CN105803433A - 一种氧化铝陶瓷表面无钯活化化学镀镍工艺 - Google Patents
一种氧化铝陶瓷表面无钯活化化学镀镍工艺 Download PDFInfo
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- 238000005516 engineering process Methods 0.000 title claims abstract description 21
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title abstract 8
- 239000011224 oxide ceramic Substances 0.000 title abstract 3
- 229910052574 oxide ceramic Inorganic materials 0.000 title abstract 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 116
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 58
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 23
- 239000000758 substrate Substances 0.000 claims abstract description 20
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 16
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 16
- 239000000084 colloidal system Substances 0.000 claims abstract description 15
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 8
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- 238000002156 mixing Methods 0.000 claims abstract description 3
- 238000007788 roughening Methods 0.000 claims abstract description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 72
- 239000000243 solution Substances 0.000 claims description 50
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
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- 239000007864 aqueous solution Substances 0.000 claims description 9
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 8
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- 239000001632 sodium acetate Substances 0.000 claims description 8
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- -1 wherein Chemical compound 0.000 claims description 8
- VZOPRCCTKLAGPN-ZFJVMAEJSA-L potassium;sodium;(2r,3r)-2,3-dihydroxybutanedioate;tetrahydrate Chemical compound O.O.O.O.[Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O VZOPRCCTKLAGPN-ZFJVMAEJSA-L 0.000 claims description 7
- 229940074446 sodium potassium tartrate tetrahydrate Drugs 0.000 claims description 7
