阅读说明：本技术 一种高导热碳铜的快速制备方法 (Rapid preparation method of high-thermal-conductivity carbon copper ) 是由 余欢欢 余继洋 余欢龙 于 2021-10-13 设计创作，主要内容包括：本发明公开了一种高导热碳铜的快速制备方法,包括混料、还原处理、装炉真空烧结、冷却这几个步骤,其碳粉、铜粉按比例混合,在高能球磨机的机械咬合搅拌下可以更好地在球磨过程中让铜粉去包裹碳粉,粉料均质性达最佳状态且混合时间相对短,随后填充粉料到模具装炉烧结通过调节升温速度使粉末快速达到塑化状态,并在高达80Mpa以上压力下快速成型,碳铜合金完全致密；同时这种工艺在真空状态下,温度相对比普通工艺温度较低且均匀,使得烧结且合金化时间短,整个生产高效连贯性促使这种工艺效率高,烧结成型的碳铜合金导热率可达670W/m.k以上,强度也随之提高,能更好地满足碳铜合金在基板、半导体及电子封装领域的应用。(The invention discloses a method for quickly preparing high-thermal-conductivity carbon copper, which comprises the steps of mixing, reduction treatment, furnace charging and vacuum sintering and cooling, wherein carbon powder and copper powder are mixed in proportion, the copper powder can be better wrapped by the carbon powder in the ball milling process under the mechanical interlocking stirring of a high-energy ball mill, the homogeneity of the powder is in an optimal state, the mixing time is relatively short, then the powder is filled into a die and charged for sintering, the powder is quickly plasticized by adjusting the temperature rise speed, the powder is quickly molded under the pressure of more than 80Mpa, and the carbon copper alloy is completely compact; meanwhile, the temperature of the process is lower and uniform than that of the common process in a vacuum state, so that the sintering and alloying time is short, the efficiency of the process is high due to the high-efficiency continuity of the whole production, the thermal conductivity of the sintered and formed carbon-copper alloy can reach more than 670W/m.k, the strength is improved, and the application of the carbon-copper alloy in the fields of substrates, semiconductors and electronic packaging can be better met.)

1. A rapid preparation method of carbon copper with high thermal conductivity is characterized by comprising the following steps,

s1: mixing materials, namely filling carbon powder into a high-energy ball mill according to a formula proportion, then filling copper powder, covering the carbon powder with the copper powder, and finally covering and filling zirconium balls on the surfaces of the copper powder, wherein the ratio of the zirconium balls to the total weight of the copper powder and the carbon powder is 5: 1, starting the high-energy ball mill to mix materials according to set time;

s2: reduction treatment, namely, reducing the powder obtained by ball milling and mixing in the step S1 for 2 hours in a hydrogen furnace at the temperature of 380-400 ℃;

s3: charging and vacuum sintering, namely charging the powder subjected to reduction treatment in the step S2 into a mold, conveying the powder into a sintering furnace, sintering the powder in a vacuum environment, maintaining the pressure for 10-60S under the condition of 20Mpa, and then heating; when the powder is plasticized, the pressure is increased to 120Mpa at the rate of every 5Mpa, and the temperature is increased to 480 ℃ at the temperature rising speed of 55 ℃/min;

after the powder is completely plasticized, heating to 860-920 ℃ at the heating rate of 22 ℃/min, and maintaining the pressure for 5-15min under the pressure condition of 120 Mpa;

s4: cooling for 2 h.

2. The method for rapidly preparing carbon copper with high thermal conductivity according to claim 1, wherein the zirconium balls have a sphere diameter of 3mm, 5mm or 10 mm.

3. The method for rapidly preparing carbon-copper with high thermal conductivity according to claim 1, wherein in step S3, the pressure is maintained at 20Mpa for 10-60S, and then the temperature is increased at a temperature increasing rate of 120 ℃/min until the powder begins to plasticize.

4. The method for rapidly preparing carbon copper with high thermal conductivity as claimed in claim 1, wherein the carbon powder is natural crystalline flake graphite with a particle size of 3-4 mm.

5. The method for rapidly preparing carbon copper with high thermal conductivity according to claim 1, wherein the mixing time of the high-energy ball mill is 2-3 h.

Technical Field

The invention belongs to the technical field of carbon-copper alloy production, and particularly relates to a preparation method of high-thermal-conductivity carbon copper.

Background

The carbon-copper alloy has the thermal conductivity and good layering of carbon, the strength and the electrical conductivity of copper, and has a wide market application prospect, but the carbon-copper alloy is a material which is extremely difficult to form compactly and achieve high thermal conductivity. The carbon-copper alloy produced by the traditional mould pressing process commonly used in the market has the advantages of uneven material distribution, loose compactness and poor heat conduction effect, the heat conductivity can only reach the heat conductivity of copper, namely 310-350W/m.k, and the market requirement can not be completely met, so that the application of the carbon-copper alloy can not be well popularized, and the carbon-copper alloy can only be used reluctantly under the condition of reducing the material performance even if being applied to some extent. Meanwhile, the production of the existing carbon-copper alloy also has the problems of long production period and low efficiency.

Disclosure of Invention

Aiming at the defects of the prior art, the invention aims to provide a rapid preparation method of high-thermal conductivity carbon copper, which can prepare carbon copper alloy with uniform and compact material distribution, high thermal conductivity and stable performance, and has short production period and high production efficiency.

