CN100348778C - Chemical copper plating process for the surface of SiC ceramic grain - Google Patents
Chemical copper plating process for the surface of SiC ceramic grain Download PDFInfo
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- CN100348778C CN100348778C CNB2005100299052A CN200510029905A CN100348778C CN 100348778 C CN100348778 C CN 100348778C CN B2005100299052 A CNB2005100299052 A CN B2005100299052A CN 200510029905 A CN200510029905 A CN 200510029905A CN 100348778 C CN100348778 C CN 100348778C
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- 239000000919 ceramic Substances 0.000 title claims abstract description 66
- 238000007747 plating Methods 0.000 title claims abstract description 31
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 21
- 239000010949 copper Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 11
- 239000000126 substance Substances 0.000 title 1
- 239000002245 particle Substances 0.000 claims abstract description 57
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 16
- 239000010937 tungsten Substances 0.000 claims abstract description 16
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000007788 roughening Methods 0.000 claims abstract description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 7
- 239000001257 hydrogen Substances 0.000 claims abstract description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 7
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 230000010355 oscillation Effects 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 7
- LXAHHHIGZXPRKQ-UHFFFAOYSA-N 5-fluoro-2-methylpyridine Chemical compound CC1=CC=C(F)C=N1 LXAHHHIGZXPRKQ-UHFFFAOYSA-N 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 5
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 5
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000011068 loading method Methods 0.000 claims description 5
- 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 claims description 5
- 235000011006 sodium potassium tartrate Nutrition 0.000 claims description 5
- XOGGUFAVLNCTRS-UHFFFAOYSA-N tetrapotassium;iron(2+);hexacyanide Chemical compound [K+].[K+].[K+].[K+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] XOGGUFAVLNCTRS-UHFFFAOYSA-N 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 abstract description 6
- 238000000576 coating method Methods 0.000 abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 abstract description 4
- 206010070834 Sensitisation Diseases 0.000 abstract description 3
- 229910021607 Silver chloride Inorganic materials 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 230000008313 sensitization Effects 0.000 abstract description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 abstract description 3
- 229960000583 acetic acid Drugs 0.000 abstract description 2
- 239000012362 glacial acetic acid Substances 0.000 abstract description 2
- 229910002666 PdCl2 Inorganic materials 0.000 abstract 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 abstract 1
- 229960002163 hydrogen peroxide Drugs 0.000 description 5
- 229960000935 dehydrated alcohol Drugs 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 101150003085 Pdcl gene Proteins 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
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Abstract
一种SiC陶瓷颗粒表面化学镀铜方法，首先对SiC陶瓷颗粒表面进行硝酸粗化处理，用钨粉、双氧水，无水乙醇和冰乙酸制备得到溶胶，然后将粗化处理后的SiC陶瓷颗粒泡入溶胶之中并辅以超声振荡，使在陶瓷颗粒表面形成溶胶薄层，再经干燥及氢气还原，得到镀覆钨的SiC陶瓷颗粒后，再进行化学镀铜处理。由于铜对钨良好的润湿性和钨自身的催化活性，从而可以得到铜包裹均匀的陶瓷。相对已有的化学镀铜工艺，本发明无需用昂贵的PdCl2或者AgCl对陶瓷表面进行活化，省略了敏化步骤，具有易于操作，包覆均匀，成本低廉的优势。A method for electroless copper plating on the surface of SiC ceramic particles. First, roughen the surface of SiC ceramic particles with nitric acid, prepare a sol with tungsten powder, hydrogen peroxide, absolute ethanol and glacial acetic acid, and then soak the SiC ceramic particles after the roughening treatment. Into the sol and supplemented by ultrasonic vibration to form a thin layer of sol on the surface of the ceramic particles, and then dry and hydrogen reduction to obtain tungsten-coated SiC ceramic particles, and then perform electroless copper plating. Due to the good wettability of copper to tungsten and the catalytic activity of tungsten itself, ceramics with uniform copper coating can be obtained. Compared with the existing electroless copper plating process, the present invention does not need to use expensive PdCl2 or AgCl to activate the ceramic surface, omits the sensitization step, and has the advantages of easy operation, uniform coating and low cost.
Description
Technical field
The present invention relates to a kind of SiC ceramic grain surface electroless copper plating method, the copper facing ceramic particle that makes can be widely used in the preparation of metal-base composites and stupalith, belongs to technical field of function materials.
Background technology
Because SiC pottery is bad with the wettability of some metals, therefore in Composite Preparation, often need in advance at its copper coating to improve the combination between SiC and the metal.The copper-plated common technology of SiC particle surface is an electroless copper at present, and its technology comprises substantially pre-treatment such as particle surface alligatoring, sensitization and activation, and then carries out plating.Usually the activator that adopts is expensive PdCl
2Perhaps AgCl.Simultaneously strict, not easy to operate between each step of pre-treatment, the phenomenon that copper is not gone up in the even even plating of uneven coating appears easily.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of SiC ceramic grain surface electroless copper plating method is provided, simple, cheap, the ceramic grain surface copper coating that makes coats evenly.
