CN101406955A - Method for preparing powder deformed composite material - Google Patents

Method for preparing powder deformed composite material Download PDF

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Publication number
CN101406955A
CN101406955A CNA2008102095424A CN200810209542A CN101406955A CN 101406955 A CN101406955 A CN 101406955A CN A2008102095424 A CNA2008102095424 A CN A2008102095424A CN 200810209542 A CN200810209542 A CN 200810209542A CN 101406955 A CN101406955 A CN 101406955A
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powder
composite material
specific embodiment
blank
preparation
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于洋
王尔德
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Abstract

The invention relates to a method for preparing a powder deformation composite material, which relates to a method for preparing a composite material. The method solves the problems that the prior method for preparing the composite material of W-Cu and Mo-Cu has high equipment cost, difficulty in precise control of components, complex technical process, high product price, low product relative density which is lower than 99 percent, difficult two-phase interface combination of the product, and low performance after heat treatment, and the method for preparing high-tungsten and high-molybdenum composite materials of the W-Cu and the Mo-Cu by adopting large extrusion ratio is difficult to use practically in industry. The method comprises the following steps: firstly, preparing composite powders; secondly, preparing a cold pressing blank and then sintering the blank; thirdly, performing hot extrusion on the sintered blank; and fourthly, performing heat treatment on the blank after the hot extrusion to obtain the powder deformation composite material. The method adopts the prior equipment, thus the cost is low, the process is simple, the relative density of the product is between 99.5 and 99.6, and the composite material can be prepared by adopting the large extrusion ratio; besides, the method is applicable to industrial production, and the powder deformation composite material has good performance after the heat treatment.

Description

A kind of preparation method of powder deformed composite material
Technical field
The present invention relates to a kind of preparation method of composite.
Background technology
W-Cu in the powder deformed composite material and Mo-Cu composite are owing to contain the tungsten of high-melting-point, high rigidity, the copper of molybdenum element and high conduction, thermal conductivity, make W-Cu and Mo-Cu composite combine the advantage of these two kinds of elements, have high-termal conductivity, electric conductivity, low thermal coefficient of expansion, nonmagnetic and preferable high-temperature behavior, so be widely used in fields such as the heat sink material of electronic devices such as the lead frame of electric discharging machining electrode material, electronic package material, large scale integrated circuit and solid state microwave pipe and space flight high-temperature material.But because tungsten is immiscible between molybdenum and the copper, only form pseudo-alloy between the two, to such an extent as to influence the combination property of alloy, and conventional founding and powder metallurgic method are difficult to produce high-end W-Cu and Mo-Cu composite.
At present, the preparation method of W-Cu and Mo-Cu composite mainly contains melting infiltration sintering method, activated sintering method, vacuum hot-pressing and hot isostatic pressing method, but these methods all exist that equipment cost height, composition are difficult to that accurate control, complex technical process, product price height, product density are lower than 99%, the product two-phase interface is in conjunction with the problem of difficulty; Adopt large extrusion ratio to prepare deformed composite material, the composite process that has the W-Cu (W is more than 70%) of high tungsten of preparation and high molybdenum and a Mo-Cu (Mo is more than 70%) is difficult to practical application industrial.Performance after the heat treatment of prior art for preparing gained W-Cu powder deformed composite material is low, and showing as the alloy electrical conductivity is 33.2m/ Ω .mm 2, hardness HV is 152, and thermal conductivity is 250W/mK, and thermal coefficient of expansion is 103 * 10 -7/ ℃, relative density is 98.8%.Performance after the heat treatment of prior art for preparing gained Mo-Cu powder deformed composite material is low, and showing as the alloy electrical conductivity is 28m/ Ω .mm 2, hardness is HB85, and thermal conductivity is 206W/mK, and thermal coefficient of expansion is 103 * 10 -7/ ℃, relative density is 98.5%.
