CN1362536A - Surface metallizing process of ceramic electronic device - Google Patents
Surface metallizing process of ceramic electronic device Download PDFInfo
- Publication number
- CN1362536A CN1362536A CN01138020.9A CN01138020A CN1362536A CN 1362536 A CN1362536 A CN 1362536A CN 01138020 A CN01138020 A CN 01138020A CN 1362536 A CN1362536 A CN 1362536A
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- Prior art keywords
- silver
- complexing agent
- plating
- ceramic electronic
- concentration
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- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000000919 ceramic Substances 0.000 title claims abstract description 18
- 238000007747 plating Methods 0.000 claims abstract description 32
- 229910052709 silver Inorganic materials 0.000 claims abstract description 22
- 239000004332 silver Substances 0.000 claims abstract description 22
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000008139 complexing agent Substances 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052802 copper Inorganic materials 0.000 claims abstract description 11
- 239000010949 copper Substances 0.000 claims abstract description 11
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid group Chemical group C(CC(O)(C(=O)O)CC(=O)O)(=O)O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 9
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims abstract description 4
- 238000007654 immersion Methods 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 9
- 238000006263 metalation reaction Methods 0.000 claims description 7
- 206010070834 Sensitisation Diseases 0.000 claims description 6
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical group CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 claims description 6
- 230000004913 activation Effects 0.000 claims description 6
- 230000008313 sensitization Effects 0.000 claims description 6
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 3
- 229940095064 tartrate Drugs 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 21
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 238000005238 degreasing Methods 0.000 abstract description 2
- 230000001235 sensitizing effect Effects 0.000 abstract description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 abstract 1
- 230000003213 activating effect Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 125000003916 ethylene diamine group Chemical group 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 239000011975 tartaric acid Substances 0.000 abstract 1
- 235000002906 tartaric acid Nutrition 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- 238000002242 deionisation method Methods 0.000 description 5
- 229910000906 Bronze Inorganic materials 0.000 description 4
- 239000010974 bronze Substances 0.000 description 4
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 229910052573 porcelain Inorganic materials 0.000 description 4
- 238000002203 pretreatment Methods 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 2
- 239000012964 benzotriazole Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000001465 metallisation Methods 0.000 description 2
- 239000001509 sodium citrate Substances 0.000 description 2
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 2
- 229940038773 trisodium citrate Drugs 0.000 description 2
- LXAHHHIGZXPRKQ-UHFFFAOYSA-N 5-fluoro-2-methylpyridine Chemical compound CC1=CC=C(F)C=N1 LXAHHHIGZXPRKQ-UHFFFAOYSA-N 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 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 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000011006 sodium potassium tartrate Nutrition 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 235000011150 stannous chloride Nutrition 0.000 description 1
- 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 description 1
- DHCDFWKWKRSZHF-UHFFFAOYSA-L thiosulfate(2-) Chemical compound [O-]S([S-])(=O)=O DHCDFWKWKRSZHF-UHFFFAOYSA-L 0.000 description 1
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
Landscapes
- Chemically Coating (AREA)
Abstract
The method for metallizing surface of ceramic electronic device includes: degreasing ceramic substrate, coarsing, sensitizing, activating and chemically-plating copper, then dip-plating in silver dip-plating liquor, washing with water and drying. The silver dipo-plating liquor is formed from silver ntirate, complexing agent and auxiliary complexing agent, in which concentration of silver nitrate is 0.1g-20g/l, concentration of coplexing agent i 10g-100g/l, and auxiliary complexing agent concentration is 0.5g-5g/l, and the complexing agent is citric acid or tartaric acid or its salt and auxiliary complexing agent is ethylenediamine or diethyltriamine.
Description
One, technical field
The present invention is a kind of method of carrying out metalized on the ceramic electronic component surface, and is especially a kind of in the metallized method of mobile phone pottery protective tube outside surface.
