CN105541417A - Production method for cladding copper on surface of aluminum nitride ceramic - Google Patents
Production method for cladding copper on surface of aluminum nitride ceramic Download PDFInfo
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- CN105541417A CN105541417A CN201610103860.7A CN201610103860A CN105541417A CN 105541417 A CN105541417 A CN 105541417A CN 201610103860 A CN201610103860 A CN 201610103860A CN 105541417 A CN105541417 A CN 105541417A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
- C04B41/90—Coating or impregnation for obtaining at least two superposed coatings having different compositions at least one coating being a metal
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- Electroplating Methods And Accessories (AREA)
Abstract
The invention discloses a production method for cladding copper on the surface of an aluminum nitride ceramic and aims at achieving the effects that the process is simple, and operation is convenient. The method comprises the steps of surface treatment of the aluminum nitride ceramic, chemical nickel treatment, heat treatment, nickel layer preplating and copper electroplating, so that a aluminum nitride ceramic surface copper-clad plate is obtained. A copper layer of the copper-clad plate can be bound with the ceramic well and is good in compactness, conducting performance of each conducting hole is high, and the method is suitable for producing fine lines.
Description
Technical field
The present invention relates to a kind of aluminium nitride ceramics surface and covered copper making method, particularly relate to a kind of aluminium nitride ceramics board manufacturing method covering copper in aluminium nitride ceramics surface and hole.
Background technology
Aluminum nitride ceramic substrate material with its excellent thermal conductivity and resistance to air loss and electric property, extensively
Generally be applied to the fields such as power electronic, Electronic Packaging, mixing microelectronics and multi-chip module.The heat conductivility of aluminum nitride ceramic substrate excellence makes its alternative aluminium oxide ceramic substrate, and become optimal baseplate material in high-end electronic industry, the method for aluminium nitride ceramics surface metalation mainly contains: Mo-Mn method, active metal method, electroless plating, vacuum vapor deposition method, chemical Vapor deposition process etc.But aforesaid method also cannot really be applied in practice.
At present, Chinese patent CN200510047855.0 " ceramic-substrate sputtered copper foil production method " discloses ceramic-substrate sputtered copper foil production method, is to adopt non-balance magnetically controlled sputter method to produce ceramic copper-clad substrate.Chinese patent CN101798238.A " method of ceramic metallization " discloses the method for ceramic metallization, is to adopt solution of gold nanoparticles to make activator, the ceramic substrate direct electroless nickel after activation, because using golden nanometer particle, causes production cost to rise.The metallization slip of SEI Corporation patent of invention CN95108652.9 " has metallized ceramic substrate and the manufacture method thereof of smooth plating layer " on aluminium nitride ceramic substrate biscuit coating and W/ or Mo, flatten, sinter, and form one or more layers above-mentioned coating etc.United States Patent (USP) U.ApatNO.4008343 uses a kind of colloidal palladium pretreatment fluid that electroless plating can be carried out smoothly, but the sticking power of matrix and coating is not strong.
There are some problems to some extent in aforesaid method, as: though vacuum method easily starts, price, not easily to produce in batches; Metal nanoparticle makees activator causes production cost to rise; Chemical Vapor deposition process, equipment is complicated, not easily produces etc.
The major function covering the nitrogenize ceramic substrate after copper is as the electric conductor of interconnect devices and the thermal conductor that the heat on device spread out of.Process for copper is covered on aluminium nitride ceramics surface, and directly and Ceramic bond, coating is even, complete, and adhesion strength is high, and greatly improve substrate radiating efficiency, process stabilizing, mechanical property is better for its metal level.Therefore to cover copper significant to industrial expansion on aluminium nitride ceramics surface.
Summary of the invention
The present invention will provide a kind of aluminium nitride ceramics surface to cover copper making method, and cover its metal level of the al nitride ceramic board after copper direct and Ceramic bond in substrate surface and hole, coating is even, complete, adhesion strength is high, greatly improve substrate radiating efficiency, process stabilizing, mechanical property is better.