Summary of the invention
The present invention seeks to be difficult to for the preparation method who solves existing W-Cu and Mo-Cu composite exists equipment cost height, composition that accurate control, complex technical process, product price height, product relative density are lower than 99%, the performance of product two-phase interface after in conjunction with difficulty, heat treatment is low and adopts composite process that large extrusion ratio prepares the W-Cu of high tungsten and high molybdenum and Mo-Cu, and a kind of preparation method of powder deformed composite material is provided in the industrial problem that is difficult to practical application.
The preparation method of powder deformed composite material realizes according to the following steps: one, by weight percentage with 10%~90% copper powder and 10%~90% tungsten powder or molybdenum powder mechanical mixture 60h under the condition of 60r/min, composite powder; Two, composite powder is made the blank of colding pressing through the pressure of 500~1000MPa, place vacuum drying oven then, being evacuated to vacuum is 10 -2Pa is warming up to 900~1000 ℃ and be incubated 30min with the speed of 10 ℃/min, is warming up to 1120~1350 ℃ and be incubated 90min with the speed of 20 ℃/min again, reduces to room temperature with the speed of 20 ℃/min subsequently, the sintering blank; Three, the sintering blank being preheated to 850~950 ℃ and be incubated 30min, putting into mould then, is that 500~600MPa, extrusion ratio are hot extrusion 3~6s under 6~40 the condition at 300 ℃ of mold preheating temperatures, pressure; Four, the blank after the hot extrusion is placed vacuum drying oven, being evacuated to vacuum is 10 -2Pa is warming up to 600~1000 ℃ and be incubated 1~3h with the speed of 5~20 ℃/min, reduces to room temperature with the speed of 10~40 ℃/min then, promptly gets powder deformed composite material; Wherein copper powder is that Fisher particle size is that 20~100 μ m, quality purity are the electrolytic copper powder more than 99.5% in the step 1.
The preparation of W-Cu and Mo-Cu powder deformed composite material is adopted among the present invention is conventional equipment, cost is low, technology is simple, and composition can accurately be controlled, and the price of product reduces, the product relative density is 99.5~99.6, the product two-phase interface can adopt large extrusion ratio to prepare the W-Cu and the Mo-Cu composite of high tungsten and high molybdenum in conjunction with easily, is fit to suitability for industrialized production, W is up to 70%~90% in the W-Cu composite, and Mo is up to being 70%~90% in the Mo-Cu composite; Performance among the present invention after the heat treatment of W-Cu powder deformed composite material is good, and showing as the bar electrical conductivity is 36.5~37.0m/ Ω .mm 2, hardness HV is 180~183, and thermal conductivity is 254~257W/mK, and thermal coefficient of expansion is 100 * 10 -7~102 * 10 -7/ ℃, relative density is 99.6%~99.7%; The sheet material electrical conductivity is 33.1~33.3m/ Ω .mm 2, thermal conductivity is 238~240W/mK, thermal coefficient of expansion is 100 * 10 -7~102 * 10 -7/ ℃, hardness HV is 171~173, relative density is 99.5%~99.6%.Performance among the present invention after the heat treatment of Mo-Cu powder deformed composite material is good, and showing as the bar electrical conductivity is 33.8~34.0m/ Ω .mm 2, thermal conductivity is 252~253W/mK, thermal coefficient of expansion is 101 * 10 -7~102 * 10 -7/ ℃, hardness HV is 160~163, relative density is 99.6%~99.7%; The sheet material electrical conductivity is 29.5~30.0m/ Ω .mm 2, thermal conductivity is 238~240W/mK, thermal coefficient of expansion is 97 * 10 -7~98 * 10 -7/ ℃, hardness HV is 158~160, relative density is 99.6%~99.7%.