CN-121972664-A - Method for enhancing bonding strength between diamond particles and copper matrix

Abstract

The invention provides a method for enhancing the bonding strength between diamond particles and a copper matrix, and relates to the technical field of preparation of diamond copper composite materials. The method is characterized in that diamond particles are subjected to laser perforation, acid washing treatment, ultrasonic cleaning treatment, activation treatment, ultrasonic mixing and drying, and ultrasonic mixing and drying final heat treatment to obtain the diamond copper composite material capable of being tightly combined with copper. The heat-conducting property and the mechanical property of the diamond copper composite material prepared by the method can be synergistically improved, and the method is simple, convenient, easy to operate, low in cost, low in energy consumption, high in efficiency and beneficial to industrial mass production and popularization.

Inventors

• WEI JUNJUN
• YI TAO
• CHEN LIANGXIAN
• LIU YIBO
• HUANG XIA
• LIU JINLONG
• LI CHENGMING

Assignees

• 北京科技大学
• 北京安泰钢研超硬材料制品有限责任公司

Dates

Publication Date

20260505

Application Date

20260121

Claims (10)

1. 1. A method of enhancing the bond strength between diamond particles and a copper substrate, the method comprising the steps of: s1, laser perforation, namely uniformly filling diamond particles on a porous array die, and carrying out batch perforation treatment on the diamond particles through a modulated pulse laser array to obtain perforated diamond particles; s2, pickling, namely putting the perforated diamond particles of the S1 into a pickling solution for pickling to obtain perforated diamond particles with clean surfaces; s3, ultrasonic cleaning treatment, namely putting the perforated diamond particles with the clean surfaces of the S2 into an acetone solution for ultrasonic cleaning to obtain pure perforated diamond particles; s4, activating, namely placing the pure perforated diamond particles in the S3 in a tube furnace, and introducing hydrogen to perform activating to obtain activated perforated diamond particles; S5, ultrasonic mixing and drying, namely putting the activated perforated diamond particles of S4 into an acetone solution containing titanium isopropoxide metal organic matters, ultrasonic mixing and drying in a drying box to obtain a mixture of uniformly attaching titanium isopropoxide to the surfaces of the diamond particles; S6, final heat treatment, namely placing the mixture of the titanium isopropoxide of S5 uniformly attached to the surfaces of the diamond particles in a tubular furnace, and introducing argon gas to perform final heat treatment to obtain the diamond particles with the surfaces plated with the metal titanium; And S7, preparing the diamond copper composite material, namely mixing diamond particles with metal titanium plated on the surface of the S6 with copper powder, and carrying out spark plasma sintering to obtain the diamond copper composite material.
2. 2. The method for enhancing the bonding strength between diamond particles and a copper substrate according to claim 1, wherein the perforated diamond particles in S1 have a particle size of 50 to 600 μm and the perforated pore diameter is 1/5 to 1/3 of the particle size of the diamond particles.
3. 3. The method for enhancing the bonding strength between diamond particles and a copper substrate according to claim 1, wherein the pickling solution in S2 is obtained by mixing 98% of concentrated sulfuric acid and 99.7% of concentrated nitric acid in a ratio of 3:1, and the pickling treatment is performed for 0.5 to 2 hours.
4. 4. The method for enhancing the bonding strength between diamond particles and a copper substrate according to claim 1, wherein the concentration of acetone in S3 is required to be 99.6% or more, the ultrasonic frequency of ultrasonic cleaning is 40-100kHz, and the cleaning time is 0.5-3h.
5. 5. The method for enhancing the bonding strength between diamond particles and a copper substrate according to claim 1, wherein the vacuum state in S4 has a vacuum degree of 1 to 30Pa, a hydrogenation temperature of 750 to 950 ℃, a temperature rising rate of 10 to 20 ℃ per minute, a hydrogen flow rate of 5 to 30sccm, and a treatment time of 30 to 120 minutes.
6. 6. The method for enhancing the bonding strength between diamond particles and a copper substrate according to claim 1, wherein the content of titanium isopropoxide metal organic matters in the acetone solution of the titanium isopropoxide metal organic matters in the S5 is 50-75wt%, the purity of the titanium isopropoxide metal organic matters is not lower than 98%, the ultrasonic frequency of ultrasonic mixing is 30-50kHz, the ultrasonic time is 60-180min, the drying temperature is 30-50 ℃ and the drying time is 30-120min.
7. 7. The method for enhancing the bonding strength between diamond particles and a copper substrate according to claim 1, wherein the titanium isopropoxide in S5 is uniformly adhered to the surface of the diamond particles in a mixture having a particle size of 51 to 602 μm and an adhesion thickness of 1000 to 2000nm.
8. 8. The method of claim 1, wherein the argon gas flow in S6 is 5-30sccm, the heating rate is 10-20 ℃ per minute, the final heat treatment temperature is 500-700 ℃ per minute, and the final heat treatment time is 30-90 minutes.
9. 9. The method for enhancing the bonding strength between diamond particles and a copper substrate according to claim 1, wherein the overall particle diameter of the diamond particles surface-plated with metallic titanium in S6 is 50 to 600 μm and the metallic titanium layer thickness is 100 to 500nm.
10. 10. The method for enhancing the bonding strength between diamond particles and a copper substrate according to claim 1, wherein the volume ratio of diamond particles with surface plated metallic titanium in S7 to copper powder is 5:5-7:3, the temperature of spark plasma sintering is 850-1000 ℃, and the holding time is 5-30min.