For realizing such purpose, technical scheme of the present invention is: at first the SiC ceramic grain surface is carried out the nitric acid roughening treatment, with tungsten powder, hydrogen peroxide, dehydrated alcohol and glacial acetic acid prepare colloidal sol, then the SiC ceramic particle after the roughening treatment is steeped among the colloidal sol and be aided with sonic oscillation, make at ceramic grain surface and form colloidal sol thin layer, drying and hydrogen reducing, after obtaining the SiC ceramic particle of plating tungsten, carry out electroless copper again and handle.Because copper is wrapped up in uniform pottery to the good wettability of tungsten and the catalytic activity of tungsten self thereby can obtain copper-clad.
Method of the present invention specifically comprises the steps:
1) the SiC ceramic particle is put into concentration greater than 70% nitric acid and sonic oscillation in addition, it is carried out roughening treatment, take out after 5 minutes and use deionized water rinsing, obtain having and clean and the SiC ceramic particle of uneven surface.
2) by following proportioning and method preparation colloidal sol: get every 0.5-1 gram tungsten powder and the reaction of 2.5-5 milliliter hydrogen peroxide, reaction adds 2 milliliters of dehydrated alcohols afterwards and 0.75 milliliter of acetate mixes, and filters out reaction residual, obtains faint yellow colloidal sol.The amount of the colloidal sol of preparing wants to satisfy the needs of the complete submergence SiC of next step ceramic particle.
3) being immersed in the above-mentioned colloidal sol, be aided with sonic oscillation 10-20 minute, make SiC ceramic particle homodisperse in colloidal sol through the SiC of roughening treatment ceramic particle;
4) the SiC ceramic particle after the above processing is put into 300-350 ℃ the dry 2-3 of loft drier hour, take out cooling;
5) the good SiC ceramic particle of above drying under hydrogen atmosphere in 760-800 ℃ of reductase 12-3 hour, take out behind the furnace cooling, obtain the SiC ceramic particle of plating tungsten.
6) the preparation plating bath contains the copper sulfate of 15g/l, the formaldehyde of 25ml/l, the EDTA disodium of 25g/l, the Seignette salt of 14g/l and the yellow prussiate of potash of 10mg/l in the plating bath, and the pH value is adjusted between the 12-13 with NaOH solution, 60 ℃ of temperature.The SiC ceramic particle of above-mentioned plating tungsten is poured in the plating bath, and loading capacity is 10-18g/l.Be aided with magnetic agitation.
7) react completely after-filtration and at 120-160 ℃ of dry 3-5 hour obtains copper-clad and wraps up in uniform SiC ceramic particle.
The present invention has easy handling, coats evenly advantage with low cost.As long as the amount of required colloidal sol can be soaked the SiC ceramic particle fully in the method, need not simultaneously with expensive PdCl
2Perhaps AgCl activates ceramic surface, has omitted the sensitization step.Because copper to the good wettability of tungsten and the catalytic activity of tungsten self, can obtain the copper facing SiC ceramic particle of even adhere firmly of thickness and bright in color.The thickness of plating tungsten layer can be controlled at below the 50-200nm, and the thickness of copper coating is below 2 μ m.In the preparation of metal-base composites and stupalith, have wide practical use.This technology of the present invention goes for other as Al
2O
3, the electroless copper of materials such as graphite.
Embodiment
Below by specific embodiment technical scheme of the present invention is further described.Following examples are that the SiC ceramic particle of 20 μ m is that example describes with median size, but should not be considered as limitation of the invention.
Embodiment 1:
1. 5g SiC ceramic particle is put into 20ml concentration and be 70% nitric acid and sonic oscillation in addition, it is carried out roughening treatment.Take out after 5 minutes and use deionized water rinsing, obtain having and clean and the SiC ceramic particle of uneven surface.
2. get the reaction of 1g tungsten powder and 5ml hydrogen peroxide, reaction adds the 2ml dehydrated alcohol afterwards and 0.75ml acetate mixes.Filter out reaction residual, obtain faint yellow colloidal sol.
3. steeping in the above-mentioned colloidal sol, be aided with sonic oscillation 10 minutes, make SiC ceramic particle homodisperse in colloidal sol through the 5gSiC of roughening treatment ceramic particle.
4. the SiC ceramic particle after the above processing is put into 300 ℃ dry 3 hours of loft drier, taken out cooling.