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- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 abstract 1
- 229940074439 potassium sodium tartrate Drugs 0.000 abstract 1
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- PFPDWGGTEJAIIG-UHFFFAOYSA-L sodium nickel(2+) sulfate Chemical compound [Ni+2].S(=O)(=O)([O-])[O-].[Na+] PFPDWGGTEJAIIG-UHFFFAOYSA-L 0.000 description 6
- 230000004913 activation Effects 0.000 description 5
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- 150000002940 palladium Chemical class 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
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- 239000001119 stannous chloride Substances 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1875—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment only one step pretreatment
- C23C18/1879—Use of metal, e.g. activation, sensitisation with noble metals
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Abstract
本发明公开了一种氧化铝陶瓷表面无钯活化化学镀镍工艺，属于氧化铝陶瓷表面处理技术领域。本发明采用镍胶体活化氧化铝表面后进行化学镀镍，具体步骤为：1、打磨氧化铝表面；2、用氢氧化钠粗化氧化铝基片，并彻底冲洗干净；3、将粗化好的基片在硼氢化钠中浸渍30s，然后，在镍胶体中活化20s，镍胶体由0.08mol/L硫酸镍和0.04mol/L的酒石酸钾钠混合制备，4、化学镀镍。本发明采用镍胶体活化工艺代替传统的贵金属钯活化工艺，降低生产成本，减少环境污染，经镍胶体活化的氧化铝表面活性中心较多且分布均匀，施镀后得到了平整连续的化学镀层。本发明操作简单，成本低，反应室温进行，环境污染少，能满足工业化应用的要求。
Description
技术领域
本发明属于材料表面改性的技术领域，特别是指一种氧化铝陶瓷表面无钯活化化学镀镍工艺。
背景技术
氧化铝陶瓷是一种以α型氧化铝粉末为骨料，经高温烧成、内部形成大量彼此相通并与材料表面也相贯通的孔道结构的陶瓷材料。因其原材料廉价，制备简单，具有较高的机械强度、抗腐蚀性、抗高温氧化及耐热冲击性等优点，是一种用途广泛的陶瓷。氧化铝陶瓷用于集成电路时，需要先对其进行金属化。
陶瓷金属化的方法有很多种，如磁控溅射、电镀、真空蒸镀法、化学镀等。其中，化学镀镍具有镀层性能优良、结合强度高、耐磨、耐腐蚀、工艺简单等优点。目前，化学镀镍已在机械、电子及微电子、航空航天、石油化工、汽车、纺织、食品、军事等工业部门获得广泛应用。
发明内容
本发明提供一种氧化铝陶瓷表面无钯活化化学镀镍工艺，解决了现有技术中的采用贵金属钯作为活化原料的高成本及废液排放造成的污染问题，同时在氧化铝陶瓷表面成功镀覆一层致密连续的化学镀镍层。
本发明的氧化铝陶瓷表面无钯活化化学镀镍工艺，其主要是通过以下技术方案加以这样实现的：氧化铝陶瓷→打磨→清洗除油→粗化→清洗→镍胶体活化→化学镀镍，具体步骤如下：
(1)打磨：用砂纸打磨氧化铝表面，去除氧化层，形成粗糙的表面；
(2)清洗除油：分别用无机酸和去离子水清洗氧化铝表面；
(3)粗化：用强碱溶液粗化氧化铝表面，并冲洗干净；
(4)镍胶体活化：将粗化后的氧化铝陶瓷在硼盐溶液中浸泡20-30s，冲洗后，在镍胶体中浸泡20-30s，并彻底冲洗干净，得氧化铝基片；
(5)将步骤(4)中活化过的氧化铝基片在化学镀镍液中进行化学镀，施镀温度为70-80℃，镀液的pH值为5.0-6.0，化学镀镍溶液的组成为硫酸镍、柠檬酸钠，醋酸钠、次亚磷酸钠和乳酸，其中，硫酸镍：柠檬酸钠：醋酸钠：次磷酸钠的浓度比为2-3:1-1.5:1.5-2.5:2-3。
