CN105541417B - Cover copper preparation method in a kind of aluminium nitride ceramics surface - Google Patents
Cover copper preparation method in a kind of aluminium nitride ceramics surface Download PDFInfo
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- CN105541417B CN105541417B CN201610103860.7A CN201610103860A CN105541417B CN 105541417 B CN105541417 B CN 105541417B CN 201610103860 A CN201610103860 A CN 201610103860A CN 105541417 B CN105541417 B CN 105541417B
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- copper
- nickel
- aluminium nitride
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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
Abstract
The invention discloses the preparation method that copper is covered on a kind of aluminium nitride ceramics surface, and the purpose is to be to provide the preparation method that a kind of technique is simple, and copper is covered on easy to operate aluminium nitride ceramics surface.The present invention be by the way that aluminium nitride ceramics is surface-treated, chemical nickel, heat treatment, pre-nickel plating, electro-coppering；So as to obtain aluminium nitride ceramics copper-clad panel, its layers of copper and Ceramic bond are good, and layers of copper compactness is good, and the conduction property of via hole is high, are adapted to make fine-line.
Description
Technical field
The present invention relates to a kind of aluminium nitride ceramics surface to cover copper preparation method, more particularly to one kind in aluminium nitride ceramics table
The aluminium nitride ceramics board manufacturing method of copper is covered in face and hole.
Background technology
Aluminum nitride ceramic substrate material is with its excellent thermal conductivity and air-tightness and electric property, extensively
It is general to be applied to power electronic, Electronic Packaging, mixing microelectronics and multi-chip module etc. field.Aluminum nitride ceramic substrate
Excellent heat conductivility makes it substitute aluminium oxide ceramic substrate, turns into the baseplate material being best suitable in high-end electronic industry, nitridation
The method of aluminium ceramic surface metallization mainly has：Mo-Mn methods, active metal method, chemical plating, vacuum vapor deposition method, chemical vapor deposition
Area method etc..But the above method really can not also 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, it is using non-balance magnetically controlled sputter method production ceramic copper-clad substrate.Chinese patent
The method that CN101798238.A " method of ceramic metallization " discloses ceramic metallization, is done using solution of gold nanoparticles
Activator, the ceramic substrate direct electroless nickel after activation, because using golden nanometer particle, causing production cost to rise.Japan lives
Friendly electrical industry Co., Ltd. patent of invention CN95108652.9 " has metallized ceramic substrate and its manufacturer of smooth plating layer
Method " is applied on aluminium nitride ceramic substrate biscuit and W/or Mo metallization slurry, flattens, sintering, and form above-mentioned one
Layer or multilayer coating etc..United States Patent (USP) U.A pat NO.4008343 enable chemical plating suitable using a kind of colloid palladium pretreatment fluid
Profit is carried out, but the adhesive force of matrix and coating is not strong.
The above method there are problems that to some extent, such as：Though vacuum method easily starts, price, batch life is not easy
Production；Metal nanoparticle, which makees activator, causes production cost to rise；Chemical vapour deposition technique, equipment are complicated, be not easy to produce etc..
Cover the electric conductor for functioning primarily as interconnection devices of the nitridation ceramic substrate after copper and pass the heat on device
The heat conductor gone out.Process for copper is covered on aluminium nitride ceramics surface, and its metal level directly uniformly, completely, adheres to Ceramic bond, coating
Intensity is high, substantially improves substrate radiating efficiency, process stabilizing, and mechanical property is preferable.Therefore copper is covered to work in aluminium nitride ceramics surface
The development of industry is significant.
The content of the invention
The present invention is to provide for a kind of aluminium nitride ceramics surface and covers copper preparation method, and covering the al nitride ceramic board after copper, it is golden
Category layer directly uniformly, completely, adhesive strength height, substantially improves substrate and radiated in substrate surface and hole with Ceramic bond, coating
Efficiency, process stabilizing, mechanical property are preferable.
