CN110055533A - Coarsening solution is used in a kind of surface treatment of diamond/copper semiconductor composite - Google Patents
Coarsening solution is used in a kind of surface treatment of diamond/copper semiconductor composite Download PDFInfo
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- CN110055533A CN110055533A CN201910479269.5A CN201910479269A CN110055533A CN 110055533 A CN110055533 A CN 110055533A CN 201910479269 A CN201910479269 A CN 201910479269A CN 110055533 A CN110055533 A CN 110055533A
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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
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1827—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment only one step pretreatment
- C23C18/1834—Use of organic or inorganic compounds other than metals, e.g. activation, sensitisation with polymers
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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
- C23C18/1882—Use of organic or inorganic compounds other than metals, e.g. activation, sensitisation with polymers
-
- 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/18—Acidic compositions for etching copper or alloys thereof
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemically Coating (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
A kind of diamond/copper semiconductor composite surface treatment coarsening solution, the present invention relates to a kind of surface treatment coarsening solutions, to solve the problems, such as that it is non-uniform that traditional coarsening solution is roughened, a kind of diamond/copper semiconductor composite surface treatment coarsening solution provided by the invention, the coarsening solution includes the A liquid for etching diamond and the B liquid of etch copper.The beneficial effects of the present invention are, compared with traditional roughening process, obtained material has preferably roughening effect after carrying out roughening treatment to diamond/copper based composites surface using new coarsening solution, and the nickel gold plate after plating is smooth, bright, binding force and heat-resist.
Description
Technical field
The present invention relates to a kind of surface treatment coarsening solutions, and in particular to a kind of diamond/copper semiconductor composite surface
Coarsening solution is used in processing.
Background technique
Diamond/copper composite material is made of high heat conductance, the diamond of low bulk and the good copper of heating conduction
Composite material that is non-solid-solution and can playing each constituent element characteristic, preparing novel microelectronic encapsulating material has lot of advantages,
It can replace and be widely used at present the materials such as Cu, W-Cu, Al/SiC and AlN, in various microwave diodes, the pedestal of integrated circuit
With all had a wide range of applications in mobile phone.But diamond/copper material causes weldability poor due to the introducing of diamond,
Although having certain intensity and thermal conductivity and matched thermal expansion coefficient, as encapsulating material, diamond/copper is multiple for it
Condensation material needs to carry out it before being put into use to be electroplated/and the method for chemical plating makes it meet thermal diffusivity and weldability.Usually
In the case of, industry is met using the method for chemical plating in diamond/copper substrate surface plating one layer of metal or alloy at present
It is required that wherein the pretreating process before plating technic has great influence to entire plating technic.
Diamond/copper semiconductor composite belongs to apolar substance, surface according to traditional coarsing processing method,
It is not in place or sting erosion phenomenon to be then easy to happen roughening.Because the wellability between diamond and water isopolarity medium is poor, tradition
Liquid medicine usually contains nitric acid solution, the heating carried out in use process, and the nitric acid solution after heating is aoxidized with diamond/copper
Reaction, diamond properties are stablized, and surface treatment difficulty is big.There is copper in mixture, copper is more active, general processing method, and copper is easy
Overtreating, and diamond does not react.Diamond corrosion is not in place, in fact it could happen that and diamond surface is not roughened, and if
It is roughened not in place, the phenomenon that being usually present plating leakage after diamond/copper composite material chemical nickel plating；Roughening excessively, is easy to appear pair
Copper stings erosion phenomenon, and pit occurs in entire substrate surface, cannot obtain even curface, generates bad shadow to subsequent plating ni au
It rings.
Conventional roughening treatment mode and effect are as follows at present:
A. nitric acid
Diamond/copper composite material is surface-treated using nitric acid solution, sample surfaces copper be etched it is too fast, C's
Be roughened it is limited, it is asynchronous, flat surface cannot be obtained；
B. sulfuric acid
Diamond/copper composite material is surface-treated using sulfuric acid solution, excessive concentration be easy to cause diamond at
The carbonization divided, concentration is too low can not to be roughened diamond components；
C. hydrochloric acid
It is unable to reach the purpose of roughening sample；
D. sandblasting
Diamond particles can not be roughened, and increase the roughness on substrate sample surface, granular sensation is big, and surface is smooth,
It can not carry out nickel plating/gold process perhaps；
E. manual polishing
The impurity component that surface can only be removed cannot play the roughing in surface force limited of diamond particles substantially
Roughening effect.