The good SiC ceramic particle of above drying under hydrogen atmosphere in 760 ℃ of reduction 3 hours, take out behind the furnace cooling, obtain the SiC ceramic particle of plating tungsten.
6. press 7.5g copper sulfate+12.5ml formaldehyde+12.5g EDTA disodium+7g Seignette salt+5mg yellow prussiate of potash configuration plating bath 500ml, the pH value is adjusted between the 12-13 with NaOH solution, 60 ℃ of temperature.The surface is wrapped up the powder of W layer and pour in the plating bath, loading capacity is 10g/l.Be aided with magnetic agitation.
7. react completely after-filtration and 120 ℃ of dryings 5 hours promptly obtains copper-clad and wraps up in uniform SiC ceramic particle.
Embodiment 2:
1. 7g SiC ceramic particle is put into 20ml concentration and be 80% nitric acid and sonic oscillation in addition, it is carried out roughening treatment.Take out after 5 minutes and use deionized water rinsing, obtain having and clean and the SiC ceramic particle of uneven surface.
2. get the reaction of 2g tungsten powder and 5ml hydrogen peroxide, reaction adds the 4ml dehydrated alcohol afterwards and 1.5ml acetate mixes.Filter out reaction residual, obtain faint yellow colloidal sol.
3. steeping in the above-mentioned colloidal sol, be aided with sonic oscillation 15 minutes, make SiC ceramic particle homodisperse in colloidal sol through the 7g of roughening treatment SiC ceramic particle.
4. the SiC ceramic particle after the above processing is put into 320 ℃ dry 2.5 hours of loft drier, taken out cooling.
The good SiC ceramic particle of above drying under hydrogen atmosphere in 780 ℃ of reductase 12 .5 hours, take out behind the furnace cooling, obtain the SiC ceramic particle of plating tungsten.
6. press 7.5g copper sulfate+12.5ml formaldehyde+12.5g EDTA disodium+7g Seignette salt+5mg yellow prussiate of potash configuration plating bath 500ml, the pH value is adjusted between the 12-13 with NaOH solution, 60 ℃ of temperature.The surface is wrapped up the powder of W layer and pour in the plating bath, loading capacity is 14g/l.Be aided with magnetic agitation.
7. react completely after-filtration and 140 ℃ of dryings 4 hours promptly obtains copper-clad and wraps up in uniform SiC ceramic particle.
Embodiment 3:
1. 9g SiC ceramic particle is put into 20ml concentration and be 90% nitric acid and sonic oscillation in addition, it is carried out roughening treatment.Take out after 5 minutes and use deionized water rinsing, obtain having and clean and the SiC ceramic particle of uneven surface.
2. get the reaction of 4g tungsten powder and 40ml hydrogen peroxide, reaction adds the 16ml dehydrated alcohol afterwards and 3ml acetate mixes.Filter out reaction residual, obtain faint yellow colloidal sol.
3. steeping in the above-mentioned colloidal sol, be aided with sonic oscillation 20 minutes, make SiC ceramic particle homodisperse in colloidal sol through the 9gSiC of roughening treatment ceramic particle.
4. the SiC ceramic particle after the above processing is put into 350 ℃ dry 2 hours of loft drier, taken out cooling.
The good SiC ceramic particle of above drying under hydrogen atmosphere in 800 ℃ of reductase 12s hour, take out behind the furnace cooling, obtain the SiC ceramic particle of plating tungsten.
6. press 7.5g copper sulfate+12.5ml formaldehyde+12.5g EDTA disodium+7g Seignette salt+5mg yellow prussiate of potash configuration plating bath 500ml, the pH value is adjusted between the 12-13 with NaOH solution, 60 ℃ of temperature.The surface is wrapped up the powder of W layer and pour in the plating bath, loading capacity is 18g/l.Be aided with magnetic agitation.
7. react completely after-filtration and 160 ℃ of dryings 3 hours promptly obtains copper-clad and wraps up in uniform SiC ceramic particle.
