CN109082652A - 一种非导电基体表面非晶态合金导电层制备技术 - Google Patents
一种非导电基体表面非晶态合金导电层制备技术 Download PDFInfo
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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Abstract
本发明提供了一种非导电基体表面非晶态合金的导电层制备技术,即用化学镀法在非导电基体表面制备Pd‑Ni‑P三元非晶合金薄膜,包括:1)将非导电基体表面进行前处理,2)将基体浸入Pd‑Ni‑P化学镀液进行化学镀。化学镀液的成分包括Pd(OAc)2溶液、NiSO4溶液、还原剂NaH2PO2、稳定剂等。用化学镀法制备的Pd‑Ni‑P三元非晶合金薄膜具有优异的三维成型能力、抗化学腐蚀性能和机械性能。本发明实用性广,操作方便,可在复杂表面形成厚度均匀、强度较高,又具有显著防腐性能的膜,尤其适用致密基体,如陶瓷、玻璃、塑料等。
Description
技术领域
本发明涉及一种新的Pd-Ni-P化学镀液,用于非导电基体化学镀,以得到厚度均匀、强度较高,又具有显著防腐性能的金属镀层。
背景技术
腐蚀在各个领域都会发生,在被腐蚀的过程中,材料的结构和性能会发生巨大变化,使得材料失效,容易造成巨大的财产损失。非晶合金涂层由于其独特的结构,相比晶态合金具有更为优良的力学性能和耐腐蚀性能,具有重要的应用价值和经济效益。
非晶合金涂层由于在制备的过程中,对工艺和设备的要求高以及工艺复杂等因素,很难获得多种尺寸以及多种成分的非晶合金。常规的制备方法主要有快速冷却、气相沉积法、固体反应,但是生产效率低,局限性大。
熔体水淬法操作简便,冷却速度快,但由于石英管可能与母材发生反应,会影响母合金的非晶形成能力;熔滴喷溅法会使一些无法通过熔体急冷得到非晶的合金得到非晶合金,但沉积条件要求较高,容易受到环境因素影响,制备速度很慢;铜模吸铸法铜模的冷却速率会很快降低,所以不能制备大体积的块体非晶。
化学镀法是利用目标合金的金属盐及相应比例的稳定剂制成溶液,并加入适量还原剂使金属离子沉积或结晶在基体上的一种方法。由其制备的非晶合金薄膜厚度均匀、强度较高、耐腐蚀性好。
相对于二元体系,三组分非晶合金薄膜具有更高的耐腐蚀性和耐磨性,其薄膜厚度可达几个甚至几十微米。该发明制备的Pd-Ni-P三元非晶合金薄膜三维成型能力、腐蚀性能和机械性能优良。
发明内容
本发明的目的在于提供一种非导电基体表面非晶态合金导电层制备技术。
本研究中的化学镀的工艺流程如下:
(1)打磨。
(2)有机溶剂除油。有机溶剂有利于除去不可皂化油,本发明采用的是分析纯无水乙醇。
(3)化学除油。化学除油通过皂化的方法除去试样表面的油脂,其效率较高,本发明采用的除油工艺条件为:NaOH 45-50g/L,Na3PO4·12H2O 35-40g/L,Na2CO3 35-40g/L,乳化剂OP-10 1-2ml/L。
(4)酸洗活化。采用70℃的20%-40%(体积分数)的H2SO4进行活化。
(5)前处理之后立即将基体浸入化学镀液,化学镀钯液的成分包括主盐,络合剂,稳定剂,还原剂等。本发明所用主盐为Pd(OAc)2,加入氨水与之形成能溶于水的钯的络合物,同时氨水还起到调节pH值的作用。选用的还原剂是次亚磷酸钠,此外还加入了稳定剂,化学镀液的具体成分及工艺如下:
1)Pd(OAc)2溶液的制备:称取一定量的Pd(OAc)2溶于盐酸溶液中,配比为 Pd(OAc)2:HCl=1g:25-30mL,待Pd(OAc)2完全溶于盐酸溶液中后,再在溶液中缓慢加入氨水(25-30mL),边加边震荡,使溶液呈现透明粉红色时,停止加氨水,静止直至溶液完全无色透明。
