CN101070461A - Super-high heat-conductive diamond-copper composite package material and production method - Google Patents
Super-high heat-conductive diamond-copper composite package material and production method Download PDFInfo
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- CN101070461A CN101070461A CN 200710034951 CN200710034951A CN101070461A CN 101070461 A CN101070461 A CN 101070461A CN 200710034951 CN200710034951 CN 200710034951 CN 200710034951 A CN200710034951 A CN 200710034951A CN 101070461 A CN101070461 A CN 101070461A
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Abstract
The invention discloses a diamond-copper composite-encapsulation material and its manufacturing method. The matrix-material is copper. The granular mass of diamond is 2-60%,and the particle diameter is about 1-150um. The adjunct is copper or silver which granular mass is 0.1-10%. Gild the adjunct on the surface of the diamond powder granola in a way of chemical plating. The steps as follows: (1). Gild the adjunct o the surface of the diamond powder granola in a way of chemical plating, and form a coat of 0.1-5%um. Around. (2). Put the granola on the metallic mold dispersive, and then put the mold into electrolysis bath. (3). Make the metallic mold cathode, the copper anode, and cupric phosphate solution bath composition. Then separate out the copper on the mold, until it covers the diamond. (4). Take out the sample and wash it carefully, then cut it according to the needed size. The material of the invention has the advantages of high thermal coefficient and low thermal expansion coefficient.
Description
Technical field
The present invention relates to a kind of diamond-copper composite encapsulating material, the invention still further relates to the production method of this composite encapsulating material.
Background technology
20th century, the eighties rose, and microelectronic packaging technology and packaged material become one of important factor that influences the microelectronics development gradually.Packaged material plays a part fixed chip, protection inner member, transmits electrical signal and outwards distribute the element heat in unicircuit, is the key part of unicircuit.Along with unicircuit develops to high-density, miniaturization, multifunction, requirement to electronic package material is more and more harsher, packaged material commonly used at present can not adapt to the development need of microelectronics well, mainly show as: though 1. the thermal conductivity of pure copper material reaches 398W/ (mK), but the intensity of fine copper is very low, easy deformation, though adopt copper alloy can improve intensity within the specific limits, heat conductivility can obviously reduce; 2. the thermal expansivity of fine copper is bigger, is difficult to be complementary with the hot expansibility of semiconductor materials such as silicon; 3. the thermal conductivity of packaged material can't be higher than the thermal conductivity of fine copper.Therefore it is significant to research and develop the high-strength highly-conductive hot encapsulation material.At present, various novel encapsulated materials have become the focus that various countries competitively research and develop, the novel microelectronic packaged material not only to have low specific inductivity, low dielectric loss, with the semiconductor material matched coefficient of thermal expansion, high thermal conductivity is the key of the novel encapsulated material capacity of heat transmission.Under such background, become outshining others in numerous packaged materials just with high heat conductance filler enhanced metal-base composites.
Copper is the high-thermal conductive metal material of using always, and its thermal conductivity is 398W/ (mK), thermal expansivity 17 * 10
-6/ ℃.Because the intensity of fine copper is lower, thermal expansivity is big, with semiconductor material coupling difficulty such as silicon, so its application is restricted.Diamond is the highest material of occurring in nature thermal conductivity, and its thermal conductivity can reach 2000W/ (mK), is 5 times of fine copper, thermal expansivity 1.0 * 10
-6/ ℃.Therefore diamond and copper are made composite encapsulating material, can improve thermal conductivity, the adjusting thermal expansivity of packaged material, make it to be complementary with semiconductor material such as silicon.Diamond-copper composite encapsulating material becomes the research focus of encapsulation with the super-high heat-conductive material gradually.W.Z.Shao etc. adopt powder metallurgical technique, and pressing pressure 300MPa at 1159～1220K sintering temperature, has prepared diamond-copper composite material, and density is higher than 98%.The but easy carbonization of diamond particles under 900 ℃ of temperature generates CO or CO
2, influence material structure and performance.K.hanada has prepared diamond-copper composite material with powder metallurgy method, and thermal conductivity reaches 400W/ (mK), but its detailed preparation technology aspect is not open.