Copper making method is covered on a kind of aluminium nitride ceramics surface, after aluminum nitride ceramic substrate surface pretreatment, form the electroless nickel layer of 1-3um by chemical nickel, make at high operating temperatures nickel and Ceramic bond firm, the pre-nickel plating of preplating 0.1-0.5um in electroless nickel layer, then electro-coppering on pre-nickel plating again.
Copper making method is covered on a kind of aluminium nitride ceramics surface, and described surface treatment is at 10%-20%
Sodium hydroxide solution in process 2-4 minute, then by clean for aluminium nitride ceramics surface cleaning under room temperature.
Copper making method is covered, described chemical nickel in a kind of aluminium nitride ceramics surface, and its flow process is colloid
Palladium activation-ionic palladium activation-acceleration-chemical nickel.
Copper making method is covered, described thermal treatment in a kind of aluminium nitride ceramics surface, is at 300-400 DEG C
High temperature under process 1-3 hour.
Copper making method is covered, described nickel preplating in a kind of aluminium nitride ceramics surface, and its preplating liquid medicine can
To be single nickel salt nickel plating, sulfamic acid nickel, nickelous chloride nickel plating; Its preplating current density is 20-50ASF; Its preplating time is 2-4 minute.
Copper making method is covered, described electro-coppering, its electro-coppering liquid medicine in a kind of aluminium nitride ceramics surface
Low internal stress copper sulfate copper facing liquid medicine.
[accompanying drawing explanation]
For convenience of explanation, the present invention is described in detail by following preferably case study on implementation and accompanying drawing.
Fig. 1 is the surperficial fabrication processing figure covering copper of aluminium nitride ceramics of the embodiment of the present invention.
Fig. 2 is the structure iron of the one side aluminium nitride ceramics copper-clad panel of the embodiment of the present invention 1.
Fig. 3 is the structure iron of the two-sided aluminium nitride ceramics copper-clad panel of the embodiment of the present invention 2.
Label declaration in accompanying drawing
101 copper plate 102 pre-nickel plating 103 electroless nickel layer 104 nickel oxide layer 105 aluminum nitride ceramic substrate layer 206 through holes
[embodiment]
Case study on implementation one
Fig. 1 gives the Making programme figure that copper is covered on aluminium nitride ceramics of the present invention surface; Fig. 2 gives the structure iron of the one side aluminium nitride ceramics copper-clad panel of the embodiment of the present invention 1, covers copper making method illustrated below in conjunction with accompanying drawing 1-2 to one side aluminium nitride ceramics surface:
The making idiographic flow that copper is covered on aluminium nitride ceramics surface is as follows: 1) surface treatment 10; 2) chemical nickel 11; 3) thermal treatment 12; 4) nickel preplating 13; 5) electro-coppering 14.
The aluminium nitride ceramics copper-clad panel structure formed is: copper plate 101, pre-nickel plating 102, electroless nickel layer 103, nickel oxide layer 104, aluminum nitride ceramic substrate layer 105.
Concrete steps are described below:
Step 1, surface treatment 10; Process 2-4 minute under the al nitride ceramic board of thick 1.6mm being placed in the sodium hydroxide solution room temperature of 10-20%, then use ultrasonic cleaning 10-30 minute, after taking-up, obtain aluminum nitride ceramic substrate after pre-treatment with deionized water rinsing;
Ultrasonic frequency during described ultrasonic cleaning is 40KHz, and power is 250-450W.