In order to achieve the purpose, the invention adopts the following technical scheme:

a method for rapidly preparing carbon copper with high thermal conductivity comprises the following steps,

s1: mixing materials, namely filling carbon powder into a high-energy ball mill according to a formula proportion, then filling copper powder, covering the carbon powder with the copper powder, and finally covering and filling zirconium balls on the surface of the copper powder, wherein the ratio of the weight parts of the zirconium balls to the total weight of the copper powder and the carbon powder is 5: 1, and starting the high-energy ball mill to mix the materials according to a set time;

s2: reduction treatment, namely, reducing the powder obtained by ball milling and mixing in the step S1 for 2 hours in a hydrogen furnace at the temperature of 380-400 ℃;

s3: charging and vacuum sintering, namely charging the powder subjected to reduction treatment in the step S2 into a mold, conveying the powder into a sintering furnace, sintering the powder in a vacuum environment, maintaining the pressure for 10-60S under the condition of 20Mpa, and then heating; when the powder is plasticized, the pressure is increased to 120Mpa at the rate of every 5Mpa, and the temperature is increased to 480 ℃ at the temperature rising speed of 55 ℃/min; after the powder is completely plasticized, heating to 860-920 ℃ at the heating rate of 22 ℃/min, and maintaining the pressure for 5-15min under the pressure condition of 120 Mpa;

s4: cooling for 2 h.

According to the preparation method of the carbon-copper alloy, carbon powder and copper powder are mixed in proportion, the copper powder can be better wrapped by the carbon powder in the ball milling process under the mechanical interlocking stirring of a high-energy ball mill, the homogeneity of the powder is in an optimal state, the mixing time is relatively short, then the powder is filled into a die, the powder is rapidly in a plasticized state by adjusting the temperature rise speed and is rapidly molded in place under the pressure of more than 80MPa, and the carbon-copper alloy is completely compact; meanwhile, the temperature of the process is lower and uniform than that of the common process in a vacuum state, so that the sintering and alloying time is short, the efficiency of the process is high due to the high-efficiency continuity of the whole production, the thermal conductivity of the finally sintered and formed carbon-copper alloy can reach more than 670W/m.k, the strength is improved, and the application of the carbon-copper alloy in the fields of substrates, semiconductors and electronic packaging can be better met.

The invention has the following beneficial effects:

the rapid preparation method of the high-thermal-conductivity carbon copper has the characteristics of uniform and compact material distribution, high thermal conductivity and stable performance, the thermal conductivity of the prepared carbon copper alloy can reach more than 670W/m.k, and meanwhile, the method is beneficial to shortening the production period of the carbon copper alloy and improving the production efficiency.

Drawings

Fig. 1 is a test report of the thermal conductivity of the carbon-copper alloy prepared by the rapid preparation method of high thermal conductivity carbon-copper of the invention.

Detailed Description

The invention will be further described with reference to the accompanying drawings and specific embodiments so as to more clearly understand the technical idea of the invention claimed.

A method for rapidly preparing carbon copper with high thermal conductivity comprises the following steps,

s1: mixing materials, namely filling carbon powder into a high-energy ball mill according to a formula proportion, wherein the carbon powder preferably adopts natural crystalline flake graphite with the particle size of 3-4mm, then filling copper powder, covering the copper powder with the carbon powder, and finally covering and filling zirconium balls on the surfaces of the copper powder, wherein the zirconium balls can adopt zirconium balls with the particle size of 3mm, 5mm or 10mm according to the ball diameter, the ratio of the zirconium balls to the total weight of the copper powder and the carbon powder is 5: 1 according to the weight part, starting the high-energy ball mill for mixing materials according to a set time, and the starting time for mixing materials is preferably 2-3 h;

s2: reduction treatment, namely reducing the powder obtained by ball milling and mixing in the step S1 at the temperature of 380-400 ℃ for 2h in a hydrogen furnace in a heat preservation way to treat the deoxidation content of the powder obtained by ball milling and mixing;

s3: loading into a furnace and sintering in vacuum, namely loading the powder subjected to reduction treatment in the step S2 into a mold, conveying the powder into a sintering furnace, sintering in a vacuum environment, maintaining the pressure for 10-60S under the condition of 20MPa, and then heating, preferably at the heating speed of 120 ℃/min until the powder starts to plasticize; when the powder is plasticized, the pressure is increased to 120Mpa at the rate of every 5Mpa, and the temperature is increased to 480 ℃ at the temperature rising speed of 55 ℃/min; after the powder is completely plasticized, heating to 860-920 ℃ at the heating rate of 22 ℃/min, and maintaining the pressure for 5-15min under the pressure condition of 120 Mpa;

s4: and cooling for 2h to obtain the carbon-copper alloy with uniform and compact material distribution, high thermal conductivity and stable performance.

It should be noted that the above mentioned high energy ball mill, hydrogen furnace and sintering furnace all belong to the prior art, and the specific structure thereof is not described herein.

According to the method for quickly preparing the high-thermal-conductivity carbon copper, the carbon powder and the copper powder are mixed in proportion, the copper powder can be better wrapped by the carbon powder in the ball milling process under the mechanical interlocking stirring of a high-energy ball mill, the homogeneity of the powder is in an optimal state, the mixing time is relatively short, then the powder is filled into a die, the temperature rising speed is adjusted to enable the powder to be in a plasticized state quickly, the powder is quickly molded in place under the pressure of more than 80MPa, and the carbon copper alloy is completely compact; meanwhile, the temperature of the process is lower and uniform than that of the common process in a vacuum state, so that the sintering and alloying time is short, the efficiency of the process is high due to the high-efficiency continuity of the whole production, the thermal conductivity of the finally sintered and formed carbon-copper alloy can reach more than 670W/m.k as shown in a heat conductivity test report shown in figure 1, the strength is improved accordingly, and the application of the carbon-copper alloy in the fields of substrates, semiconductors and electronic packaging can be better met.

Various other changes and modifications to the above-described embodiments and concepts will become apparent to those skilled in the art from the above description, and all such changes and modifications are intended to be included within the scope of the present invention as defined in the appended claims.