There is the method that adopts galvanic deposit to prepare the technology of nickel-diamond composite in the production of diamond abrasive tool material, this technology is electrolytic solution with the single nickel salt, diamond particles is suspended in the solution, and logical direct current makes nickel in cathodic deposition, and diamond is buried.But because diamond is non-conductive, so nickel combines just piling up of machinery with adamantine, and the interface combination is very weak, and thermal resistance is very big; Because the thermal conductivity of nickel is not fine, therefore directly adopt the nickel-diamond composite heat conductivility of this explained hereafter relatively poor simultaneously, can not be satisfied with the requirement of packaged material.In addition, the technology of depositing diamond is stirred in this suspension can't produce the high goods of diamond content, and diameter is effectively suspended greater than the diamond particles of 10 μ m, the goods that therefore only suitable diamond grit is little, mark is lower.
Summary of the invention
Technical problem to be solved by this invention provides a kind of super-high heat-conductive diamond-copper composite package material with high heat conductance, low thermal coefficient of expansion.
Another technical problem that the present invention also will solve provides the preparation method of this composite encapsulating material.
In order to solve the problems of the technologies described above, super-high heat-conductive diamond-copper composite package material provided by the invention, constitute by copper matrix and the additive that is distributed in heat conduction, the intensity enhancing thing diamond particles in the copper matrix and improves interface bonding state, described heat conduction, intensity enhancing thing diamond particles content are 2～60% in mass, select for use particle size range to be: 1 μ m～150 μ m, described additive is copper or silver.
The method of this diamond-copper composite encapsulating material of production provided by the invention the steps include:
A. diamond pre-treatment: after selecting for use particle size range to be the diamond oil removing, roughening treatment of 1 μ m～150 μ m, activate again and sensitization;
The diamond particles that B. will activate after the sensitization carries out electroless plating, and the electroless plating condition is as shown in table 1, can control thickness of coating copper or silver by adjusting plating time, and thickness of coating is 0.1～6 μ m.Diamond particles pattern behind the electroless copper as shown in Figure 3, the diamond particles pattern behind the chemical silvering is as shown in Figure 4.
Table 1 diamond electroless plating condition
| Electroless Cu Plating | Electroless plating Ag | ||
| Composition | Content (gL -1) | Composition | Content (gL -1) |
| CuSO 4·5H 2O | 15 | AgNO 3 | 1.5 |
| Formaldehyde (36%) | 15 | Ammoniacal liquor | 10 |
| Seignette salt | 14 | Formaldehyde | 0.15mL·L -1 |
| EDTA | 14.6 | Ethanol | 100mL·L -1 |
| NaOH | (adjust pH) in right amount | ||
| The duplex pyridine | 0.02 | ||
| Yellow prussiate of potash | 0.01 | ||
| The pH value | 12.5 | ||
| Temperature/℃ | 43 | Temperature/℃ | 35 |
| Time/min | 20-100 | Time/min | 5-60 |
C. the diamond particles homodisperse behind electroless copper or the silver is placed a metal die, and be negative electrode with this mould, copper-bath is an electrolytic solution, the fine copper plate is an anode, carry out galvanic deposit, make copper separate out and gradually diamond particles be buried at negative electrode and cover, electrodeposition condition is as shown in table 2, regulate the preparation sample thickness by the control electrodeposition time, making diamond particles content was 2～60% (in mass).Electric deposition device as shown in Figure 5, among the figure: 1. reometer; 2. thermometer; 3. pure copper anode; 4. negative electrode mould; 5. stir; 6. copper sulfate electroplate liquid; 7. well heater; 8 magnetic agitation; 9 current regulator power supplies.