Step 2, chemical nickel 11; Chemical nickel flow process is that chemical nickel is accelerated in the activation of colloidal palladium activation-ionic palladium.Al nitride ceramic board through pre-treatment is inserted 35 DEG C, in the colloidal pd activation solution of 5-8%, place and take out sample after 10 minutes, with deionized water rinsing; Put into ionic palladium activation solution process 5 minutes again, be placed in the chemical nickel liquid of 85 DEG C again, place and take out sample after 8 minutes, obtain the aluminum nitride ceramic substrate after chemical nickel with deionized water rinsing after accelerating process, the nickel layer thickness in its surperficial and hole is 1-3um;
Contain in described ionic palladium activation solution 1L: 37% hydrochloric acid 270mL; Tin protochloride 5.5g; Colloidal palladium concentrated solution 8mL; Surplus is deionized water;
In described chemical nickel liquid, the concentration of single nickel salt is 15/L, and ortho phosphorous acid na concn is 20g/L, and the concentration of boric acid is 25g/L, and the concentration of Trisodium Citrate is 45g/L.
Step 3, thermal treatment 12.By there being the al nitride ceramic board of electroless nickel layer to process 1-3 hour under the high temperature of 300-400 DEG C, the electroless nickel layer with al nitride ceramic board surface contact being oxidized, generating the nickel oxide layer that tack is extremely strong.
Step 4, nickel preplating 13; Hydrochloric acid soln through 0.5-1.0% cleans, and after removing electroless nickel layer surface oxidation nickel, in sulfamic acid nickel liquid, with current density 20-50ASF big current preplating 2-4 minute, forms pre-nickel plating in ceramic surface and hole.
Composition and the concentration of described sulfamic acid nickel liquid are: nickel sulfamic acid 65-75g/L, and secondary nickelous chloride is 15-35g/L, and the concentration of boric acid is 35-45g/L.
Step 5, electro-coppering 14; To have the aluminium nitride ceramics of pre-nickel plating by low-stress electroplate copper bath electroplate copper, when tank liquor temperature 25 DEG C, electroplate 60 minutes with current density 2.0A/ square decimeter, in surface and hole, copper layer thickness reaches 18um, finally forms aluminium nitride ceramics copper-clad panel.
Described low-stress electrolytic copper plating solution is cupric sulfate pentahydrate, 98% sulfuric acid, hydrochloric acid, open cylinder agent, the mixed solution of low-stress brightening agent, and anode is phosphorus copper plate, contains in 1L electroplate liquid: cupric sulfate pentahydrate 200g; 98% sulfuric acid 55g; Hydrochloric acid 50mg; Open cylinder agent 3.5ml; Low-stress brightening agent 0.3ml; Surplus is deionized water.
The present embodiment makes the one side aluminium nitride ceramics copper-clad panel produced, and well, compactness of electroplating is good for its metal level and ceramic base surface bonding, and metal level structural constituent is even, is applicable to making fine-line.
Case study on implementation two
Fig. 1 gives the Making programme figure that copper is covered on aluminium nitride ceramics of the present invention surface; Fig. 3 gives the structure iron of the two-sided aluminium nitride ceramics copper-clad panel of the embodiment of the present invention 2, is illustrated the making that copper is covered on two-sided aluminium nitride ceramics surface below in conjunction with accompanying drawing 1,3:
The making idiographic flow that copper is covered on aluminium nitride ceramics surface is as follows: 1) surface treatment 10; 2) chemical nickel 11; 3) thermal treatment 12; 4) nickel preplating 13; 5) electro-coppering 14.
The aluminium nitride ceramics copper-clad panel structure formed is: copper plate 101, pre-nickel plating 102, electroless nickel layer 103, nickel oxide layer 104, aluminum nitride ceramic substrate layer 105, through hole 206.The present embodiment aluminium nitride ceramics copper-clad panel is double-sided copper-clad.
Concrete steps are described below:
Step 1, surface treatment 10; Process 2-4 minute under the al nitride ceramic board being drilled with hole being placed in the sodium hydroxide solution room temperature of 10-20%, then use ultrasonic cleaning 10-30 minute, after taking-up, obtain aluminum nitride ceramic substrate after pre-treatment with deionized water rinsing;
Ultrasonic frequency during described ultrasonic cleaning is 40KHz, and power is 250-450W.