Finding a kind of suitable coarsening solution has great influence to the surface treatment of diamond/copper composite material.
Summary of the invention
A kind of new coarsening solution effectively carries out roughening treatment to diamond/copper composite material surface, solves traditional roughening
Problem bring the plating leakage and coating (ni au) bright property, binding force and poor heat resistance of subsequent technique the problems such as.
Successively successively diamond/copper based composites are surface-treated using A, B liquid.
Wherein A liquid forms are as follows: (alkaline group, etch diamond)
Potassium hydroxide, 15-25g/L；
Copper sulphate, 10-20g/L；
Potassium permanganate, 5-10g/L；
Potassium hypophosphite, 1-2g/L；
Triethanolamine, 5-10ml/L；
Surplus, pure water.
Above-mentioned A liquid configuration method:
A. the potassium hydroxide for weighing mass ratio is soluble in water, is thoroughly mixed uniformly, obtains uniform potassium hydroxide
Solution；
B. the anhydrous cupric sulfate of proportion mass parts is added into above-mentioned potassium hydroxide solution, 10-20g/L is mixed equal
It is even；
C. the potassium permanganate of proportion mass parts is added into above-mentioned mixed solution, mass fraction 5-10g/L is mixed equal
It is even；
D. the potassium hypophosphite of proportion mass parts is added into above-mentioned mixed solution, 1-2g/L is mixed evenly；
E. the triethanolamine of proportion mass parts is added into above-mentioned mixed solution, 5-10g/L is mixed evenly；
F. pure water is added into above-mentioned mixed solution, constant volume is mixed evenly.
B liquid composition are as follows: (acid group, microetch copper)
Copper chloride, 10-20g/L；
Fluorine potassium carbonate, 5-10g/L；
Hydrochloric acid, mass fraction 31%, 40-55ml/L；
Sulfamic acid sodium 1-3g/L；
Surplus, pure water.
The configuration method of B liquid:
A. the industrial concentrated hydrochloric acid that the mass fraction for measuring volume ratio is 31% is soluble in water, stirs while being added
It mixes, obtains uniform hydrochloric acid solution；
A. the copper chloride for weighing mass ratio is dissolved in above-mentioned hydrochloric acid solution, is thoroughly mixed uniformly；
B. the fluorine potassium carbonate of proportion mass parts is added into above-mentioned mixed solution, 5-10g/L is mixed evenly；
C. the sulfamic acid sodium of proportion mass parts is added into above-mentioned mixed solution, mass fraction 1-3g/L is mixed
Uniformly；
D. pure water is added into above-mentioned mixed solution, constant volume is mixed evenly.
Application method:
A. the diamond/copper composite material after oil removing being cleaned is put into coarsening solution A liquid, uses glass bar at 50-60 DEG C
Agitating solution is suspended in diamond/copper composite material in coarsening solution, and each face of substrate can adequately contact solution；For
There is the diamond Copper base material of punching, plastics filament or special hanger fixing substrate can be used, suspends and hang in the solution, 5 ±
It is clean with pure water rinsing after 1min.
B. the diamond Copper base material immersion rinsed well after being roughened above-mentioned in A liquid is suspended in B liquid, room temperature (20 ±
10 DEG C), (20 ± 10 DEG C) of low temperature drying, to subsequent machining technology.
The beneficial effects of the present invention are multiple to diamond/copper base using new coarsening solution compared with traditional roughening process
Condensation material surface, which carries out the material obtained after roughening treatment, has preferably roughening effect, and the nickel coating after plating is smooth, bright,
Binding force and heat-resist.
Detailed description of the invention
The SEM figure that Fig. 1-Fig. 4 is roughening treatment scheme 1-4 in embodiment 1.
Specific embodiment
Embodiment 1
Solution components, wherein A liquid forms are as follows:
Potassium hydroxide, 20g/L；
Copper sulphate, 15g/L；
Potassium permanganate, 5g/L；
Potassium hypophosphite, 1g/L；
Triethanolamine, 8ml/L；
Surplus, pure water.