Table 2 galvanic deposit plating bath is formed and processing condition
| Electrodeposit liquid is formed | The electrodeposition technology condition | ||
| Title | Content g L -1 | Project | Processing parameter |
| Copper sulfate (CuSO 4·5H 2O) | 80-250 | Current density Adm -2 | 2.2-10 |
| The vitriol oil (H 2SO 4) | 65 | Stirring velocity rmin -1 | 150-500 |
| Chlorion (Cl -1) | 0.06 | Temperature ℃ | 25 |
| Sodium polydithio-dipropyl sulfonate | 0.1 | Diamond particle size μ m | 1-150 |
| Polyoxyethylene glycol | 0.1 | ||
D. cut processing: adopt wire cutting technology with the materials processing desired size.
The present invention carries out electroless plating with the diamond powder particle earlier, copper or silver are plated on diamond surface, make it have conductivity, then the diamond particles homodisperse after the electroless plating is placed a metal die, and be negative electrode with this mould, copper-bath is an electrolytic solution, the fine copper plate is an anode, carry out galvanic deposit, make copper separate out and gradually diamond particles be buried and cover, solved diamond and copper interface resistance height at negative electrode, the difficult problem that the diamond volume fraction is low has produced and has had high heat conductance, the diamond-copper composite encapsulating material of low thermal coefficient of expansion satisfies the service requirements of encapsulation of electronic devices and components and surface-mounted integrated circuit and heat sink material.
The present invention prepares diamond/copper composite encapsulating material and compares with existing packaged material performance and production technique and have the following advantages:
1. the present invention adopts the first electroless plating prepared diamond/copper composite encapsulating material of galvanic deposit again, improved the interface bond strength between copper and the diamond, reduced interface resistance, thereby made the thermal conductivity of diamond/copper composite encapsulating material reach 300～550W/ (mK); Again owing to adopt mould prepackage bortz powder to carry out galvanic deposit, make that adamantine volume weight mark reaches 60% in the matrix material, so thermal expansivity reaches 6 * 10 during its 323K
-6/ ℃, can satisfy the requirement of packaged material.And encapsulation commonly used at present copper base packaged material such as Cu-W, Cu-Mo, Al-SiC etc., thermal conductivity is general only between 150～220W/ (mK).
2. the electroless plating pre-treatment that proposes of the present invention technology of galvanic deposit again, it is simple to have technology, control easily, to less demanding advantages such as experimental installation and places.
In sum, the present invention is a kind of super-high heat-conductive diamond-copper composite package material with high heat conductance, low thermal coefficient of expansion, and the preparation method of this composite encapsulating material is simple and reliable.
Description of drawings
Fig. 1 is the diamond particles pattern photo before handling among the embodiment 1;
Fig. 2 is a diamond particles pattern photo after the alligatoring among the embodiment 1;
Fig. 3 is the SEM photo after the diamond particles Electroless Cu Plating among the embodiment 1;
Fig. 4 is the SEM photo behind the diamond particles electroless plating Ag among the embodiment 2;
Fig. 5 is the electric deposition device structural representation;
Fig. 6 is a sample SEM photo among the embodiment 1.
Embodiment
The present invention is described in detail below by embodiment, following Example just meets several examples of the technology of the present invention content, do not illustrate that the present invention only limits to the described content of following example, the technician in the industry all belongs to content of the present invention according to the product of claim item of the present invention manufacturing.
Embodiment 1:
1. select for use mean particle size 10 μ m diamond particles to carry out pre-treatment, oil removing: place 10% NaOH solution violent stirring to boil 30min in diamond, the back is extremely neutral with distilled water flushing; Alligatoring: in 30% dilute nitric acid solution, boil 30min then, extremely neutral with distilled water flushing again.Fig. 1 is the diamond particles pattern photo before handling, and Fig. 2 is a diamond particles pattern photo after the alligatoring;
2. diamond surface Electroless Cu Plating, diamond electroless copper condition: CuSO
45H
2O 15gL
-1, 36% formaldehyde 15gL
-1, Seignette salt 14gL
-1, EDTA 14.6gL
-1, NaOH adjusts pH, duplex pyridine 0.02gL in right amount
-1, yellow prussiate of potash 0.01gL
-1, pH value 12.5,43 ℃ of temperature, plating time 20 minutes, thickness of coating 1 μ m, the SEM photo after the diamond particles Electroless Cu Plating as shown in Figure 3;
3. the diamond particles homodisperse behind the electroless copper being placed copper mould, is negative electrode with this mould, and copper-bath is an electrolytic solution, and the fine copper plate is an anode, carries out galvanic deposit, and electrodeposit liquid is formed: copper sulfate (CuSO
45H
2O) 250gL
-1, the vitriol oil (H
2SO
4) 65gL
-1, chlorion (Cl
-1) 0.06gL
-1, sodium polydithio-dipropyl sulfonate 0.1gL
-1, polyoxyethylene glycol 0.1gL
-1Electrodeposition technology condition: current density 10Adm
-2, stirring velocity 150rmin
-1, 25 ℃ of temperature, depositing time 10 hours makes copper separate out and gradually diamond particles be buried at negative electrode and covers, electric deposition device as shown in Figure 5;
4. adopt wire cutting technology that the goods that galvanic deposit obtains are cut into desired size, be used for Performance Detection, detected result is as shown in table 3.Sample SEM photo as shown in Figure 6.
