专利实例

电镀铜五则97601碳纤维上电镀铜首先除去碳纤维表面的胶，然后镀覆较氢活泼的金属（Fe或Zn），其厚度≤0．1μm，再电镀或化学镀铜。所镀覆的金属与镀铜液中的H＋离子作用释放出H2，这样，可促使碳纤维在镀液中分散开，从而可以均匀地镀铜。中国专利CN1，094，100（1994－10－26）97602挠性印制线路板电镀铜溶液该镀液含有硫酸铜60，～100g／L；硫酸170～220g／L（二者做为主要成分）。此外还加入羟基羧酸如柠檬酸（其与硫酸铜的摩尔比≥0．5），氯离子10～1000mg／L以及硫脲或其衍生物（如乙酰硫脲或1，3-二乙基硫脲）。电沉积铜层的应…     

乙醛酸化学镀铜工艺

研究了以乙醛酸为还原剂的化学镀铜工艺、镀层结构和形貌。其镀液组成和操作条件为:28.0 g/L CuSO4.5H2O,44.0 g/L EDTA-2Na,10.0 mg/Lα,α’-联吡啶,10.0 mg/L亚铁氰化钾,9.2 g/L乙醛酸,pH为11.5～12.5,θ为40～50℃。实验结果表明,化学镀铜溶液较稳定;镀液温度和硫酸铜质量浓度提高,铜沉积速率增大;较高的镀液温度下,化学镀铜反应的活化能较低,镀液稳定性下降;镀液pH在11.5～12.5可获得较好的铜镀层;随乙醛酸和络合剂质量浓度提高,铜沉积速率变化不大,但过量的乙醛酸导致镀液的稳定性降低;铜镀层为面心立方混晶结构,呈光亮的粉红色块状形貌,有较高的韧性。     

专利实例

一种化学镀铜方法;化学镀金溶液;一种镀金溶液;金-镍基非晶态合金镀层;电镀用铜阳极铜球的制造方法;电镀锡-银-铜三元合金;一种电镀锡合金电解液;酸性锡-铟合金电镀液;无铅的锡-银合金或锡-铜合金镀液;防止阳极置换反应的锡合金镀液;铝件经电镀锌互相连接;镍-钨-磷基合金电镀液;电镀镍-锡合金镀层。     

半导体硅表面化学镀铜

介绍了以次磷酸钠为还原剂、硫酸镍为再活化剂的半导体N型硅表面化学镀铜工艺及其前处理。探讨了镀液中铜盐含量、还原剂含量、pH及温度对沉积速率的影响。确定了化学镀铜最佳工艺条件:0.15 mol/L CuSO4.5H2O,0.03 mol/LN iSO4.6H2O,0.75 mol/L NaH2PO2.H2O,0.08 mol/LNa3C6H5O7.H2O,0.5 mol/L H3BO3,<0.2 mg/L硫脲,60~65℃,pH 12.0~12.5。采用扫描电镜及能谱仪分别对镀覆30 m in及40 m in制得的2种镀层表面形貌及成分进行了分析与比较。结果表明,镀覆30 m in镀层组织较为致密,而镀覆40 m in的镀层组织较粗糙;随镀覆时间的延长,镀层中铜含量明显提高。该镀层接触电阻基本能满足微制冷器的要求。     

ABS塑料表面无钯活化化学镀铜

以20 g/L硫酸铜(CuSO_4)溶液为预活化液、50 g/L次亚磷酸钠(NaH_2PO_2)酸性溶液为活化液,在高温条件下直接还原吸附在丙烯腈-丁二烯-苯乙烯(ABS)塑料上的铜离子形成活化中心,实现了ABS塑料表面无钯活化化学镀铜。通过单因素分析法研究了基体预活化时间、活化液p H值、活化温度及时间对基体镀层覆盖率的影响。采用扫描电镜与能谱仪对活化后基体的表面形貌和元素成分进行分析,利用X射线衍射仪分析了镀层结构,并通过高低温冲击法对镀层结合性进行评价。结果表明,当预活化时间为20 min,活化液p H值为3,活化温度为70℃,活化时间为10 min时,活化效果最佳;活化后,基体表面生成大量胞状铜微粒,对化学镀铜具有较强的催化作用;施镀后,镀层结构均匀致密,覆盖率为100%,结合性良好。     