Two, background technology
Mobile phone pottery protective tube production now all is to adopt silver slurry silk screen process agglomerating method again, and not only production efficiency is low, and fixed investment is big, and the energy consumption height, and silver layer is inhomogeneous.Though ceramic direct chemical is silver-plated is a kind of possible selection, and existing processes all can not meet the demands: contain the plating bath instability of ammoniacal liquor, and be easy to generate the triazo-compound of explosion hazard; Be to influence weldability because can be mingled with sulfide in the sedimentary coating of plating bath of complexing agent with thiosulphate; The plating bath that contains prussiate has limited its application owing to its toxicity.All in addition electroless plating silver layers all can't reach the requirement (about 6 microns) [Cheng et al., Plating and SurfaceFinishing, 77,130-1329 (1990)] of ceramic protective tube.
Three, summary of the invention
(1) goal of the invention
The purpose of this invention is to provide that a kind of surface is fine and close, smooth more, the method for ceramic electronic component surface metalation with good combination power.
(2) technical scheme
The method of ceramic electronic component surface metalation of the present invention is deposition one deck chemical plating copper layer on ceramic bases, and then immersion silver, concrete process is first oil removing, alligatoring, sensitization, activation and electroless copper, immersion plating in silver-colored immersion plating liquid then, immersion plating after washing, oven dry.Silver immersion plating liquid is made up of Silver Nitrate, complexing agent, auxiliary complex-former, and wherein, the concentration of Silver Nitrate is 0.1 gram～20 grams per liters, and the concentration of complexing agent is 10 grams～100 grams per liters, and the concentration of auxiliary complex-former is 0.5 gram～5 grams per liters.Complexing agent is citric acid or tartrate and salt thereof.Auxiliary complex-former is quadrol or Diethylenetriamine and salt thereof.Continue after the immersion plating to prevent the variable color processing, to keep the weldability of silver layer with benzotriazole solution.
(3) technique effect
The present invention adopts deposition one deck chemical plating copper layer on ceramic bases earlier, and then the method for immersion silver realization metallization, and gained metallic silver layer thickness is even, is particularly suitable for surface mount, and has good weldability and bonding force.Experimental results show that this method can not only enhance productivity greatly, and facility investment is few, can save the silver consumption.
When the metal that metallicity is strong was immersed in the metal ion solution that contains relative inertness, the metal ion of relative inertness can be reduced to metallic state and active metal is oxidized.Under appropriate condition, inert metal can form smooth, fine and close settled layer, Here it is so-called displacement plating or immersion plating on the reactive metal surface.Copper surface immersion silver has been utilized this principle just.But the bonding force of general immersion plating silver layer is relatively poor.
The present invention has realized the metallization of ceramic surface by electroless copper.Found a kind of prescription and technology that obtains to have the immersion silver of good combination power: make coating fine and close, smooth more by adding auxiliary complex-formers such as quadrol, Diethylenetriamine with the chemical copper surface.This technology is equally applicable to other purposes, the copper face immersion silver process during for example printed circuit board is produced.
Four, embodiment
Embodiments of the invention are as follows:
All samples of embodiment are the ceramic protective tube in the mobile telephone.External diameter 1.5mm, internal diameter 1.0mm, long 5.0mm.
Use alkaline degreasing liquid, chromic acid coarsening solution, tin protochloride sensitizing solution among the embodiment.Used electroless copper liquid formula is as follows:
Copper sulfate 16/l
Tartrate first sodium 14/l
EDTA disodium 19.5/l
Sodium hydroxide 14.5/l
Formaldehyde (37%) 15ml/l
A, a '-dipyridyl 20mg/l
Yellow prussiate of potash 10mg/l
PH 12.5
Temperature 40-50 ℃
Silver immersion plating liquid is made up of Silver Nitrate, complexing agent, auxiliary complex-former, the optimum concn of Silver Nitrate is 0.5 gram～10 grams per liters, concentration the best of complexing agent is 10 grams～100 grams per liters, and concentration the best of auxiliary complex-former is 0.5～5 grams per liter, and anti-blushing agent is the derivative of triazole.
