CN110712419A - Preparation method of copper-molybdenum-copper alloy material - Google Patents
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- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
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- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/16—Drying; Softening; Cleaning
- B32B38/164—Drying
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- 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
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- C23F1/18—Acidic compositions for etching copper or alloys thereof
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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
- 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
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- C23F1/10—Etching compositions
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- B32B2038/0052—Other operations not otherwise provided for
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Abstract
The invention belongs to a metal composite material, and particularly relates to a preparation method of a copper-molybdenum-copper alloy material, which comprises the following steps: uniformly coating sulfuric acid liquid films on the front surface and the back surface of the molybdenum plate, and then placing the molybdenum plate in a reaction kettle for constant-pressure heating reaction for 10-20min to obtain a rough coated molybdenum plate; placing the rough film-coated molybdenum plate into distilled water, ultrasonically cleaning, and quickly drying to obtain a rough molybdenum plate; uniformly coating a dilute hydrochloric acid liquid film on the surface of the copper plate, standing for 10-20min, heating for 30-60min, washing and drying to obtain a microporous copper plate; covering copper plates on the front and back surfaces of a molybdenum plate respectively, and performing hydraulic pressure to obtain a composite plate; putting the composite board into an electric heating sintering furnace, sealing and hot-pressing for 2-4h to obtain a secondary composite board; and (4) carrying out grinding leveling on the secondary composite board to obtain the copper-molybdenum-copper alloy material. The invention solves the problem of poor bonding force of the existing copper-molybdenum-copper composite plate, forms a rough surface layer structure by utilizing surface roughening, and forms compact composite under hydraulic pressure and sintering treatment, thereby greatly improving the bonding strength.
Description
Technical Field
The invention belongs to a metal composite material, and particularly relates to a preparation method of a copper-molybdenum-copper alloy material.
Background
Copper is a good heat-conducting and electric-conducting material, has good flexibility, is easy to process and form, and is widely applied to the field of electronic packaging materials. But because of its large coefficient of thermal expansion, it cannot match many semiconductor materials, limiting its further applications; the refractory metal molybdenum has excellent high-temperature strength, low thermal expansion coefficient and good heat conduction and electric conductivity, meanwhile, the molybdenum belongs to a body-centered cubic structure, the copper belongs to a face-centered cubic structure, the molybdenum and the copper are mutually incompatible and are combined together to prepare a composite material, the advantages of the molybdenum and the copper are integrated, and the molybdenum and the copper are respectively kept relatively independent on components, so that the special performance which is not possessed by a single material can be obtained; in addition, the designable thermal expansion coefficient and good heat conduction and electric conductivity can be achieved by changing the thickness ratio of the copper-molybdenum-copper composite material. The copper-molybdenum-copper three-layer composite board not only has the performances, but also has good forming performance and good high-temperature strength. Therefore, the method is widely applied to the field of electronic industry. With the continuous progress of science and technology, the development of the electronic industry is leapfrog, and the demand of copper-molybdenum-copper composite materials is continuously increased. Compared with materials such as molybdenum copper, tungsten copper and the like, the material has the advantages of low production cost, good plane thermal conductivity and high density; meanwhile, the copper-molybdenum-copper laminated composite material has wide application prospect in the fields of HB-LEDs, multi-substrate-group plate materials, electronic packaging, heat sink materials, aerospace and the like.
The current method for manufacturing the copper-molybdenum-copper composite material comprises the following steps: rolling cladding method, explosion cladding method, liquid-solid phase casting-rolling cladding method, reverse solidification method and laser surface cladding technology. The rolling compounding method is more conventional, but the composite plate produced by the method has poor surface quality, insufficient compounding degree and difficult performance meeting the use requirement.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a copper-molybdenum-copper alloy material, which solves the problem of poor bonding force of the existing copper-molybdenum-copper composite plate, forms a rough surface layer structure by using surface roughening, and forms compact composite under hydraulic pressure and sintering treatment, thereby greatly improving the bonding strength.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a preparation method of a copper-molybdenum-copper alloy material comprises the following steps:
step 1, uniformly coating sulfuric acid liquid films on the front surface and the back surface of a molybdenum plate, and then placing the molybdenum plate in a reaction kettle for constant-pressure heating reaction for 10-20min to obtain a rough coated molybdenum plate;
step 2, placing the rough coated molybdenum plate into distilled water for ultrasonic cleaning, and then quickly drying to obtain a rough molybdenum plate;
step 3, uniformly coating a dilute hydrochloric acid liquid film on the surface of the copper plate, standing for 10-20min, heating for 30-60min, washing and drying to obtain the microporous copper plate;
step 4, covering the copper plates on the front and back surfaces of the molybdenum plate respectively, and performing hydraulic pressure to obtain a composite plate;
step 5, putting the composite board into an electric heating sintering furnace, sealing and hot-pressing for 2-4h to obtain a secondary composite board;
and 6, carrying out grinding leveling on the secondary composite board to obtain the copper-molybdenum-copper alloy material.