Copper preparation method is covered on a kind of aluminium nitride ceramics surface, after aluminum nitride ceramic substrate surface pretreatment, passes through chemical nickel
1-3um electroless nickel layer is formed, makes nickel firm with Ceramic bond at high operating temperatures, then the preplating 0.1- in electroless nickel layer
0.5um pre-nickel plating, then the electro-coppering on pre-nickel plating.
Copper preparation method is covered on a kind of aluminium nitride ceramics surface, and described surface treatment is in 10%-20%
Sodium hydroxide solution in handle 2-4 minutes at room temperature, it is then that aluminium nitride ceramics surface clean is clean.
Copper preparation method, described chemical nickel are covered in a kind of aluminium nitride ceramics surface, and its flow is colloid
Palladium activation-ionic palladium activation-acceleration-chemical nickel.
Copper preparation method is covered on a kind of aluminium nitride ceramics surface, described heat treatment, is at 300-400 DEG C
At a high temperature of handle 1-3 hours.
Copper preparation method is covered on a kind of aluminium nitride ceramics surface, and described nickel preplating, its preplating liquid medicine can
To be sulfuric acid nickel, sulfamic acid nickel, chlorination nickel；Its preplating current density is 20-50ASF；Its is pre-
The plating time is 2-4 minutes.
Cover copper preparation method, described electro-coppering, its electro-coppering liquid medicine in a kind of aluminium nitride ceramics surface
It is low internal stress copper sulphate copper facing liquid medicine.
[brief description of the drawings]
For convenience of description, the present invention is described in detail by following preferably case study on implementation and accompanying drawings.
Fig. 1 is that the fabrication processing figure of copper is covered on the aluminium nitride ceramics surface of the embodiment of the present invention.
Fig. 2 is the structure chart of the one side aluminium nitride ceramics copper-clad panel of the embodiment of the present invention 1.
Fig. 3 is the structure chart of the two-sided aluminium nitride ceramics copper-clad panel of the embodiment of the present invention 2.
Label declaration in accompanying drawing
The aluminum nitride ceramic substrate layer of 101 copper plate, 102 pre-nickel plating, 103 electroless nickel layer, 104 nickel oxide layer 105
206 through holes
[embodiment]
Case study on implementation one
Fig. 1 gives the Making programme figure that copper is covered on aluminium nitride ceramics surface of the invention；Fig. 2 gives the embodiment of the present invention
The structure chart of 1 one side aluminium nitride ceramics copper-clad panel, below in conjunction with the accompanying drawings 1-2 copper is covered to one side aluminium nitride ceramics surface
Illustrated as method:
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）Heat 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.
Specific steps are described as follows：
Step 1, surface treatment 10；Thick 1.6mm al nitride ceramic board is placed in room in 10-20% sodium hydroxide solution
Temperature lower processing 2-4 minutes, then cleaned 10-30 minutes with ultrasonic wave, nitrogenized after obtaining pre-treatment with deionized water rinsing after taking-up
Aluminium ceramic substrate；
The supersonic frequency during ultrasonic cleaning is 40KHz, power 250-450W.
Step 2, chemical nickel 11；Chemical nickel flow is that colloid palladium activation-ionic palladium activation accelerates chemical nickel.Will be through
The al nitride ceramic board for crossing pre-treatment inserts 35 DEG C, in 5-8% colloidal pd activation solution, takes out sample after placing 10 minutes, spends
Ionized water rinses；Place into ionic palladium activating solution and handle 5 minutes, be placed in 85 DEG C of chemical nickel liquid, put again after acceleration processing
Sample is taken out after putting 8 minutes, the aluminum nitride ceramic substrate after obtaining chemical nickel with deionized water rinsing, the nickel dam in its surface and hole
Thickness is 1-3um；
Contain in described ionic palladium activating solution 1L：37% hydrochloric acid 270mL；Stannous chloride 5.5g；Colloid palladium concentrate
8mL；Surplus is deionized water；
The concentration of nickel sulfate is 15/L in the chemical nickel liquid, and ortho phosphorous acid na concn is 20g/L, and the concentration of boric acid is
25g/L, the concentration of sodium citrate is 45g/L.