Embodiment 1.
After 20 porcelain tubes conspired to create string, after pre-treatment such as oil removing, alligatoring, sensitization, activation, plating was 40 minutes in above-mentioned chemical bronze plating liquid, took out, and deionization washing back was immersed in the following solution 30 seconds:
Silver Nitrate 1g/l
Trisodium citrate 60g/l
Quadrol 1g/l
PH 5.5
25 ℃ of washings of temperature, 60 ℃ of oven dry.The gained silver layer is a white, bonding force, good weldability.
Embodiment 2.
After 20 porcelain tubes conspired to create string, after pre-treatment such as oil removing, alligatoring, sensitization, activation, plating was 40 minutes in above-mentioned chemical bronze plating liquid, took out, and deionization washing back was immersed in the following solution 30 seconds:
Silver Nitrate 1g/l
Trisodium citrate 60g/l
Quadrol 2g/l
PH 8.0
25 ℃ of washings of temperature, 60 ℃ of oven dry.The gained silver layer is a white, bonding force, good weldability.
Embodiment 3.
After 20 porcelain tubes conspired to create string, after pre-treatment such as oil removing, alligatoring, sensitization, activation, plating was 40 minutes in above-mentioned chemical bronze plating liquid, took out, and deionization washing back was immersed in the following solution 30 seconds:
Silver Nitrate 1g/l
Seignette salt 60g/l
Quadrol 2g/l
PH 7.0
25 ℃ of washings of temperature, 60 ℃ of oven dry.The gained silver layer is a white, bonding force, good weldability.
Embodiment 4.
After 20 porcelain tubes conspire to create string, after pre-treatment such as oil removing, alligatoring, sensitization, activation, plating is 40 minutes in above-mentioned chemical bronze plating liquid, take out, deionization washing back is immersed as in the solution as described in the embodiment 2 50 seconds, the deionization washing is left standstill in 2% benzotriazole solution and was prevented the variable color processing in 1 minute, to keep the weldability of silver layer.Washing, 60 ℃ of oven dry.After preserving 20 days under 40 ℃, relative humidity 93% condition, all samples color and luster substantially becomes, and when wave soldering was welded on the mobile telephone circuitry plate, weldability and electrical property were all qualified.
Claims (4)
1, a kind of method of ceramic electronic component surface metalation, it is characterized in that deposition one deck chemical plating copper layer on ceramic bases, and then immersion silver, concrete process is first oil removing, alligatoring, sensitization, activation and electroless copper, immersion plating in silver-colored immersion plating liquid then, immersion plating after washing, oven dry.
2, the method for ceramic electronic component surface metalation according to claim 1, it is characterized in that silver-colored immersion plating liquid is made up of Silver Nitrate, complexing agent, auxiliary complex-former, wherein, the concentration of Silver Nitrate is 0.1 gram～20 grams per liters, the concentration of complexing agent is 10 grams～100 grams per liters, and the concentration of auxiliary complex-former is 0.5 gram～5 grams per liters.
3, the method for ceramic electronic component surface metalation according to claim 2 is characterized in that complexing agent is citric acid or tartrate and salt thereof.