2)NiSO4溶液的制备:依次将药品HBO3 45-50g/L,NiSO4·6H2O 45-50g/L,Na3C6H5O7·2H2O 45-50g/L,NH4Cl 35-37.5g/L,(NH4)2SO4 35-37.5g/L溶于40ml 60℃去离子水中,待溶质完全溶于水中,自然冷却。
3)NaH2PO2溶液的制备:称取2.5-3g的NaH2PO2溶于50ml去离子水中。
(6)制备过程
制备100mL化学镀液:将制备好的Pd(OAc)2溶液和40mL NiSO4溶液混合于烧杯中,用氢氧化钠调pH至5-6,至于40-45℃水浴锅中,待溶液温度上升至40-45℃后,量取50mLNaH2PO2溶液倒入前面的溶液中,若总溶液不足100mL,则加入去离子水补足100mL,再放入制备好的基体,实验条件为沉积温度40-45℃,pH至5-6,沉积时间30-50min。使其反应,待溶液颜色变深,此时取出硅基体,用去离子水冲洗基体表面,冷风干燥。
本发明实用性广,操作方便,可在复杂表面形成厚度均匀、强度较高,又具有显著防腐性能的膜,尤其适用致密基体,如陶瓷、玻璃、塑料等。
附图说明
图1.实施例1的镀液中0.08g Pd(OAc)2时的Pd-Ni-P非晶合金薄膜的表面微观形貌图
图2.实施例2的镀液中0.12g Pd(OAc)2时的Pd-Ni-P非晶合金薄膜的表面微观形貌图
图3.实施例3的镀液中0.16g Pd(OAc)2时的Pd-Ni-P非晶合金薄膜的表面微观形貌图
图4.实施例4的镀液中0.20g Pd(OAc)2时的Pd-Ni-P非晶合金薄膜的表面微观形貌图
具体实施方式
下面通过实施例对本发明做进一步说明,其目的仅在于更好地理解本发明的内容而非限制本发明的保护范围。
实施例1
制备100mL化学镀液:称取0.08g Pd(OAc)2溶于2mL盐酸溶液中,待Pd(OAc)2完全溶于盐酸溶液中后,再在溶液中缓慢加入2mL氨水,边加边震荡,使溶液呈现透明粉红色时,停止加氨水,静止直至溶液完全无色透明,备用。
将制备好的Pd(OAc)2溶液和40mL NiSO4溶液混合于烧杯中,用氢氧化钠调pH至6,至于40℃水浴锅中,待溶液温度上升至40℃后,量取50mL NaH2PO2溶液倒入前面的溶液中,若总溶液不足100mL,则加入去离子水补足100mL,再放入制备好的基体,使其反应,实验条件为沉积温度40℃,pH至6,沉积时间30min。待溶液颜色变深,此时取出基体,用去离子水冲洗基体表面,冷风干燥。
实施例2
制备100mL化学镀液:称取0.12g Pd(OAc)2溶于3.5mL盐酸溶液中,待Pd(OAc)2完全溶于盐酸溶液中后,再在溶液中缓慢加入3.5mL氨水,边加边震荡,使溶液呈现透明粉红色时,停止加氨水,静止直至溶液完全无色透明,备用。
将制备好的Pd(OAc)2溶液和40mL NiSO4溶液混合于烧杯中,用氢氧化钠调pH至6,至于40℃水浴锅中,待溶液温度上升至40℃后,量取50mL NaH2PO2溶液倒入前面的溶液中,若总溶液不足100mL,则加入去离子水补足100mL,再放入制备好的基体,使其反应,实验条件为沉积温度40℃,pH至6,沉积时间45min。待溶液颜色变深,此时取出基体,用去离子水冲洗基体表面,冷风干燥。
实施例3
制备100mL化学镀液:称取0.16g Pd(OAc)2溶于4mL盐酸溶液中,待Pd(OAc)2完全溶于盐酸溶液中后,再在溶液中缓慢加入4mL氨水,边加边震荡,使溶液呈现透明粉红色时,停止加氨水,静止直至溶液完全无色透明,备用。
将制备好的Pd(OAc)2溶液和40mL NiSO4溶液混合于烧杯中,用氢氧化钠调pH至5,至于40℃水浴锅中,待溶液温度上升至40℃后,量取50mL NaH2PO2溶液倒入前面的溶液中,若总溶液不足100mL,则加入去离子水补足100mL,再放入制备好的基体,使其反应,实验条件为沉积温度40℃,pH至5,沉积时间30min。待溶液颜色变深,此时取出基体,用去离子水冲洗基体表面,冷风干燥。
实施例4