The sulfuric acid concentration of the sulfuric acid liquid film in the step 1 is 50-60%, and the coating amount of the liquid film is 2-4g/cm2The temperature of constant pressure heating is 100-110 ℃, and the pressure is 0.14-0.23 MPa.
The ultrasonic frequency of the ultrasonic cleaning in the step 2 is 30-60kHz, the temperature is 40-60 ℃, and the drying temperature is 130-150 ℃.
The concentration of the dilute hydrochloric acid in the step 3 is 0.01-0.03mol/L, and the coating amount of the dilute hydrochloric acid liquid film is 0.5-1.3mL/cm2The standing temperature is 10-20 ℃, the temperature for heating is 100-.
The hydraulic pressure in the step 4 is 15-20 MPa.
The sealing hot-pressing temperature in the step 5 is 1000-.
The thickness ratio of the copper layer, the molybdenum layer and the copper layer after the turning, grinding and leveling in the step 6 is 1:2-6: 1.
And the copper plate in the step 3 is an electrolytic copper plate.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the problem of poor bonding force of the existing copper-molybdenum-copper composite plate, forms a rough surface layer structure by utilizing surface roughening, and forms compact composite under hydraulic pressure and sintering treatment, thereby greatly improving the bonding strength.
2. The invention solves the problem of difficult treatment of molybdenum materials, changes the concentration of a sulfuric acid liquid film by using the temperature to achieve the effect of surface treatment of the molybdenum plate, and forms the roughened surface of the molybdenum plate.
Detailed Description
The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.
Example 1
A preparation method of a copper-molybdenum-copper alloy material comprises the following steps:
step 1, uniformly coating sulfuric acid liquid films on the front surface and the back surface of a molybdenum plate, and then placing the molybdenum plate in a reaction kettle for constant-pressure heating reaction for 10min to obtain a rough coated molybdenum plate;
step 2, placing the rough coated molybdenum plate into distilled water for ultrasonic cleaning, and then quickly drying to obtain a rough molybdenum plate;
step 3, uniformly coating a dilute hydrochloric acid liquid film on the surface of the copper plate, standing for 10min, heating for 30min, washing and drying to obtain a microporous copper plate;
step 4, covering the copper plates on the front and back surfaces of the molybdenum plate respectively, and performing hydraulic pressure to obtain a composite plate;
step 5, putting the composite board into an electric heating sintering furnace, sealing and hot-pressing for 2 hours to obtain a secondary composite board;
and 6, carrying out grinding leveling on the secondary composite board to obtain the copper-molybdenum-copper alloy material.
The sulfuric acid concentration of the sulfuric acid liquid film in the step 1 is 50%, and the coating amount of the liquid film is 2g/cm2The temperature of constant pressure heating is 100 ℃, and the pressure is 0.14 MPa.
The ultrasonic frequency of the ultrasonic cleaning in the step 2 is 30kHz, the temperature is 40 ℃, and the drying temperature is 130 ℃.
The concentration of the dilute hydrochloric acid in the step 3 is 0.01mol/L, and the coating amount of the dilute hydrochloric acid liquid film is 0.5mL/cm2The temperature of standing is 10 ℃, the temperature of heating is 100 ℃, and the temperature of drying is 100 ℃.
The hydraulic pressure in the step 4 is 15 MPa.
And 5, sealing and hot-pressing at 1000 ℃ under 10MPa in the step, wherein the environment of sealing and hot-pressing is a protective gas atmosphere, and the protective gas is hydrogen.
The thickness ratio of the copper layer, the molybdenum layer and the copper layer after the turning, grinding and leveling in the step 6 is 1:2: 1.
And the copper plate in the step 3 is an electrolytic copper plate.