Embodiment 2:
1. select for use mean particle size 50 μ m diamond particles to carry out pre-treatment, oil removing: place 10%NaOH solution violent stirring to boil 30min in diamond, the back is extremely neutral with distilled water flushing; Alligatoring: in 30% dilute nitric acid solution, boil 30min then, extremely neutral with distilled water flushing again;
2. diamond surface electroless plating Ag, diamond chemical silvering condition: AgNO
31.5gL
-1, ammoniacal liquor 10gL
-1, formaldehyde 0.15mLL
-1, ethanol 100mLL
-1, 35 ℃ of temperature, time 60min, thickness of coating 3 μ m.SEM photo behind the diamond particles electroless plating Ag as shown in Figure 4;
3. the diamond particles homodisperse behind the electroless plating Ag being placed copper mould, is negative electrode with this mould, and copper-bath is an electrolytic solution, and the fine copper plate is an anode, carries out galvanic deposit, and electrodeposit liquid is formed: copper sulfate (CuSO
45H
2O) 80gL
-1, the vitriol oil (H
2SO
4) 65gL
-1, chlorion (Cl
-1) 0.06gL
-1, sodium polydithio-dipropyl sulfonate 0.1gL
-1, polyoxyethylene glycol 0.1gL
-1Electrodeposition technology condition: current density 2.2Adm
-2, stirring velocity 150rmin
-1, 25 ℃ of temperature, depositing time 12 hours makes copper separate out and gradually diamond particles be buried at negative electrode and covers, electric deposition device as shown in Figure 5;
4. adopt wire cutting technology that the goods that galvanic deposit obtains are cut into desired size, be used for Performance Detection, detected result is as shown in table 3.
Embodiment 3:
1. select for use mean particle size 150 μ m diamond particles to carry out pre-treatment, oil removing: place 10%NaOH solution violent stirring to boil 30min in diamond, the back is extremely neutral with distilled water flushing; Alligatoring: in 30% dilute nitric acid solution, boil 30min then, extremely neutral with distilled water flushing again;
2. diamond surface electroless plating Ag, diamond chemical silvering condition: AgNO
31.5gL
-1, ammoniacal liquor 10gL
-1, formaldehyde 0.15mLL
-1, ethanol 100mLL
-1, 35 ℃ of temperature, plating time 60 minutes, the about 6 μ m of thickness of coating;
3. the diamond particles homodisperse behind the electroless plating Ag being placed copper mould, is negative electrode with this mould, and copper-bath is an electrolytic solution, and the fine copper plate is an anode, carries out galvanic deposit, and electrodeposit liquid is formed: copper sulfate (CuSO
45H
2O) 180gL
-1, the vitriol oil (H
2SO
4) 65gL
-1, chlorion (Cl
-1) 0.06gL
-1, sodium polydithio-dipropyl sulfonate 0.1gL
-1, polyoxyethylene glycol 0.1gL
-1Electrodeposition technology condition: current density 8Adm
-2, stirring velocity 500rmin
-1, 25 ℃ of temperature, depositing time 15 hours makes copper separate out and gradually diamond particles be buried at negative electrode and covers, electric deposition device as shown in Figure 5;
4. adopt wire cutting technology that the goods that galvanic deposit obtains are cut into desired size, be used for Performance Detection, detected result is as shown in table 3.