本发明氧化铝陶瓷表面无钯活化化学镀镍工艺，采用镍胶体代替传统的贵金属钯作为原料对基体表面进行活化，避免了贵金属钯的使用，降低了生产成本，同时减少了钯废液排放带来的环境污染，是一个环保的低成本基体活化工艺。采用此工艺预处理过的氧化铝陶瓷，表面活性中心较多且分布均与，化学镀后氧化铝表面获得了平整连续致密的镀层。
作为一种优选的实施方案，所述步骤(4)中镍胶体配制工艺为：称取1.05g硫酸镍和0.56g酒石酸钾钠，40-45℃下配成50ml水溶液并恒温5min。
作为一种优选的实施方案，所述步骤(4)中硼盐溶液为硼氢化钠，其浓度为：20g/L。
作为一种优选的实施方案，所述步骤(5)中化学镀镍溶液的成分及含量为：
作为一种优选的实施方案，所述步骤(5)中的化学镀镍溶液的制备方法为：
(a)取料：取硫酸镍、次亚磷酸钠、柠檬酸钠、醋酸钠，分别用适量去离子水充分溶解，形成4种水溶液，取乳酸备用；
(b)混料：先将硫酸镍溶液加入柠檬酸钠溶液中，再加入乳酸及醋酸钠溶液，最后加入次亚磷酸钠溶液，搅匀得溶液；
(c)用碱调整镀液的pH值至5.0-6.0，过滤溶液，得化学镀镍溶液。
作为一种优选的实施方案，步骤(3)中氧化铝陶瓷表面粗化工艺为：采用1-2mol/L氢氧化钠溶液浸泡0.5-1min。
作为一种优选的实施方案，步骤(2)中氧化铝陶瓷表面除油工艺为：采用1-2mol/L盐酸溶液浸泡5min。
本发明的有益效果：采用镍胶体活化工艺代替传统的贵金属钯活化工艺，降低了生产成本，减少贵金属钯排放带来的环境污染问题；采用镍胶体活化过的氧化铝陶瓷表面活性中心较多且分布均匀，在化学镀镍液中施镀30min后，得到了平整连续且致密的化学镀镍层。本发明操作简单，成本低，反应室温进行，环境污染少，能满足工业化应用的要求。
附图说明
图1为实施例1制备的氧化铝陶瓷表面化学镀镍层的扫描电镜图片；
图2为实施例2制备的氧化铝陶瓷表面化学镀镍层的扫描电镜图片；
图3为实施例2制备的氧化铝陶瓷表面化学复合镀镍层的X射线衍射谱图；
图4为实施例3制备的氧化铝陶瓷表面化学复合镀镍层的扫描电镜图片；
具体实施方式
下面将结合本发明的具体实施例对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明的一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例一传统氯化钯活化氧化铝表面化学镀镍
将氧化铝也称氧化铝基片、氧化铝陶瓷或氧化铝陶瓷基片，用W28金相砂纸打磨，分别用1mol/L盐酸水溶液和去离子水清洗除油，用1mol/L的NaOH溶液粗化30s，冲洗干净后用30g/L的氯化亚锡溶液室温敏化5分钟，用2g/L的氯化钯溶液活化5min，反复冲洗基片后，放到如下配方溶液中化学镀镍；
| 硫酸镍 | 次磷酸钠 | 柠檬酸钠 | 醋酸钠 | 乳酸 |
| 20-30g/L | 20-30g/L | 10-15g/L | 15-25g/L | 15-25ml/L |
镀液温度70-80℃，pH值为5-6，施镀时间30min，得到的镀层平整但不连续，多处出现裂纹、小坑等瑕疵，如图1所示。
实施例二镍胶体活化氧化铝表面化学镀镍
将氧化铝基片用W28金相砂纸打磨，分别用1mol/L盐酸水溶液和去离子水清洗除油，用1mol/L的NaOH溶液粗化30s，冲洗干净后用20g/L的硼氢化钠水溶液活化20s，稍微冲洗再用21g/L硫酸镍和11.2g/L酒石酸钾钠配制的镍胶体反应30s，反复冲洗基片，放到如下配方溶液中化学镀镍；
| 硫酸镍 | 次磷酸钠 | 柠檬酸钠 | 醋酸钠 | 乳酸 |
| 20-30g/L | 20-30g/L | 10-15g/L | 15-25g/L | 15-25ml/L |
镀液温度70-80℃，pH值为5-6，施镀时间30min，得到了平整连续致密化学镀镍层，如图2、3所示。
实施例三镍胶体活化氧化铝表面化学复合镀镍钛硅分子筛
将氧化铝基片用W28金相砂纸打磨，分别用1mol/L盐酸水溶液和去离子水清洗除油，用1mol/L的NaOH溶液粗化30s，冲洗干净后用20g/L的硼氢化钠水溶液活化20s，稍微冲洗再用21g/L硫酸镍和11.2g/L酒石酸钾钠配制的镍胶体反应30s，反复冲洗基片，放到如下配方溶液中化学镀镍；
| 硫酸镍 | 次磷酸钠 | 柠檬酸钠 | 醋酸钠 | 乳酸 | 钛硅分子筛 | SDS |
| 20-30g/L | 20-30g/L | 10-15g/L | 15-25g/L | 15-25ml/L | 2g/L | 30mg/L |
镀液温度70-80℃，pH值为5-6，施镀时间30min，得到的镀层平整连续致密，钛硅分子筛均匀分布于镀层中，如图4所示。