Claims (1)
1, a kind of SiC ceramic grain surface electroless copper plating method is characterized in that comprising the steps:
1) the SiC ceramic particle is put into concentration greater than 70% nitric acid and sonic oscillation in addition, it is carried out roughening treatment, take out after 5 minutes and use deionized water rinsing, obtain having and clean and the SiC ceramic particle of uneven surface;
2) by following proportioning and method preparation colloidal sol: get every 0.5-1 gram tungsten powder and the reaction of 2.5-5 milliliter hydrogen peroxide, reaction adds 2 milliliters of dehydrated alcohols afterwards and 0.75 milliliter of acetate mixes, and filters out reaction residual, obtains faint yellow colloidal sol; The amount of the colloidal sol of preparing wants to satisfy the needs of the complete submergence SiC of next step ceramic particle;
3) being immersed in the above-mentioned colloidal sol, be aided with sonic oscillation 10-20 minute, make SiC ceramic particle homodisperse in colloidal sol through the SiC of roughening treatment ceramic particle;
4) the SiC ceramic particle after the above processing is put into 300-350 ℃ the dry 2-3 of loft drier hour, take out cooling;
5) the good SiC ceramic particle of above drying under hydrogen atmosphere in 760-800 ℃ of reductase 12-3 hour, take out behind the furnace cooling, obtain the SiC ceramic particle of plating tungsten;
6) preparation plating bath, contain the copper sulfate of 15g/l, the formaldehyde of 25ml/l, the EDTA disodium of 25g/l, the Seignette salt of 14g/l and the yellow prussiate of potash of 10mg/l in the plating bath, the pH value is adjusted between the 12-13 with NaOH solution, 60 ℃ of temperature, the SiC ceramic particle of above-mentioned plating tungsten is poured in the plating bath, loading capacity is 10-18g/l, is aided with magnetic agitation;
7) react completely after-filtration and at 120-160 ℃ of dry 3-5 hour obtains copper-clad and wraps up in uniform SiC ceramic particle.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100299052A CN100348778C (en) | 2005-09-22 | 2005-09-22 | Chemical copper plating process for the surface of SiC ceramic grain |
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|---|---|---|---|
| CNB2005100299052A CN100348778C (en) | 2005-09-22 | 2005-09-22 | Chemical copper plating process for the surface of SiC ceramic grain |
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| CN1740382A CN1740382A (en) | 2006-03-01 |
| CN100348778C true CN100348778C (en) | 2007-11-14 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798238B (en) * | 2010-03-26 | 2013-05-01 | 山东建筑大学 | Ceramic metallizing method |
| CN102642025A (en) * | 2012-04-26 | 2012-08-22 | 上海交通大学 | Method for plating tungsten on surface of SiC particle |
| CN103966601B (en) * | 2013-02-05 | 2018-05-18 | 汉达精密电子(昆山)有限公司 | Production method of nonmetal basal body conducting wire and products thereof |
| CN103498156A (en) * | 2013-09-27 | 2014-01-08 | 成都四威高科技产业园有限公司 | Surface coating technology of silicon carbide particle reinforced aluminium-based composite |
| CN104561942B (en) * | 2014-12-24 | 2017-02-22 | 北方民族大学 | Palladium-free activation method of silicon carbide powder |
| CN104630751B (en) * | 2015-02-05 | 2017-05-24 | 山西中通高技术有限责任公司 | Boron carbide particle surface nickel plating method |
| CN105296792B (en) * | 2015-11-10 | 2017-08-01 | 东华大学 | Ceramic-reinforced copper-based composite material for electronic packaging and preparation method thereof |
| CN111825460B (en) * | 2020-07-31 | 2021-07-30 | 贵州师范学院 | A kind of high-efficiency and low-cost thermal reduction nickel plating method on the surface of silicon carbide particles |
| CN113003608A (en) * | 2021-03-16 | 2021-06-22 | 宁波伯宇科技有限公司 | Method for manufacturing electrochromic material semi-finished product |
| CN115029688A (en) * | 2021-12-28 | 2022-09-09 | 中国矿业大学 | Three-dimensional porous ceramic surface chemical copper plating solution, preparation method and copper plating process |
| CN114315368A (en) * | 2022-01-05 | 2022-04-12 | 河南科技大学 | Composite material of metallic copper and MoAlB ceramic and its preparation method and application |
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|---|---|---|---|---|
| US4762695A (en) * | 1985-03-04 | 1988-08-09 | Kabushiki Kaisha Toshiba | Methods for preparing high-purity molybdenum or tungsten powder and high-purity oxides powder of the same |
| CN1188158A (en) * | 1997-01-13 | 1998-07-22 | 中国科学院金属研究所 | Method for preparing metal-base composite material reinforced by non-continuous ceramics reinforcing agent |
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| CN1419985A (en) * | 2001-11-21 | 2003-05-28 | 中国科学院金属研究所 | Method for mfg. Cu/Ti3SiC2 composite material by chemical copper plating |
-
2005
- 2005-09-22 CN CNB2005100299052A patent/CN100348778C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4762695A (en) * | 1985-03-04 | 1988-08-09 | Kabushiki Kaisha Toshiba | Methods for preparing high-purity molybdenum or tungsten powder and high-purity oxides powder of the same |
| CN1188158A (en) * | 1997-01-13 | 1998-07-22 | 中国科学院金属研究所 | Method for preparing metal-base composite material reinforced by non-continuous ceramics reinforcing agent |
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Non-Patent Citations (1)
| Title |
|---|
| SiCp表面化学镀铜工艺研究 陈曙光，丁厚福，郑治祥，刘君武.热加工工艺，第1期 2001 * |
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