Embodiment 4:
1. select for use mean particle size 1.0 μ m diamond particles to carry out pre-treatment, oil removing: place 10%NaOH solution violent stirring to boil 30min in diamond, the back is extremely neutral with distilled water flushing; Alligatoring: in 30% dilute nitric acid solution, boil 30min then, extremely neutral with distilled water flushing again;
2. diamond surface electroless plating Ag, diamond chemical silvering condition: AgNO
31.5gL
-1, ammoniacal liquor 10gL
-1, formaldehyde 0.15mLL
-1, ethanol 100mLL
-1, 35 ℃ of temperature, plating time 5 minutes, the about 0.1 μ m of thickness of coating;
3. the diamond particles homodisperse behind the electroless plating Ag being placed copper mould, is negative electrode with this mould, and copper-bath is an electrolytic solution, and the fine copper plate is an anode, carries out galvanic deposit, and electrodeposit liquid is formed: copper sulfate (CuSO
45H
2O) 180gL
-1, the vitriol oil (H
2SO
4) 65gL
-1, chlorion (Cl
-1) 0.06gL
-1, sodium polydithio-dipropyl sulfonate 0.1gL
-1, polyoxyethylene glycol 0.1gL
-1Electrodeposition technology condition: current density 8Adm
-2, stirring velocity 80rmin
-1, 25 ℃ of temperature, depositing time 15 hours makes copper separate out and gradually diamond particles be buried at negative electrode and covers, electric deposition device as shown in Figure 5;
4. adopt wire cutting technology that the goods that galvanic deposit obtains are cut into desired size, be used for Performance Detection, detected result is as shown in table 3.
Embodiment 5:
1. select for use mean particle size 80 μ m diamond particles to carry out pre-treatment, oil removing: place 10%NaOH solution violent stirring to boil 30min in diamond, the back is extremely neutral with distilled water flushing; Alligatoring: in 30% dilute nitric acid solution, boil 30min then, extremely neutral with distilled water flushing again.
2. diamond surface Electroless Cu Plating, diamond electroless copper condition: CuSO
45H
2O 15gL
-1, 36% formaldehyde 15gL
-1, Seignette salt 14gL
-1, EDTA 14.6gL
-1, NaOH adjusts pH, duplex pyridine 0.02gL in right amount
-1, yellow prussiate of potash 0.01gL
-1, pH value 12.5,43 ℃ of temperature, plating time 100 minutes, thickness of coating 6 μ m;
3. the diamond particles homodisperse behind the electroless copper being placed copper mould, is negative electrode with this mould, and copper-bath is an electrolytic solution, and the fine copper plate is an anode, carries out galvanic deposit, and electrodeposit liquid is formed: copper sulfate (CuSO
45H
2O) 250gL
-1, the vitriol oil (H
2SO
4) 65gL
-1, chlorion (Cl
-1) 0.06gL
-1, sodium polydithio-dipropyl sulfonate 0.1gL
-1, polyoxyethylene glycol 0.1gL
-1Electrodeposition technology condition: current density 10Adm
-2, stirring velocity 150rmin
-1, 25 ℃ of temperature, depositing time 10 hours makes copper separate out and gradually diamond particles be buried at negative electrode and covers, electric deposition device as shown in Figure 5;
4. adopt wire cutting technology that the goods that galvanic deposit obtains are cut into desired size, be used for Performance Detection, detected result is as shown in table 3.
Diamond/copper composite encapsulating material the performance of table 3 electrodip process preparation.
| Numbering | Diamond weight mark (%) | Thermal conductivity (W/ (mK)) | Thermal expansivity (* 10 -6/℃) |
| Embodiment 1 | 2 | 378.5 | 13.2 |
| |
28 | 473.1 | 7.2 |
| |
60 | 528.0 | 6.5 |
| |
15 | 420.8 | 8.8 |
| Embodiment 5 | 42 | 501.5 | 6.8 |
Claims (5)
1, a kind of super-high heat-conductive diamond-copper composite package material, constitute by copper matrix and the additive that is distributed in heat conduction, the intensity enhancing thing diamond particles in the copper matrix and improves interface bonding state, it is characterized in that: described body material is a copper, described heat conduction, intensity enhancing thing diamond particles content are 2～60% in mass, select for use particle size range to be: 1 μ m～150 μ m, described additive is copper or silver.