Step 3, heat treatment 12.It is small that the al nitride ceramic board for having electroless nickel layer is handled into 1-3 at a high temperature of 300-400 DEG C
When, the electroless nickel layer contacted with aluminium nitride ceramics plate surface is aoxidized, the extremely strong nickel oxide layer of generation tack.
Step 4, nickel preplating 13；Hydrochloric acid solution cleaning through 0.5-1.0%, after removing electroless nickel layer surface oxidation nickel, in ammonia
In base sulfonic acid nickel-plating liquid, with current density 20-50ASF high current preplating 2-4 minutes, nickel preplating is formed in ceramic surface and hole
Layer.
The composition and concentration of the sulfamic acid nickel liquid be：Nickel sulfamic acid 65-75g/L, secondary nickel chloride are 15-35g/
L, the concentration of boric acid is 35-45g/L.
Step 5, electro-coppering 14；By the aluminium nitride ceramics for having pre-nickel plating by low stress electroplate copper bath electroplate copper, in groove
During 25 DEG C of liquid temperature degree, electroplated 60 minutes with current density 2.0A/ square decimeters, copper layer thickness reaches 18um in surface and hole, most
Aluminium nitride ceramics copper-clad panel is formed afterwards.
The low stress electrolytic copper plating solution is cupric sulfate pentahydrate, 98% sulfuric acid, hydrochloric acid, open cylinder agent, the mixing of low stress brightener
Liquid, anode are phosphorus copper plate, are contained in 1L electroplate liquids：Cupric sulfate pentahydrate 200g；98% sulfuric acid 55g；Hydrochloric acid 50mg；Open
Cylinder agent 3.5ml；Low stress brightener 0.3ml；Surplus is deionized water.
The present embodiment makes the one side aluminium nitride ceramics copper-clad panel of production, and its metal level is combined good with ceramic primary surface
Good, compactness of electroplating is good, and metal level structural constituent is uniform, is adapted to make fine-line.
Case study on implementation two
Fig. 1 gives the Making programme figure that copper is covered on aluminium nitride ceramics surface of the invention；Fig. 3 gives the embodiment of the present invention
The structure chart of 2 two-sided aluminium nitride ceramics copper-clad panel, below in conjunction with the accompanying drawings 1,3 pair of two-sided aluminium nitride ceramics surface cover copper
Making is illustrated:
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）Heat 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 two-sided covers
Copper.
Specific steps are described as follows：
Step 1, surface treatment 10；Porose al nitride ceramic board will be bored and be placed in room in 10-20% sodium hydroxide solution
Temperature lower processing 2-4 minutes, then cleaned 10-30 minutes with ultrasonic wave, nitrogenized after obtaining pre-treatment with deionized water rinsing after taking-up
Aluminium ceramic substrate；
The supersonic frequency during ultrasonic cleaning is 40KHz, power 250-450W.
Step 2, chemical nickel 11；Chemical nickel flow is that colloid palladium activation-ionic palladium activation accelerates chemical nickel.Will be through
The aluminum nitride ceramic substrate for crossing pre-treatment inserts 35 DEG C, in 5-8% colloidal pd activation solution, places and takes after the completion of reaction in 10 minutes
Go out sample, use deionized water rinsing；Place into ionic palladium activating solution and handle 5 minutes, be placed on 85 DEG C of change after acceleration processing again
Learn in nickel liquid, sample is taken out after placing 8 minutes, the aluminum nitride ceramic substrate after obtaining chemical nickel with deionized water rinsing, its surface
And the nickel layer thickness in hole is 1-3um；
Contain in described ionic palladium activating solution 1L：37% hydrochloric acid 270mL；Stannous chloride 5.5g；Colloid palladium concentrate
8mL；Surplus is deionized water；
The concentration of nickel sulfate is 15/L in the chemical nickel liquid, and ortho phosphorous acid na concn is 20g/L, and the concentration of boric acid is
25g/L, the concentration of sodium citrate is 45g/L.
