-aminopropyltriethoxysilane (APTES) and m-xylylene diisocyanate (m-XDI) in tetrahydrofuran (THF) and verified by ¹H MAS NMR. For direct comparison purposes, an SiO₂ coating was also prepared by the Stöber method using tetraethoxysilane (TEOS) as the reactant. Interestingly, the coating obtained from the polysilsesquioxane sol exhibited a much higher moisture resistance capability than its counterpart, which was attributed to its more compact feature between nanoparticles as characterized by N₂ absorption experiment and transmission electron microscopy (TEM). Furthermore, its high transparency of about 92% showed potential for application in the protection of optical crystals.