Configuration method:
A. it weighs 20g potassium hydroxide to be dissolved in 800ml water, is thoroughly mixed uniformly, it is molten to obtain uniform potassium hydroxide
Liquid；
B. 15g anhydrous cupric sulfate is added into above-mentioned potassium hydroxide solution, is mixed evenly；
C. 5g potassium permanganate is added into above-mentioned mixed solution, is mixed evenly；
D. 1g potassium hypophosphite is added into above-mentioned mixed solution, is mixed evenly；
E. 8ml triethanolamine is added into above-mentioned mixed solution, is mixed evenly；
F. pure water is added into above-mentioned mixed solution, constant volume 1L is mixed evenly, for use.
B liquid composition are as follows: (acid group, microetch copper)
Copper chloride, 15g/L；
Fluorine potassium carbonate, 5g/L；
Hydrochloric acid, mass fraction 31%, 45ml/L；
Sulfamic acid sodium 2g/L；
Surplus, pure water.
Configuration method:
A. it measures the industrial concentrated hydrochloric acid that 45ml mass fraction is 31% to be dissolved in 800ml water, be stirred while being added,
Obtain uniform hydrochloric acid solution；
A. it weighs 15g copper chloride to be dissolved in above-mentioned hydrochloric acid solution, be thoroughly mixed uniformly；
B. 5g fluorine potassium carbonate is added into above-mentioned mixed solution, is mixed evenly；
C. 2g amino acid acid sodium is added into above-mentioned mixed solution, is mixed evenly；
D. pure water is added into above-mentioned mixed solution, constant volume 1L is mixed evenly.
Application method:
Step 1 takes appropriate A liquid in container, and the diamond/copper composite material after oil removing is cleaned is put into coarsening solution A liquid
In, glass bar agitating solution is used at 50-60 DEG C, is suspended in diamond/copper composite material in coarsening solution, each face energy of substrate
Enough adequately contact solution；For there is the diamond Copper base material of punching, base can be fixed with plastics filament or special hanger
Material suspends and hangs in the solution, clean with pure water rinsing after 5 ± 1min.
Step 2 takes appropriate B liquid in container, and the above-mentioned diamond Copper base material rinsed well after roughening in A liquid is soaked
Bubble is suspended in B liquid, room temperature (20 ± 10 DEG C), low temperature drying, to subsequent machining technology.
Comparative experiments group, comparative experiments group roughening treatment scheme are as follows:
Scheme one: pure water
Scheme two: polishing
Scheme three: nitric acid solution (10%)
Scheme four: A, B liquid provided by the invention.
The roughening operating method of scheme one, three, four and A, B liquid processing method in the present invention are completely the same, and scheme two uses
The operating method of sandblasting polishing will after the sampling grinding of treated diamond copper base, surface sweeping electricity under the microscope its be roughened feelings
Condition.As a result as shown in the picture, as can be seen from the figure:
SEM schemes after the roughening of diamond/copper composite material
Surface is carried out using the diamond/copper substrate after coarsening solution roughening treatment described in the technical solution in the present invention
Plating technic, first chemical nickel plating is rear gold-plated, obtains ni au coating, carries out binding force of cladding material performance to the gold-plated sample of diamond copper
Test, test result is as follows:
| Binding force of cladding material test item | Time | Phenomenon |
| (320 DEG C) are tested in high temperature examination baking | 10min | Coating is without peeling, obscission |
| The test of hundred lattice | / | Coating is without peeling, obscission |
| Thermal shock test (250 DEG C) | 30min | Coating is without peeling, obscission |
| Welding performance | / | It is very good |
。
Claims (6)
1. a kind of diamond/copper semiconductor composite surface treatment coarsening solution, which is characterized in that the coarsening solution includes
There are the A liquid of etching diamond and the B liquid of microetch copper.
2. diamond/copper semiconductor composite surface treatment coarsening solution as described in claim 1, which is characterized in that institute
The A liquid stated includes
Potassium hydroxide, 15-25g/L；
Copper sulphate, 10-20g/L；
Potassium permanganate, 5-10g/L；
Potassium hypophosphite, 1-2g/L；
Triethanolamine, 5-10ml/L.