Cu2＋、Zn2＋对玻璃弹簧负载型P／TiO2光催化还原Cr（Ⅵ）的影响研究

金属铬[Cr（Ⅵ）]是一种很常见的重金属污染物,在电镀、冶金、化工等一些加工行业废水中含量很大。Cr（Ⅵ）具有很强的致癌性和毒性,消除水体中Cr（Ⅵ）污染的研究具有重要的意义。本实验在低温条件下用双氧水制备了P／TiO2溶胶,并将其负载于玻璃弹簧上,形成负载型P／TiO2光催化剂。在紫外光照下,该催化剂光催化还原Cu2＋和Cr（Ⅵ）共存溶液或Zn2＋和Cr（Ⅵ）共存溶液中的Cr（V1）时,随着Cu2＋或Zn2＋浓度的增大Cr（Ⅵ）的还原率先增加后下降;在Cu2＋浓度为O．004mol／L时或Zn2＋浓度为O．0025mol／L时,Cr（VI）的还原率最高。     

SiC粉体化学镀铜工艺研究

介绍了SiC粉体的敏化、活化及其碱性化学镀铜的工艺配方。分别对镀液稳定性的影响因素和各工艺条件对镀速的影响进行了研究。结果表明,SiC粉体颗粒越细、镀液pH增大、温度升高,都容易导致镀液分解;增加甲醛含量,可以提高镀速,但是镀液稳定性下降;适宜的络合剂,可以提高镀层质量,保持镀液稳定,但络合剂含量增加,镀速降低。得出了最佳的工艺条件：φ（甲醛）10～20mL／L,ρ（络合剂）50～70g/L,温度15～35℃,pH12．5～13。碱性化学镀铜后的SiC-Cu复合粉体及其于1050℃热处理后的X-射线衍射分析表明,镀层中含Cu、SiC和Cu2O,且Cu呈结晶态;铜镀层在高温下与SiC粉体能够较好共存,无脱落现象。扫描电镜照片显示,SiC-Cu复合粉体分散性良好,镀层表面平滑、均匀,并有细小的金属胞状颗粒随机堆积而成。     

添加剂对无氰电镀铜-锡合金(低锡)镀层性能的影响

通过赫尔槽试验与直流电解试验,研究了添加剂在焦磷酸盐溶液体系无氰电镀铜-锡合金(低锡)工艺中的作用。该体系镀液组成与工艺条件为:Cu2P2O7·3H2O25g/L,Sn2P2O71.0g/L,K4P2O7·3H2O250g/L,K2HPO4·3H2O60g/L,温度25℃,pH8.5,电流密度1.0A/dm2。采用扫描电镜(SEM)、X射线衍射(XRD)、能谱(EDS)、中性盐雾试验等方法研究了添加剂对镀层组成结构、外观、耐腐蚀性能及微观形貌的影响。结果表明,焦磷酸盐溶液体系无氰电镀铜-锡合金(低锡)时使用有机胺类添加剂可抑制Sn的析出,使合金镀层致密均匀,耐蚀性能好。镀层结晶主要为Cu13.7Sn结构,镀层中Sn含量为9%～11%。镀液中添加剂的使用量增加,则合金镀层中的Sn含量降低。     

Ni-P/n-Al2 O3 化学复合镀镀液及工艺研究

以电位和镀速为评价指标,通过正交实验和单因素实验,确定了Ni-P／n-Al2O3化学复合镀的最佳工艺配方为：温度85～95℃,气体搅拌,pH值为4．5～5。所得镀液的最佳组成为：ρ（次亚磷酸钠）为21g/L,ρ（柠檬酸钠）为14g/L,ρ（苹果酸）12g/L,ρ（添加剂丁二酸）5g/L,ρ（氧化铝）8g/L,通过级差分析得到镀液配方中各因素对镀层耐蚀性能的影响次序为：柠檬酸〉次磷酸酸钠〉纳米氧化铝〉添加剂〉苹果酸。扫描电镜研宄表明,镀层均匀致密,为明显的胞状物;X-射线衍射实验证实,复合镀层的结构为非晶态。与Ni-P镀层相比,Ni-P／n-Al2O3化学复合镀镀层在质量分数分别为3．5％的氯化钠、10％的稀盐酸和10％的稀硫酸溶液中的耐蚀性能有了明显的提高。     

镀铜液及电镀方法

介绍了一种酸性镀铜液和电镀方法。酸性镀铜液包含铜离子、有机酸或无机酸、氯离子、控制电沉积反应的高分子表面活性剂和促进镀速的含硫的饱和有机化合物。其中,高分子表面活性剂含有两个或两个以上不同的疏水性基团。该方法主要是在一部分凹凸结构的半导体材料上进行电镀,并获得镀层的方法。该方法包含了对导体层提供一个阴极电位和与阳极电连接的镀液,溶液中含25-75g／L铜离子和0．4mol／L有机酸或无机酸,并在导体层和阳极之间放置一个电阻。同时,     

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.