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: the preparation method of present embodiment powder deformed composite material realizes according to the following steps: one, by weight percentage with 10%~90% copper powder and 10%~90% tungsten powder or molybdenum powder mechanical mixture 60h under the condition of 60r/min, composite powder; Two, composite powder is made the blank of colding pressing through the pressure of 500~1000MPa, place vacuum drying oven then, being evacuated to vacuum is 10 -2Pa is warming up to 900~1000 ℃ and be incubated 30min with the speed of 10 ℃/min, is warming up to 1120~1350 ℃ and be incubated 90min with the speed of 20 ℃/min again, reduces to room temperature with the speed of 20 ℃/min subsequently, the sintering blank; Three, the sintering blank being preheated to 850~950 ℃ and be incubated 30min, putting into mould then, is that 500~600MPa, extrusion ratio are hot extrusion 3~6s under 6~40 the condition at 300 ℃ of mold preheating temperatures, pressure; Four, the blank after the hot extrusion is placed vacuum drying oven, being evacuated to vacuum is 10 -2Pa is warming up to 600~1000 ℃ and be incubated 1~3h with the speed of 5~20 ℃/min, reduces to room temperature with the speed of 10~40 ℃/min then, promptly gets powder deformed composite material; Wherein copper powder is that Fisher particle size is that 20~100 μ m, quality purity are the electrolytic copper powder more than 99.5% in the step 1.
The relative density of blank of colding pressing in the present embodiment is 85%.
The relative density of sintering blank is 97% in the present embodiment.
The specific embodiment two: present embodiment and the specific embodiment one are different is by weight percentage with 10%~30% copper powder and 70%~90% tungsten powder or molybdenum powder mechanical mixture 60h under the condition of 60r/min in the step 1.Other step and parameter are identical with the specific embodiment one.
The specific embodiment three: present embodiment and the specific embodiment one are different is by weight percentage with 15%~25% copper powder and 75%~85% tungsten powder or molybdenum powder mechanical mixture 60h under the condition of 60r/min in the step 1.Other step and parameter are identical with the specific embodiment one.
The specific embodiment four: present embodiment and the specific embodiment one are different is by weight percentage with 15%~85% copper powder and 15%~85% tungsten powder or molybdenum powder mechanical mixture 60h under the condition of 60r/min in the step 1.Other step and parameter are identical with the specific embodiment one.
The specific embodiment five: present embodiment and the specific embodiment one are different is by weight percentage with 10% copper powder and 90% tungsten powder or molybdenum powder mechanical mixture 60h under the condition of 60r/min in the step 1.Other step and parameter are identical with the specific embodiment one.
The specific embodiment six: present embodiment and the specific embodiment one are different is by weight percentage with 20% copper powder and 80% tungsten powder or molybdenum powder mechanical mixture 60h under the condition of 60r/min in the step 1.Other step and parameter are identical with the specific embodiment one.
The specific embodiment seven: present embodiment and the specific embodiment one are different is by weight percentage with 25% copper powder and 75% tungsten powder or molybdenum powder mechanical mixture 60h under the condition of 60r/min in the step 1.Other step and parameter are identical with the specific embodiment one.
The specific embodiment eight: what present embodiment and the specific embodiment one were different is that copper powder is that Fisher particle size is 30~90 μ m in the step 1, and quality purity is 99.7% electrolytic copper powder.Other step and parameter are identical with the specific embodiment one.
The specific embodiment nine: what present embodiment and the specific embodiment one were different is that copper powder is that Fisher particle size is 70 μ m in the step 1, and quality purity is 99.8% electrolytic copper powder.Other step and parameter are identical with the specific embodiment one.
The specific embodiment ten: present embodiment and the specific embodiment one are different is that the Fisher particle size of tungsten powder in the step 1 is 2~10 μ m, and quality purity is more than 99.5%.Other step and parameter are identical with the specific embodiment one.
The specific embodiment 11: present embodiment and the specific embodiment one are different is that the Fisher particle size of tungsten powder in the step 1 is 3~9 μ m, and quality purity is 99.7%.Other step and parameter are identical with the specific embodiment one.