Description

Method for enhancing bonding strength between diamond particles and copper matrix Technical Field The invention relates to the technical field of preparation of diamond copper composite materials, in particular to a method for enhancing the bonding strength between diamond particles and a copper matrix. Background Miniaturization and integration of electronic devices increase the heat flux density of the power devices, thereby affecting the heat dissipation of the devices. This requires a higher thermal conductivity to improve heat dissipation and stabilize the device performance. Diamond is widely used in electronic devices because of its unique and excellent properties, and is the substance with the highest brinell hardness in nature, and at the same time, the thermal conductivity is the highest in nature. The metal copper is widely applied to the field of electronic packaging due to the excellent performance, and the diamond has good heat conduction potential, has higher heat conductivity and lower thermal expansion coefficient, and can effectively solve the heat dissipation problem of a power device. However, the interface bonding between diamond and copper is weak, and the wettability between diamond and copper is too poor, so that the diamond is subjected to surface treatment, the wetting angle between diamond and copper is reduced, and good interface bonding is formed, so that the aim of improving the heat conductivity is fulfilled. To solve the interface problem between diamond and copper, there are generally two types of methods, one is diamond surface metallization and one is matrix alloying. The diamond surface metallization effect is better than matrix alloying in the two methods. Common methods for metallizing diamond surfaces include vacuum plating, magnetron sputtering, and the like, which have drawbacks such as uneven coating and high cost. Chinese patent CN115821211A discloses a method for preparing diamond/copper composite material at low temperature and high pressure, which adopts PVD method to deposit nano titanium layer on the surface of diamond monocrystal particle, then mixes with copper powder by wet method, and obtains the product by low temperature low pressure vacuum exhaust sintering and low temperature high pressure densification sintering, and obviously the method has the defects of incapability of industrial application, serious heat management performance and the like. Chinese patent CN104625077A discloses a high heat conduction diamond/copper composite material and a preparation method thereof, wherein the method adopts a magnetron sputtering method to plate titanium or chromium on the surfaces of diamond particles with different particle diameters respectively, places a metal copper sheet on the diamond particles for assembly, loads the diamond particles into a pyrophyllite mold after vacuum heat treatment, and finally carries out ultrahigh pressure infiltration sintering under different sintering process conditions to prepare the high heat conduction diamond copper composite material, which obviously has the advantages of much higher preparation cost, high-temperature and high-pressure sintering, complex operation process and adverse industrial production. Chinese patent CN113462924A discloses a titanium-plated diamond copper composite material and a preparation method thereof, wherein the titanium-plated diamond copper composite material is prepared by plating a titanium layer on the surface of diamond particles through a vacuum evaporation plating method and carrying out vacuum hot-pressing sintering on copper powder and titanium-plated diamond powder to prepare titanium-plated diamond copper alloy, and then crushing, ball milling and drying are carried out to obtain powder for producing the titanium-plated diamond copper composite material through an SLM (selective laser deposition) process. Disclosure of Invention The invention mainly aims to solve the technical problems that in the prior art, interface bonding between diamond and copper is weak, wettability between diamond and copper is too poor, wetting is difficult, and heat conduction performance, electric conduction performance, mechanical performance and the like of a diamond copper composite material cannot be comprehensively improved. Therefore, a method for enhancing the bonding strength between diamond particles and a copper matrix is proposed, which can solve the problems, and the diamond particles are perforated by laser, and metal organic matters are combined with the diamond particles to achieve the effects of uniform coating and enhanced interface bonding. The technical scheme is as follows: A method of enhancing the bond strength between diamond particles and a copper substrate, the method of enhancing the bond strength between diamond particles and a copper substrate comprising the steps of: s1, laser perforation, namely uniformly filling diamond particles on a porous array die, and carrying out batch