Example 2
A preparation method of a copper-molybdenum-copper alloy material comprises the following steps:
step 1, uniformly coating sulfuric acid liquid films on the front surface and the back surface of a molybdenum plate, and then placing the molybdenum plate in a reaction kettle for constant-pressure heating reaction for 20min to obtain a rough coated molybdenum plate;
step 2, placing the rough coated molybdenum plate into distilled water for ultrasonic cleaning, and then quickly drying to obtain a rough molybdenum plate;
step 3, uniformly coating a dilute hydrochloric acid liquid film on the surface of the copper plate, standing for 20min, heating for 60min, washing and drying to obtain a microporous copper plate;
step 4, covering the copper plates on the front and back surfaces of the molybdenum plate respectively, and performing hydraulic pressure to obtain a composite plate;
step 5, putting the composite board into an electric heating sintering furnace, sealing and hot-pressing for 4 hours to obtain a secondary composite board;
and 6, carrying out grinding leveling on the secondary composite board to obtain the copper-molybdenum-copper alloy material.
The sulfuric acid concentration of the sulfuric acid liquid film in the step 1 is 60%, and the coating amount of the liquid film is 4g/cm2The temperature of constant pressure heating is 110 ℃, and the pressure is 0.23 MPa.
The ultrasonic frequency of the ultrasonic cleaning in the step 2 is 60kHz, the temperature is 60 ℃, and the drying temperature is 150 ℃.
The concentration of the dilute hydrochloric acid in the step 3 is 0.03mol/L, and the coating amount of the dilute hydrochloric acid liquid film is 1.3mL/cm2The temperature of standing is 20 ℃, the temperature of heating is 130 ℃, and the temperature of drying is 110 ℃.
The hydraulic pressure in the step 4 is 20 MPa.
And 5, sealing and hot-pressing at 1200 ℃ under 12MPa, wherein the environment of sealing and hot-pressing is a protective gas atmosphere, and the protective gas is nitrogen.
The thickness ratio of the copper layer, the molybdenum layer and the copper layer after the turning, grinding and leveling in the step 6 is 1:6: 1.
And the copper plate in the step 3 is an electrolytic copper plate.
Example 3
A preparation method of a copper-molybdenum-copper alloy material comprises the following steps:
step 1, uniformly coating sulfuric acid liquid films on the front surface and the back surface of a molybdenum plate, and then placing the molybdenum plate in a reaction kettle for constant-pressure heating reaction for 15min to obtain a rough coated molybdenum plate;
step 2, placing the rough coated molybdenum plate into distilled water for ultrasonic cleaning, and then quickly drying to obtain a rough molybdenum plate;
step 3, uniformly coating a dilute hydrochloric acid liquid film on the surface of the copper plate, standing for 15min, heating for 50min, washing and drying to obtain a microporous copper plate;
step 4, covering the copper plates on the front and back surfaces of the molybdenum plate respectively, and performing hydraulic pressure to obtain a composite plate;
step 5, putting the composite board into an electric heating sintering furnace, sealing and hot-pressing for 3 hours to obtain a secondary composite board;
and 6, carrying out grinding leveling on the secondary composite board to obtain the copper-molybdenum-copper alloy material.
The sulfuric acid concentration of the sulfuric acid liquid film in the step 1 is 55%, and the coating amount of the liquid film is 3g/cm2The temperature of constant pressure heating is 105 ℃, and the pressure is 0.18 MPa.
The ultrasonic frequency of the ultrasonic cleaning in the step 2 is 50kHz, the temperature is 50 ℃, and the drying temperature is 140 ℃.
The dilute salt in the step 3The concentration of the acid was 0.02mol/L, and the coating amount of the dilute hydrochloric acid liquid film was 0.9mL/cm2The temperature of standing is 15 ℃, the temperature of heating is 120 ℃, and the temperature of drying is 105 ℃.
The pressure of the hydraulic pressure in the step 4 is 18 MPa.
And 5, sealing and hot-pressing at the temperature of 1100 ℃ under the pressure of 11MPa in the step 5, wherein the environment of sealing and hot-pressing is a protective gas atmosphere, and the protective gas adopts hydrogen.
The thickness ratio of the copper layer, the molybdenum layer and the copper layer after the turning, grinding and leveling in the step 6 is 1:4: 1.
And the copper plate in the step 3 is an electrolytic copper plate.