The specific embodiment 12: present embodiment and the specific embodiment one are different is that the Fisher particle size of tungsten powder in the step 1 is 8 μ m, and quality purity is 99.9%.Other step and parameter are identical with the specific embodiment one.
The specific embodiment 13: present embodiment and the specific embodiment one are different is that the Fisher particle size of molybdenum powder in the step 1 is 2~10 μ m, and quality purity is more than 99.5%.Other step and parameter are identical with the specific embodiment one.
The specific embodiment 14: present embodiment and the specific embodiment one are different is that the Fisher particle size of molybdenum powder in the step 1 is 3~9 μ m, and quality purity is 99.8%.Other step and parameter are identical with the specific embodiment one.
The specific embodiment 15: present embodiment and the specific embodiment one are different is that the Fisher particle size of molybdenum powder in the step 1 is 7 μ m, and quality purity is 99.9%.Other step and parameter are identical with the specific embodiment one.
The specific embodiment 16: what present embodiment and the specific embodiment one were different is that composite powder is made the blank of colding pressing through the pressure of 550~950MPa in the step 2.Other step and parameter are identical with the specific embodiment one.
The specific embodiment 17: what present embodiment and the specific embodiment one were different is that composite powder is made the blank of colding pressing through the pressure of 600MPa in the step 2.Other step and parameter are identical with the specific embodiment one.
The specific embodiment 18: what present embodiment and the specific embodiment one were different is that composite powder is made the blank of colding pressing through the pressure of 700MPa in the step 2.Other step and parameter are identical with the specific embodiment one.
The specific embodiment 19: what present embodiment and the specific embodiment one were different is to be warming up to 950 ℃ and insulation in the step 2.Other step and parameter are identical with the specific embodiment one.
The specific embodiment 20: what present embodiment and the specific embodiment one were different is to be warming up to 1200 ℃ and insulation in the step 2.Other step and parameter are identical with the specific embodiment one.
The specific embodiment 21: present embodiment and the specific embodiment one are different is in the step 3 sintering blank to be preheated to 850~950 ℃ and be incubated 30min.Other step and parameter are identical with the specific embodiment one.
The specific embodiment 22: present embodiment and the specific embodiment one are different is to be that 520~580MPa, extrusion ratio are hot extrusion 4~5s under 7~25 the condition at 300 ℃ of mold preheating temperatures, pressure in the step 3.Other step and parameter are identical with the specific embodiment one.
The specific embodiment 23: what present embodiment and the specific embodiment one were different is evenly to apply aquadag in the step 3 mould.Other step and parameter are identical with the specific embodiment one.
The specific embodiment 24: present embodiment and the specific embodiment one are different is to be warming up to 700~900 ℃ and be incubated 1.5~2.5h with the speed of 5~15 ℃/min in the step 4, reduces to room temperature with the speed of 20~35 ℃/min then.Other step and parameter are identical with the specific embodiment one.
The specific embodiment 25: present embodiment and the specific embodiment one are different is to be warming up to 800 ℃ and be incubated 2h with the speed of 10 ℃/min in the step 4, reduces to room temperature with the speed of 30 ℃/min then.Other step and parameter are identical with the specific embodiment one.