Step 2, chemical nickel 11; Chemical nickel flow process is that chemical nickel is accelerated in the activation of colloidal palladium activation-ionic palladium.Aluminum nitride ceramic substrate through pre-treatment is inserted 35 DEG C, in the colloidal pd activation solution of 5-8%, place and within 10 minutes, reacted rear taking-up sample, with deionized water rinsing; Put into ionic palladium activation solution process 5 minutes again, be placed in the chemical nickel liquid of 85 DEG C again, place and take out sample after 8 minutes, obtain the aluminum nitride ceramic substrate after chemical nickel with deionized water rinsing after accelerating process, the nickel layer thickness in its surperficial and hole is 1-3um;
Contain in described ionic palladium activation solution 1L: 37% hydrochloric acid 270mL; Tin protochloride 5.5g; Colloidal palladium concentrated solution 8mL; Surplus is deionized water;
In described chemical nickel liquid, the concentration of single nickel salt is 15/L, and ortho phosphorous acid na concn is 20g/L, and the concentration of boric acid is 25g/L, and the concentration of Trisodium Citrate is 45g/L.
Step 3, thermal treatment 12.By there being the aluminium nitride ceramics of electroless nickel layer to process 1-3 hour under the high temperature of 300-400 DEG C, the electroless nickel layer with aluminum nitride ceramic substrate surface contact being oxidized, generating the nickel oxide layer that tack is extremely strong.
Step 4, nickel preplating 13; Hydrochloric acid soln through 0.5-1.0% cleans, and after removing electroless nickel layer surface oxidation nickel, in sulfamic acid nickel liquid, with current density 20-50ASF big current preplating 2-4 minute, forms pre-nickel plating in ceramic surface and hole.
Composition and the concentration of described sulfamic acid nickel liquid are: nickel sulfamic acid 65-75g/L, and secondary nickelous chloride is 15-35g/L, and the concentration of boric acid is 35-45g/L.
Step 5, electro-coppering 14; To the aluminium nitride ceramics of pre-nickel plating be had by low-stress electroplate copper bath electroplate copper, when tank liquor temperature 25 DEG C, electroplate 60 minutes with current density 2.0A/ square decimeter, surface and hole in copper layer thickness reach 18um, finally form the aluminium nitride ceramics of surface metalation.
Described low-stress electrolytic copper plating solution is cupric sulfate pentahydrate, 98% sulfuric acid, hydrochloric acid, open cylinder agent, the mixed solution of low-stress brightening agent, and anode is phosphorus copper plate, contains in 1L electroplate liquid: cupric sulfate pentahydrate 200g; 98% sulfuric acid 55g; Hydrochloric acid 50mg; Open cylinder agent 3.5ml; Low-stress brightening agent 0.3ml; Surplus is deionized water.
The present embodiment makes the two-sided aluminium nitride ceramics copper-clad plate of producing, and well, compactness of electroplating is good for its metal level and ceramic base surface bonding, and metal level structural constituent is even, and the conduction property of through hole is good, is applicable to production fine-line.
Above specific embodiments of the invention are described.It is to be appreciated that the present invention is not limited to above-mentioned particular implementation, the equipment wherein do not described in detail to the greatest extent and structure are construed as to be implemented with the usual manner in this area; Those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (6)
1. a making method for copper is covered on aluminium nitride ceramics surface, and it is characterized in that, it comprises six step process: 1) surface treatment; 2) chemical nickel; 3) thermal treatment; 4) nickel preplating; 5) electro-coppering.
2. copper making method is covered on a kind of aluminium nitride ceramics surface according to patent requirements 1, it is characterized in that: described surface treatment processes 2-4 minute under room temperature in the sodium hydroxide solution of 10%-20%, then by clean for aluminium nitride ceramics surface cleaning.
3. copper making method is covered on a kind of aluminium nitride ceramics surface according to patent requirements 1, it is characterized in that: described chemical nickel, and its flow process is colloidal palladium activation-ionic palladium activation-acceleration-chemical nickel.