3. the diamond/copper semiconductor composite surface treatment as claimed in claim 2 preparation method of coarsening solution, special
Sign is that the preparation method of the A liquid includes following step:
A. the potassium hydroxide for weighing mass ratio is soluble in water, is thoroughly mixed uniformly, obtains uniform potassium hydroxide solution；
B. the anhydrous cupric sulfate of proportion mass parts is added into above-mentioned potassium hydroxide solution, stirs evenly；
C. the potassium permanganate of proportion mass parts is added into above-mentioned mixed solution, stirs evenly；
D. the potassium hypophosphite of proportion mass parts is added into above-mentioned mixed solution, stirs evenly；
E. the triethanolamine of proportion mass parts is added into above-mentioned mixed solution, is mixed evenly；
F. pure water is added into above-mentioned mixed solution, constant volume is mixed evenly.
4. diamond/copper semiconductor composite surface treatment coarsening solution as described in claim 1, which is characterized in that institute
The B liquid stated includes
Copper chloride, 10-20g/L；
Fluorine potassium carbonate, 5-10g/L；
Hydrochloric acid, mass fraction 31%, 40-55ml/L；
Sulfamic acid sodium 1-3g/L.
5. the diamond/copper semiconductor composite surface treatment as claimed in claim 4 preparation method of coarsening solution, special
Sign is that the preparation method comprises the following steps that
A. amount concentrated hydrochloric acid is soluble in water, stirs while being added, obtains uniform hydrochloric acid solution；
A. the copper chloride for weighing mass ratio is dissolved in above-mentioned hydrochloric acid solution, is thoroughly mixed uniformly；
B. the fluorine potassium carbonate of proportion mass parts is added into above-mentioned mixed solution, stirs evenly；
C. the sulfamic acid sodium of proportion mass parts is added into above-mentioned mixed solution, stirs evenly；
D. pure water is added into above-mentioned mixed solution, constant volume is mixed evenly.
6. the diamond/copper semiconductor composite surface treatment as described in claim 1 application method of coarsening solution, special
Sign is that the application method comprises the following steps that
A. the diamond/copper composite material after oil removing being cleaned is put into A liquid, and glass bar agitating solution is used at 50-60 DEG C, is made
Diamond/copper composite material is suspended in coarsening solution, and each face of substrate can adequately contact solution, after 5 ± 1min, uses pure water
It rinses well.
B. it impregnates and is suspended in B liquid under the composite material room temperature rinsed well after being roughened above-mentioned in A liquid, low temperature drying is
It can.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910479269.5A CN110055533B (en) | 2019-06-04 | 2019-06-04 | Roughening liquid for diamond/copper composite material surface treatment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910479269.5A CN110055533B (en) | 2019-06-04 | 2019-06-04 | Roughening liquid for diamond/copper composite material surface treatment |
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| Publication Number | Publication Date |
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| CN110055533A true CN110055533A (en) | 2019-07-26 |
| CN110055533B CN110055533B (en) | 2021-01-22 |
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| CN201910479269.5A Active CN110055533B (en) | 2019-06-04 | 2019-06-04 | Roughening liquid for diamond/copper composite material surface treatment |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140124793A1 (en) * | 2012-11-06 | 2014-05-08 | University Of Florida Research Foundation, Inc. | Smooth diamond surfaces and cmp method for forming |
| CN105063579A (en) * | 2015-07-20 | 2015-11-18 | 深圳市瑞世兴科技有限公司 | Roughing solution for diamond-copper composite and surface nickel plating method of diamond-copper composite |
| CN107128908A (en) * | 2017-04-17 | 2017-09-05 | 安徽卡尔森新材料科技有限公司 | The potent pre-treating method of diamond super fine |
-
2019
- 2019-06-04 CN CN201910479269.5A patent/CN110055533B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140124793A1 (en) * | 2012-11-06 | 2014-05-08 | University Of Florida Research Foundation, Inc. | Smooth diamond surfaces and cmp method for forming |
| JP2016502757A (en) * | 2012-11-06 | 2016-01-28 | シンマット, インコーポレーテッドSinmat, Inc. | Smooth diamond surface and CMP method for its formation |
| CN105063579A (en) * | 2015-07-20 | 2015-11-18 | 深圳市瑞世兴科技有限公司 | Roughing solution for diamond-copper composite and surface nickel plating method of diamond-copper composite |
| CN107128908A (en) * | 2017-04-17 | 2017-09-05 | 安徽卡尔森新材料科技有限公司 | The potent pre-treating method of diamond super fine |
Non-Patent Citations (1)
| Title |
|---|
| 季兴桥 等: "超高导热金刚石铜表面镀涂技术研究", 《稀有金属》 * |
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