Performance detection
In summary, the invention has the following advantages:
1. the invention solves the problem of poor bonding force of the existing copper-molybdenum-copper composite plate, forms a rough surface layer structure by utilizing surface roughening, and forms compact composite under hydraulic pressure and sintering treatment, thereby greatly improving the bonding strength.
2. The invention solves the problem of difficult treatment of molybdenum materials, changes the concentration of a sulfuric acid liquid film by using the temperature to achieve the effect of surface treatment of the molybdenum plate, and forms the roughened surface of the molybdenum plate.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (8)
1. A preparation method of a copper-molybdenum-copper alloy material is characterized by comprising the following steps: the method comprises the following steps:
step 1, uniformly coating sulfuric acid liquid films on the front surface and the back surface of a molybdenum plate, and then placing the molybdenum plate in a reaction kettle for constant-pressure heating reaction for 10-20min to obtain a rough coated molybdenum plate;
step 2, placing the rough coated molybdenum plate into distilled water for ultrasonic cleaning, and then quickly drying to obtain a rough molybdenum plate;
step 3, uniformly coating a dilute hydrochloric acid liquid film on the surface of the copper plate, standing for 10-20min, heating for 30-60min, washing and drying to obtain the microporous copper plate;
step 4, covering the copper plates on the front and back surfaces of the molybdenum plate respectively, and performing hydraulic pressure to obtain a composite plate;
step 5, putting the composite board into an electric heating sintering furnace, sealing and hot-pressing for 2-4h to obtain a secondary composite board;
and 6, carrying out grinding leveling on the secondary composite board to obtain the copper-molybdenum-copper alloy material.
2. The method for producing a copper-molybdenum-copper alloy material according to claim 1, characterized in that: the sulfuric acid concentration of the sulfuric acid liquid film in the step 1 is 50-60%, and the coating amount of the liquid film is 2-4g/cm2The temperature of constant pressure heating is 100-110 ℃, and the pressure is 0.14-0.23 MPa.
3. The method for producing a copper-molybdenum-copper alloy material according to claim 1, characterized in that: the ultrasonic frequency of the ultrasonic cleaning in the step 2 is 30-60kHz, the temperature is 40-60 ℃, and the drying temperature is 130-150 ℃.
4. The method for producing a copper-molybdenum-copper alloy material according to claim 1, characterized in that: the concentration of the dilute hydrochloric acid in the step 3 is 0.01-0.03mol/L, and the coating amount of the dilute hydrochloric acid liquid film is 0.5-1.3mL/cm2The standing temperature is 10-20 ℃, the temperature for heating is 100-.
5. The method for producing a copper-molybdenum-copper alloy material according to claim 1, characterized in that: the hydraulic pressure in the step 4 is 15-20 MPa.
6. The method for producing a copper-molybdenum-copper alloy material according to claim 1, characterized in that: the sealing hot-pressing temperature in the step 5 is 1000-.
7. The method for producing a copper-molybdenum-copper alloy material according to claim 1, characterized in that: the thickness ratio of the copper layer, the molybdenum layer and the copper layer after the turning, grinding and leveling in the step 6 is 1:2-6: 1.
8. The method for producing a copper-molybdenum-copper alloy material according to claim 1, characterized in that: and the copper plate in the step 3 is an electrolytic copper plate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112588823A (en) * | 2020-12-21 | 2021-04-02 | 江苏时代华宜电子科技有限公司 | Surface roughness forming process for cold-rolled thin molybdenum sheet |
| CN112828291A (en) * | 2020-12-31 | 2021-05-25 | 宁波通导电子有限公司 | Manufacturing method of high-temperature operation robot |
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| CN107891636A (en) * | 2017-11-22 | 2018-04-10 | 无锡乐普金属科技有限公司 | The preparation method of copper-molybdenum copper copper composite plate |
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| CN112588823A (en) * | 2020-12-21 | 2021-04-02 | 江苏时代华宜电子科技有限公司 | Surface roughness forming process for cold-rolled thin molybdenum sheet |
| CN112588823B (en) * | 2020-12-21 | 2024-05-17 | 江苏时代华宜电子科技有限公司 | Surface roughness forming process for cold-rolled thin molybdenum sheet |
| CN112828291A (en) * | 2020-12-31 | 2021-05-25 | 宁波通导电子有限公司 | Manufacturing method of high-temperature operation robot |
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