4. copper making method is covered on a kind of aluminium nitride ceramics surface according to patent requirements 1, it is characterized in that: described thermal treatment, is process 1-3 hour under the high temperature of 300-400 DEG C.
5. copper making method is covered on a kind of aluminium nitride ceramics surface according to patent requirements 1, it is characterized in that: described nickel preplating, and its preplating liquid medicine can be single nickel salt nickel plating, sulfamic acid nickel, nickelous chloride nickel plating; Its preplating current density is 20-50ASF; Its preplating time is 1-4 minute.
6. copper making method is covered on a kind of aluminium nitride ceramics surface according to patent requirements 1, it is characterized in that: described electro-coppering, and its electro-coppering liquid medicine is low internal stress copper sulfate copper facing liquid medicine.
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| CN201610103860.7A CN105541417B (en) | 2016-02-26 | 2016-02-26 | Cover copper preparation method in a kind of aluminium nitride ceramics surface |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110167258A (en) * | 2019-05-24 | 2019-08-23 | 上海温良昌平电器科技股份有限公司 | A kind of aluminium plating copper substrate structure and its preparation process |
| CN111592382A (en) * | 2020-04-26 | 2020-08-28 | 江苏富乐德半导体科技有限公司 | Surface roughening method for aluminum nitride ceramic substrate |
| CN111751177A (en) * | 2020-06-08 | 2020-10-09 | 江苏富乐德半导体科技有限公司 | Preparation method of copper-clad ceramic substrate tensile test sample |
| CN113603474A (en) * | 2021-08-17 | 2021-11-05 | 南通大学 | Preparation method of transparent ceramic optical fiber with core-spun structure |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000226274A (en) * | 1998-12-01 | 2000-08-15 | Aichi Steel Works Ltd | Production of ceramic-metal conjugate |
| CN105801179A (en) * | 2015-04-30 | 2016-07-27 | 深圳市环基实业有限公司 | Direct metallization method for ceramic substrate |
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2016
- 2016-02-26 CN CN201610103860.7A patent/CN105541417B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000226274A (en) * | 1998-12-01 | 2000-08-15 | Aichi Steel Works Ltd | Production of ceramic-metal conjugate |
| CN105801179A (en) * | 2015-04-30 | 2016-07-27 | 深圳市环基实业有限公司 | Direct metallization method for ceramic substrate |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110167258A (en) * | 2019-05-24 | 2019-08-23 | 上海温良昌平电器科技股份有限公司 | A kind of aluminium plating copper substrate structure and its preparation process |
| CN111592382A (en) * | 2020-04-26 | 2020-08-28 | 江苏富乐德半导体科技有限公司 | Surface roughening method for aluminum nitride ceramic substrate |
| CN111592382B (en) * | 2020-04-26 | 2021-12-17 | 江苏富乐德半导体科技有限公司 | Surface roughening method for aluminum nitride ceramic substrate |
| CN111751177A (en) * | 2020-06-08 | 2020-10-09 | 江苏富乐德半导体科技有限公司 | Preparation method of copper-clad ceramic substrate tensile test sample |
| CN111751177B (en) * | 2020-06-08 | 2022-11-04 | 江苏富乐华半导体科技股份有限公司 | Preparation method of copper-clad ceramic substrate tensile test sample |
| CN113603474A (en) * | 2021-08-17 | 2021-11-05 | 南通大学 | Preparation method of transparent ceramic optical fiber with core-spun structure |
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Address after: 518125 No.9, Xinfa 2nd Road, Xinqiao community, Xinqiao street, Bao'an District, Shenzhen City, Guangdong Province Patentee after: Shenzhen Dinghua Xintai Technology Co.,Ltd. Address before: 518125 building 7, the third batch of Xinfa Industrial Zone, Shajing Xinqiao, Bao'an District, Shenzhen City, Guangdong Province Patentee before: ACCELERATED PRINTED CIRCUIT BOARD Co.,Ltd. |