Step 3, heat treatment 12.It is small that the aluminium nitride ceramics for having electroless nickel layer is handled into 1-3 at a high temperature of 300-400 DEG C
When, the electroless nickel layer contacted with aluminum nitride ceramic substrate surface is aoxidized, the extremely strong nickel oxide layer of generation tack.
Step 4, nickel preplating 13；Hydrochloric acid solution cleaning through 0.5-1.0%, after removing electroless nickel layer surface oxidation nickel, in ammonia
In base sulfonic acid nickel-plating liquid, with current density 20-50ASF high current preplating 2-4 minutes, nickel preplating is formed in ceramic surface and hole
Layer.
The composition and concentration of the sulfamic acid nickel liquid be：Nickel sulfamic acid 65-75g/L, secondary nickel chloride are 15-35g/
L, the concentration of boric acid is 35-45g/L.
Step 5, electro-coppering 14；By the aluminium nitride ceramics for having pre-nickel plating by low stress electroplate copper bath electroplate copper, in groove
During 25 DEG C of liquid temperature degree, electroplated 60 minutes with current density 2.0A/ square decimeters, copper layer thickness reaches 18um in surface and hole, most
The aluminium nitride ceramics of surface metalation is formed afterwards.
The low stress electrolytic copper plating solution is cupric sulfate pentahydrate, 98% sulfuric acid, hydrochloric acid, open cylinder agent, the mixing of low stress brightener
Liquid, anode are phosphorus copper plate, are contained in 1L electroplate liquids：Cupric sulfate pentahydrate 200g；98% sulfuric acid 55g；Hydrochloric acid 50mg；Open
Cylinder agent 3.5ml；Low stress brightener 0.3ml；Surplus is deionized water.
The present embodiment makes the two-sided aluminium nitride ceramics copper-clad plate of production, and its metal level is well combined with ceramic primary surface,
Compactness of electroplating is good, and metal level structural constituent is uniform, and the conduction property of through hole is good, is adapted to production fine-line.
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, wherein the equipment and structure be not described in detail to the greatest extent are construed as giving reality with the common mode in this area
Apply；Those skilled in the art can make various deformations or amendments within the scope of the claims, and this has no effect on the present invention's
Substantive content.
Claims (5)
1. the preparation method that copper is covered on a kind of aluminium nitride ceramics surface, it is characterised in that it includes six step process： 1）Surface
Processing；2）Chemical nickel；3）Heat treatment；4）Nickel preplating；5）Electro-coppering；
Described chemical nickel, its flow are colloid palladium activation-ionic palladium activation-acceleration-chemical nickel.
2. copper preparation method is covered on a kind of aluminium nitride ceramics surface according to patent requirements 1, it is characterised in that：Described surface
Processing is to handle 2-4 minutes at room temperature in 10%-20% sodium hydroxide solution, then does aluminium nitride ceramics surface clean
Only.
3. copper preparation method is covered on a kind of aluminium nitride ceramics surface according to patent requirements 1, it is characterised in that：At described heat
Reason, it is that 1-3 hours are handled at a high temperature of 300-400 DEG C.
4. copper preparation method is covered on a kind of aluminium nitride ceramics surface according to patent requirements 1, it is characterised in that：Described preplating
Nickel, its preplating liquid medicine can be sulfuric acid nickel, sulfamic acid nickel, chlorination nickel；Its preplating current density is 20-
50ASF；Its preplating time is 1-4 minutes.
5. copper preparation method is covered on a kind of aluminium nitride ceramics surface according to patent requirements 1, it is characterised in that：Described plating
Copper, its electro-coppering liquid medicine are low internal stress copper sulphate copper facing liquid medicine.
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| 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 |
| 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 |
| 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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| 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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