实施例四镍胶体活化氧化铝表面化学镀镍
将氧化铝基片用W28金相砂纸打磨，分别用1mol/L盐酸水溶液和去离子水清洗除油，用1mol/L的NaOH溶液粗化30s，冲洗干净后用20g/L的硼氢化钠水溶液活化20s，稍微冲洗再用21g/L硫酸镍和11.2g/L酒石酸钾钠配制的镍胶体反应30s，反复冲洗基片，放到如下配方溶液中化学镀镍；
| 硫酸镍 | 次磷酸钠 | 柠檬酸钠 | 醋酸钠 | 乳酸 |
| 20g/L | 20g/L | 10g/L | 15g/L | 15ml/L |
镀液温度70-80℃，pH值为5-6，施镀时间30min，得到平整连续致密的镀镍层。
实施例五镍胶体活化氧化铝表面化学镀镍
将氧化铝基片用W28金相砂纸打磨，分别用1mol/L盐酸水溶液和去离子水清洗除油，用1mol/L的NaOH溶液粗化30s，冲洗干净后用20g/L的硼氢化钠水溶液活化20s，稍微冲洗再用21g/L硫酸镍和11.2g/L酒石酸钾钠配制的镍胶体反应30s，反复冲洗基片，放到如下配方溶液中化学镀镍；
| 硫酸镍 | 次磷酸钠 | 柠檬酸钠 | 醋酸钠 | 乳酸 |
| 25g/L | 25g/L | 12g/L | 20g/L | 20ml/L |
镀液温度70-80℃，pH值为5-6，施镀时间30min，得到平整连续致密的镀镍层。
实施例六镍胶体活化氧化铝表面化学镀镍
将氧化铝基片用W28金相砂纸打磨，分别用1mol/L盐酸水溶液和去离子水清洗除油，用1mol/L的NaOH溶液粗化30s，冲洗干净后用20g/L的硼氢化钠水溶液活化20s，稍微冲洗再用21g/L硫酸镍和11.2g/L酒石酸钾钠配制的镍胶体反应30s，反复冲洗基片，放到如下配方溶液中化学镀镍；
| 硫酸镍 | 次磷酸钠 | 柠檬酸钠 | 醋酸钠 | 乳酸 |
| 30g/L | 30g/L | 15g/L | 25g/L | 25ml/L |
镀液温度70-80℃，pH值为5-6，施镀时间30min，得到平整连续致密的镀镍层。
本发明的有益效果：本发明的氧化铝陶瓷表面无钯活化化学镀镍工艺，所述无钯活化工艺可代替传统的钯活化工艺，减少了贵金属钯的使用及废弃，降低了生产成本，减少了环境污染；采用镍胶体活化过的氧化铝陶瓷表面活性中心较多且分布均匀，在化学镀镍液中施镀30min后，得到了平整连续且致密的化学镀镍层。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (7)
1.一种氧化铝陶瓷表面无钯活化化学镀镍工艺，其特征在于，包括以下步骤：
(1)打磨：用砂纸打磨氧化铝表面，去除氧化层，形成粗糙的表面；
(2)清洗除油：分别用无机酸和去离子水清洗氧化铝表面；
(3)粗化：用强碱溶液粗化氧化铝表面，并冲洗干净；
(4)镍胶体活化：将粗化后的氧化铝陶瓷在硼盐溶液中浸泡20-30s，冲洗后，在镍胶体中浸泡20-30s，并彻底冲洗干净，得氧化铝基片；
(5)将步骤(4)中活化过的氧化铝基片在化学镀镍液中进行化学镀，施镀温度为70-80℃，镀液的pH值为5.0-6.0，化学镀镍溶液的组成为硫酸镍、柠檬酸钠，醋酸钠、次亚磷酸钠和乳酸，其中，硫酸镍：柠檬酸钠：醋酸钠：次磷酸钠的浓度比为2-3:1-1.5:1.5-2.5:2-3。
2.根据权利要求1所述的氧化铝陶瓷表面无钯活化化学镀镍工艺，其特征在于：所述步骤(4)中镍胶体配制工艺为：称取1.05g硫酸镍和0.56g酒石酸钾钠，40-45℃下配成50ml水溶液并恒温5min。
3.根据权利要求1所述的氧化铝陶瓷表面无钯活化化学镀镍工艺，其特征在于：所述步骤(4)中硼盐溶液为硼氢化钠，其浓度为：20g/L。
4.根据权利要求1所述的氧化铝陶瓷表面无钯活化化学镀镍工艺，其特征在于，所述步骤(5)中化学镀镍溶液的成分及含量为：
5.根据权利要求4所述的氧化铝陶瓷表面无钯活化化学镀镍工艺，其特征在于，所述步骤(5)中化学镀镍溶液的制备方法为：
(a)取料：取硫酸镍、次亚磷酸钠、柠檬酸钠、醋酸钠，分别用适量去离子水充分溶解，形成4种水溶液，取乳酸备用；
(b)混料：先将硫酸镍溶液加入柠檬酸钠溶液中，再加入乳酸及醋酸钠溶液，最后加入次亚磷酸钠溶液，搅匀得溶液；
(c)用碱调整镀液的pH值至5.0-6.0，过滤溶液，得化学镀镍溶液。
6.根据权利要求1所述的氧化铝陶瓷表面无钯活化化学镀镍工艺，其特征在于：步骤(3)中氧化铝陶瓷表面粗化工艺为：采用1-2mol/L氢氧化钠溶液浸泡0.5-1min。
7.根据权利要求1所述的氧化铝陶瓷表面无钯活化化学镀镍工艺，其特征在于：步骤(2)中氧化铝陶瓷表面除油工艺为：采用1-2mol/L盐酸溶液浸泡5min。
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