The specific embodiment 26: the preparation method of present embodiment powder deformed composite material realizes according to the following steps: one, by weight percentage with 20% copper powder and tungsten powder mechanical mixture 60h under the condition of 60r/min of 80%, composite powder; Two, composite powder is made the blank of colding pressing through the pressure of 700MPa, place vacuum drying oven then, being evacuated to vacuum is 10 -2Pa is warming up to 1000 ℃ and be incubated 30min with the speed of 10 ℃/min, is warming up to 1150 ℃ and be incubated 90min with the speed of 20 ℃/min again, reduces to room temperature with the speed of 20 ℃/min subsequently, the sintering blank; Three, the sintering blank being preheated to 950 ℃ and be incubated 30min, putting into mould then, is that 600MPa, extrusion ratio are hot extrusion 6s under 7.85 and 16 the condition at 300 ℃ of mold preheating temperatures, pressure; Four, the blank after the hot extrusion is placed vacuum drying oven, being evacuated to vacuum is 10 -2Pa is warming up to 800 ℃ and be incubated 2h with the speed of 10 ℃/min, reduces to room temperature with the speed of 10 ℃/min then, promptly gets the W-Cu powder deformed composite material; Wherein copper powder is that Fisher particle size is that 40 μ m, quality purity are 99.8% electrolytic copper powder in the step 1; The Fisher particle size of tungsten powder is 5 μ m, and quality purity is more than 99.9%.
Performance in the present embodiment after the heat treatment of gained W-Cu powder deformed composite material is good, and showing as the bar electrical conductivity is 36.8m/ Ω .mm 2, hardness HV is 182, and thermal conductivity is 255W/mK, and thermal coefficient of expansion is 101 * 10 -7/ ℃, relative density is 99.6%; The sheet material electrical conductivity is 33.2m/ Ω .mm 2, thermal conductivity is 239W/mK, thermal coefficient of expansion is 102 * 10 -7/ ℃, hardness HV is 172, relative density is 99.5%.
The specific embodiment 27: the preparation method of present embodiment powder deformed composite material realizes according to the following steps: one, by weight percentage with 25% copper powder and 75% tungsten powder or molybdenum powder mechanical mixture 60h under the condition of 60r/min, composite powder; Two, composite powder is made the blank of colding pressing through the pressure of 600MPa, place vacuum drying oven then, being evacuated to vacuum is 10 -2Pa is warming up to 900 ℃ and be incubated 30min with the speed of 10 ℃/min, is warming up to 1120 ℃ and be incubated 90min with the speed of 20 ℃/min again, reduces to room temperature with the speed of 20 ℃/min subsequently, the sintering blank; Three, the sintering blank being preheated to 850 ℃ and be incubated 30min, putting into mould then, is that 500MPa, extrusion ratio are hot extrusion 6s under 7.85 and 16 the condition at 300 ℃ of mold preheating temperatures, pressure; Four, the blank after the hot extrusion is placed vacuum drying oven, being evacuated to vacuum is 10 -2Pa is warming up to 800 ℃ and be incubated 2h with the speed of 5 ℃/min, reduces to room temperature with the speed of 10 ℃/min then, promptly gets powder deformed composite material; Wherein copper powder is that Fisher particle size is 50 μ m in the step 1, and quality purity is the electrolytic copper powder more than 99.5%; The Fisher particle size of molybdenum powder is 6 μ m, and quality purity is more than 99.5%.
Performance in the present embodiment after the heat treatment of gained Mo-Cu powder deformed composite material is good, and showing as the bar electrical conductivity is 33.8m/ Ω .mm 2, thermal conductivity is 252W/mK, thermal coefficient of expansion is 102 * 10 -7/ ℃, hardness HV is 162, relative density is 99.6%; The sheet material electrical conductivity is 29.5m/ Ω .mm 2, thermal conductivity is 238W/mK, thermal coefficient of expansion is 98 * 10 -7/ ℃, hardness HV is 158, relative density is 99.6%.