2, the method for the described super-high heat-conductive diamond-copper composite package material of production claim 1 is characterized in that: the steps include:
A. diamond pre-treatment: after selecting for use particle size range to be the diamond oil removing, roughening treatment of 1 μ m～150 μ m, activate again and sensitization;
The diamond particles that B. will activate after the sensitization carries out electroless plating, plates layer of copper or silver on the diamond particles surface, and thickness of coating is 0.1～6 μ m;
C. the diamond particles homodisperse behind electroless copper or the silver is placed a metal die, and be negative electrode with this mould, copper-bath is an electrolytic solution, the fine copper plate is an anode, carry out galvanic deposit, make copper separate out and gradually diamond particles be buried at negative electrode and cover, regulate the preparation sample thickness by the control electrodeposition time, making diamond particles content is 2～60% in mass;
D. cut processing: with the materials processing desired size.
3, the production method of super-high heat-conductive diamond-copper composite package material according to claim 2 is characterized in that: electrodeposit liquid is formed: copper sulfate (CuSO
45H
2O) 80-250gL
-1, the vitriol oil (H
2SO
4) 65gL
-1, chlorion (Cl
-1) 0.06gL
-1, sodium polydithio-dipropyl sulfonate 0.1gL
-1, polyoxyethylene glycol 0.1gL
-1Electrodeposition technology condition: current density 2.2-10Adm
-2, stirring velocity 150-500rmin
-1, 25 ℃ of temperature.
4, according to the production method of claim 2 or 3 described super-high heat-conductive diamond-copper composite package materials, it is characterized in that: diamond electroless copper condition: CuSO
45H
2O 15gL
-1, 36% formaldehyde 15gL
-1, Seignette salt 14gL
-1, EDTA 14.6gL
-1, NaOH adjusts pH, duplex pyridine 0.02gL in right amount
-1, yellow prussiate of potash 0.01gL
-1, pH value 12.5,43 ℃ of temperature, time 20-100min.
5, according to the production method of claim 2 or 3 described super-high heat-conductive diamond-copper composite package materials, it is characterized in that: diamond chemical silvering condition: AgNO
31.5gL
-1, ammoniacal liquor 10gL
-1, formaldehyde 0.15mLL
-1, ethanol 100mLL
-1, 35 ℃ of temperature, time 5-60min.
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|---|---|---|---|
| CN2007100349510A CN101070461B (en) | 2007-05-18 | 2007-05-18 | Super-high heat-conductive diamond-copper composite package material and production method |
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| CN108950283A (en) * | 2018-07-13 | 2018-12-07 | 长沙博朗思达新材料科技有限公司 | A kind of preparation method of diamond/copper composite material |
| CN111805988A (en) * | 2020-07-21 | 2020-10-23 | 蒋孟瑶 | Copper-based diamond cooling fin and preparation method thereof |
| CN111805988B (en) * | 2020-07-21 | 2022-08-02 | 蒋孟瑶 | Copper-based diamond cooling fin and preparation method thereof |
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| CN112877560B (en) * | 2021-01-12 | 2022-02-08 | 江西离子型稀土工程技术研究有限公司 | Diamond/copper composite material and preparation method thereof |
| CN115418200A (en) * | 2022-09-02 | 2022-12-02 | 常州大学 | High-strength high-heat-conductivity low-roughness graphene/copper composite material and preparation method thereof |
| CN115475938A (en) * | 2022-09-23 | 2022-12-16 | 安徽工程大学 | Copper-based diamond composite board/strip and preparation method thereof |
| CN115475938B (en) * | 2022-09-23 | 2024-03-08 | 安徽工程大学 | Copper-based diamond composite board/strip and preparation method thereof |
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