制备100mL化学镀液:称取0.20g Pd(OAc)2溶于5.5mL盐酸溶液中,待Pd(OAc)2完全溶于盐酸溶液中后,再在溶液中缓慢加入5.5mL氨水,边加边震荡,使溶液呈现透明粉红色时,停止加氨水,静止直至溶液完全无色透明,备用。
将制备好的Pd(OAc)2溶液和40mL NiSO4溶液混合于烧杯中,用氢氧化钠调pH至6,至于45℃水浴锅中,待溶液温度上升至45℃后,量取50mL NaH2PO2溶液倒入前面的溶液中,若总溶液不足100mL,则加入去离子水补足100mL,再放入制备好的基体,使其反应,实验条件为沉积温度45℃,pH至6,沉积时间30min。待溶液颜色变深,此时取出基体,用去离子水冲洗基体表面,冷风干燥。
Claims (8)
1.一种非导电基体表面非晶态合金的导电薄膜制备技术,其特征在于,按照质量百分比薄膜的组成为Pd:Ni:P=1-1.8%:36-36.5%:62-65%,Pd含量为13.0-17.0at.%。
2.根据权利要求1所述的工艺,其特征在于化学镀方法采用Pd-Ni-P化学镀液,镀液的配制为:将制备好的钯盐和镍盐混合于烧杯中,pH调至5-6,溶液温度上升至40-45℃后,加入还原剂。
3.根据权利要求1所述的工艺,其特征在于基体表面的前处理,包括以下步骤:打磨,有机溶剂除油,化学除油,热水清洗,酸洗活化,冷水清洗。
4.根据权利要求1所述的工艺,其特征在于化学镀的沉积温度为40-45℃,pH为5-6。
5.根据权利要求2所述的工艺,其特征在于所述的钯盐为硝酸钯;称取Pd(OAc)2溶于盐酸溶液中,配比为Pd(OAc)2:HCl=1g:25-30mL,待Pd(OAc)2完全溶于盐酸溶液中后,再在溶液中缓慢加入氨水25-30mL。
6.根据权利要求2所述的工艺,其特征在于所述的镍盐为NiSO4溶液,依次将HBO3 45-50g/L,NiSO4·6H2O 45-50g/L,Na3C6H5O7·2H2O 45-50g/L,NH4Cl 35-37.5g/L,(NH4)2SO435-37.5g/L溶于60℃去离子水中。
7.根据权利要求2所述的工艺,其特征在于所述的还原剂为次磷酸钠。
8.根据权利要求1所述的工艺,其特征在于实用性广,操作方便,可在复杂表面形成厚度均匀、强度较高,又具有显著防腐性能的膜,适合化学镀导电膜层的工艺。
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CN101418440A (zh) * | 2008-12-15 | 2009-04-29 | 南京工业大学 | 一种在多孔基体上化学镀制备金属膜的方法 |
CN106944154A (zh) * | 2017-03-19 | 2017-07-14 | 西南石油大学 | 三元非晶合金修饰纤维素/钛酸锶复合光催化剂的制备方法及其在光分解水制氢中的应用 |
CN107376962A (zh) * | 2017-03-19 | 2017-11-24 | 西南石油大学 | 三元非晶合金/二氧化钛纳米复合催化剂材料的制备及其在光解水制氢中的应用 |
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CN101418440A (zh) * | 2008-12-15 | 2009-04-29 | 南京工业大学 | 一种在多孔基体上化学镀制备金属膜的方法 |
CN106944154A (zh) * | 2017-03-19 | 2017-07-14 | 西南石油大学 | 三元非晶合金修饰纤维素/钛酸锶复合光催化剂的制备方法及其在光分解水制氢中的应用 |
CN107376962A (zh) * | 2017-03-19 | 2017-11-24 | 西南石油大学 | 三元非晶合金/二氧化钛纳米复合催化剂材料的制备及其在光解水制氢中的应用 |
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