Claims (10)

1, a kind of preparation method of powder deformed composite material, the preparation method who it is characterized in that powder deformed composite material realizes according to the following steps: one, by weight percentage with 10%~90% copper powder and 10%~90% tungsten powder or molybdenum powder mechanical mixture 60h under the condition of 60r/min, composite powder; Two, composite powder is made the blank of colding pressing through the pressure of 500~1000MPa, place vacuum drying oven then, being evacuated to vacuum is 10 -2Pa is warming up to 900~1000 ℃ and be incubated 30min with the speed of 10 ℃/min, is warming up to 1120~1350 ℃ and be incubated 90min with the speed of 20 ℃/min again, reduces to room temperature with the speed of 20 ℃/min subsequently, the sintering blank; Three, the sintering blank being preheated to 850~950 ℃ and be incubated 30min, putting into mould then, is that 500~600MPa, extrusion ratio are hot extrusion 3~6s under 6~40 the condition at 300 ℃ of mold preheating temperatures, pressure; Four, the blank after the hot extrusion is placed vacuum drying oven, being evacuated to vacuum is 10 -2Pa is warming up to 600~1000 ℃ and be incubated 1~3h with the speed of 5~20 ℃/min, reduces to room temperature with the speed of 10~40 ℃/min then, promptly gets powder deformed composite material; Wherein copper powder is that Fisher particle size is that 20~100 μ m, quality purity are the electrolytic copper powder more than 99.5% in the step 1.
2, the preparation method of a kind of powder deformed composite material according to claim 1 is characterized in that in the step 1 by weight percentage 10%~30% copper powder and 70%~90% tungsten powder or molybdenum powder mechanical mixture 60h under the condition of 60r/min.
3, the preparation method of a kind of powder deformed composite material according to claim 1 is characterized in that in the step 1 by weight percentage 15%~85% copper powder and 15%~85% tungsten powder or molybdenum powder mechanical mixture 60h under the condition of 60r/min.
4, in the step 1 by weight percentage with 10% copper powder and 90% tungsten powder or molybdenum powder mechanical mixture 60h under the condition of 60r/min.
5, the preparation method of a kind of powder deformed composite material according to claim 1 is characterized in that in the step 1 by weight percentage 20% copper powder and 80% tungsten powder or molybdenum powder mechanical mixture 60h under the condition of 60r/min.
6, the preparation method of a kind of powder deformed composite material according to claim 1 is characterized in that copper powder is that Fisher particle size is 30~90 μ m in the step 1, and quality purity is 99.7% electrolytic copper powder.
7, the preparation method of a kind of powder deformed composite material according to claim 1, the Fisher particle size that it is characterized in that tungsten powder in the step 1 are 2~10 μ m, and quality purity is more than 99.5%.
8, the preparation method of a kind of powder deformed composite material according to claim 1, the Fisher particle size that it is characterized in that molybdenum powder in the step 1 are 2~10 μ m, and quality purity is more than 99.5%.
9, the preparation method of a kind of powder deformed composite material according to claim 1 is characterized in that composite powder is made the blank of colding pressing through the pressure of 550~950MPa in the step 2.
10, the preparation method of a kind of powder deformed composite material according to claim 1 is characterized in that in the step 4 that speed with 5~15 ℃/min is warming up to 700~900 ℃ and be incubated 1.5~2.5h, reduces to room temperature with the speed of 20~35 ℃/min then.
CNA2008102095424A 2008-11-27 2008-11-27 Method for preparing powder deformed composite material Pending CN101406955A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102492884A (en) * 2011-12-07 2012-06-13 北京理工大学 Preparation method of novel tungsten-copper-zinc alloy material
CN107326241A (en) * 2017-07-10 2017-11-07 四川大学 A kind of method that tungsten molybdenum copper composite material is prepared with discharge plasma sintering

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102492884A (en) * 2011-12-07 2012-06-13 北京理工大学 Preparation method of novel tungsten-copper-zinc alloy material
CN102492884B (en) * 2011-12-07 2013-06-05 北京理工大学 Preparation method of novel tungsten-copper-zinc alloy material
CN107326241A (en) * 2017-07-10 2017-11-07 四川大学 A kind of method that tungsten molybdenum copper composite material is prepared with discharge plasma sintering
CN107326241B (en) * 2017-07-10 2019-01-15 四川大学 A method of tungsten molybdenum copper composite material is prepared with discharge plasma sintering

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