4, the method for ceramic electronic component surface metalation according to claim 2 is characterized in that auxiliary complex-former is quadrol or Diethylenetriamine and salt thereof.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011380209A CN1156607C (en) | 2001-12-21 | 2001-12-21 | Surface metallizing process of ceramic electronic device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011380209A CN1156607C (en) | 2001-12-21 | 2001-12-21 | Surface metallizing process of ceramic electronic device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1362536A true CN1362536A (en) | 2002-08-07 |
| CN1156607C CN1156607C (en) | 2004-07-07 |
Family
ID=4674315
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011380209A Expired - Fee Related CN1156607C (en) | 2001-12-21 | 2001-12-21 | Surface metallizing process of ceramic electronic device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1156607C (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100343412C (en) * | 2005-04-30 | 2007-10-17 | 严盛喜 | Metalation technology of microwave medium multicavity filter |
| CN100362607C (en) * | 2005-02-06 | 2008-01-16 | 史宝林 | Full electrode producing process by round sheet type high voltage ceramic capacitor splash metal chemical depositing method |
| CN102747347A (en) * | 2012-07-31 | 2012-10-24 | 淮安市曼蒂科技发展有限公司 | Chemical silver plating solution and preparation method thereof |
| CN103253988A (en) * | 2012-02-16 | 2013-08-21 | 比亚迪股份有限公司 | Method of selective metallization on ceramic surface |
| CN103849861A (en) * | 2014-03-21 | 2014-06-11 | 扬州大学 | Method for cyanide-free replacement of plated silver on surface of copper-based body |
| WO2015027886A1 (en) * | 2013-08-26 | 2015-03-05 | Byd Company Limited | Silver plating solution and method of silver plating by chemical replacement |
| CN110459440A (en) * | 2019-07-24 | 2019-11-15 | 武汉理工大学 | A kind of temperature current high sensitive dual control safety element and preparation method |
| CN111732456A (en) * | 2020-06-30 | 2020-10-02 | 苏州蓝晶研材料科技有限公司 | Ceramic conductive material and preparation method and application thereof |
| CN112500193A (en) * | 2020-11-09 | 2021-03-16 | 麦德美科技（苏州）有限公司 | Chemical roughening and metallization process of calcium magnesium titanate ceramic |
| CN112899683A (en) * | 2019-12-03 | 2021-06-04 | 中兴通讯股份有限公司 | Ceramic dielectric filter surface metallization method, product and application thereof |
| 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 |
-
2001
- 2001-12-21 CN CNB011380209A patent/CN1156607C/en not_active Expired - Fee Related
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100362607C (en) * | 2005-02-06 | 2008-01-16 | 史宝林 | Full electrode producing process by round sheet type high voltage ceramic capacitor splash metal chemical depositing method |
| CN100343412C (en) * | 2005-04-30 | 2007-10-17 | 严盛喜 | Metalation technology of microwave medium multicavity filter |
| CN103253988A (en) * | 2012-02-16 | 2013-08-21 | 比亚迪股份有限公司 | Method of selective metallization on ceramic surface |
| CN102747347A (en) * | 2012-07-31 | 2012-10-24 | 淮安市曼蒂科技发展有限公司 | Chemical silver plating solution and preparation method thereof |
| CN102747347B (en) * | 2012-07-31 | 2014-06-11 | 淮安市曼蒂科技发展有限公司 | Chemical silver plating solution and preparation method thereof |
| WO2015027886A1 (en) * | 2013-08-26 | 2015-03-05 | Byd Company Limited | Silver plating solution and method of silver plating by chemical replacement |
| CN103849861A (en) * | 2014-03-21 | 2014-06-11 | 扬州大学 | Method for cyanide-free replacement of plated silver on surface of copper-based body |
| CN103849861B (en) * | 2014-03-21 | 2015-12-02 | 扬州大学 | A kind of method of carrying out on Copper substrate surface without cyanogen replacement ag plating |
| CN110459440A (en) * | 2019-07-24 | 2019-11-15 | 武汉理工大学 | A kind of temperature current high sensitive dual control safety element and preparation method |
| CN112899683A (en) * | 2019-12-03 | 2021-06-04 | 中兴通讯股份有限公司 | Ceramic dielectric filter surface metallization method, product and application thereof |
| CN111732456A (en) * | 2020-06-30 | 2020-10-02 | 苏州蓝晶研材料科技有限公司 | Ceramic conductive material and preparation method and application thereof |
| CN112500193A (en) * | 2020-11-09 | 2021-03-16 | 麦德美科技（苏州）有限公司 | Chemical roughening and metallization process of calcium magnesium titanate ceramic |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1156607C (en) | 2004-07-07 |
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