CN112359245A - Nanocluster reinforced copper-based composite material and preparation method thereof - Google Patents

Nanocluster reinforced copper-based composite material and preparation method thereof Download PDF

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Publication number
CN112359245A
CN112359245A CN202011246367.3A CN202011246367A CN112359245A CN 112359245 A CN112359245 A CN 112359245A CN 202011246367 A CN202011246367 A CN 202011246367A CN 112359245 A CN112359245 A CN 112359245A
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composite material
based composite
cuo
reinforced copper
furnace
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刘佳
刘继拓
付翀
王彦龙
燕阳天
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Xian Polytechnic University
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Xian Polytechnic University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a nanocluster reinforced copper-based composite material which comprises Cu, CuO, Ti and YH2The four components comprise, by mass, 95-97.5 wt% of Cu, 1-1.5 wt% of CuO, 1-1.5 wt% of Ti and YH20.5-2 wt%, the sum of the mass percent of the components is 100%, the invention also discloses a preparation method of the nanocluster reinforced copper-based composite material, which comprises the steps of firstly, mixing Cu with the purity of more than 99.9%, CuO with the purity of more than 99.99%, Ti with the purity of more than 99.99% and YH with the purity of more than 99.99%2Weighing, ball milling, sintering and agingAnd (6) processing. The invention solves the problem that the contradiction between high strength and high conductivity of the copper alloy is increased and decreased in the prior art.

Description

Nanocluster reinforced copper-based composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of metal matrix composite materials, and particularly relates to a nanocluster reinforced copper matrix composite material and a preparation method of the nanocluster reinforced copper matrix composite material.
Background
The high-strength high-conductivity copper-based material has high strength and good plasticity, high conductivity and good heat conductivity, is an indispensable novel structural functional material in advanced technical fields of aviation, aerospace, 5G communication, high-speed rail and the like, becomes a core component of an integrated circuit lead frame, a rotor lead of a large-scale high-speed turbine generator, an electric locomotive contact wire and the like, and provides higher requirements for the comprehensive performance of the high-strength high-conductivity copper-based material. However, the existing high-strength and high-conductivity copper-based material can not overcome the contradiction between high strength and high conductivity, and the high-temperature stress relaxation resistance of the alloy is not obviously improved, so that the development of a novel copper-based material with both high strength and high conductivity is significant.
Disclosure of Invention
The invention aims to provide a nanocluster reinforced copper-based composite material, which solves the problem of contradiction between high strength and high conductivity of a copper alloy in the prior art.
The first technical scheme adopted by the invention is that the nanocluster reinforced copper-based composite material comprises Cu, CuO, Ti and YH2The four components comprise, by mass, 95-97.5 wt% of Cu, 1-1.5 wt% of CuO1, 1-1.5 wt% of Ti and YH20.5-2 wt%, and the sum of the mass percentages of the components is 100%.
The second technical scheme adopted by the invention is that the preparation method of the nanocluster reinforced copper-based composite material is implemented according to the following steps:
step 1, raw material proportioning:
cu with the purity of more than 99.9 percent, CuO with the purity of more than 99.99 percent, Ti with the purity of more than 99.99 percent and YH with the purity of more than 99.99 percent2Weighing the following components in percentage by mass:
Cu：95-97.5％；
CuO：1-1.5wt％；
Ti：1-1.5wt％；
YH2：0.5-2wt％；
step 2, high-energy ball milling:
CuO, Ti and YH weighed in the step 12Ball-milling in a high-energy ball mill, wherein a process control agent is absolute ethyl alcohol or stearic acid, and mixing the ball-milled composite powder with the Cu powder weighed in the step 1 to obtain uniformly-mixed powder;
and step 3, sintering:
sintering the uniformly mixed powder in a spark plasma sintering furnace, raising the furnace temperature, then preserving the heat, keeping constant pressure during the period, and cooling along with the furnace after the heat preservation is finished;
step 4, aging treatment:
and (3) preserving heat in an open type vacuum-atmosphere tubular furnace, wherein the protective atmosphere is Ar gas, and the cooling mode is furnace cooling.
The second technical aspect of the present invention is also characterized in that,
and in the step 2, the rotation speed of the high-energy ball mill is 300-500 rpm.
And (3) controlling the time of the high-energy ball milling in the step (2) to be 2-8 h.
And in the step 2, the material mixing time is controlled to be 20-60 min.
In step 2, the process control agent is mixed with CuO, Ti and YH2The mass ratio of the total powder is 1: 5000-10000.
And 3, raising the temperature of the furnace to 700-850 ℃, and then preserving the heat for 10-15 min.
And 3, keeping the pressure in the sintering furnace at 30-35 MPa.
And 4, controlling the heat preservation temperature to be 300-600 ℃.
And 4, keeping the temperature for 1-8 h.
The invention has the beneficial effects that the nanocluster reinforced copper-based composite material and the preparation method thereof can form nanoclusters in composite powder by a simple powder metallurgy method, the nanoclusters are uniformly distributed in a composite material matrix after sintering treatment, the alloy is reinforced, the nanoclusters have little influence on the conductivity of the composite material, and the novel high-strength high-conductivity copper-based composite material can be prepared.
Drawings
Fig. 1 is a flow chart of a preparation method of a nanocluster reinforced copper-based composite material of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a nanocluster reinforced copper-based composite material which comprises Cu, CuO, Ti and YH2The four components comprise, by mass, 95-97.5 wt% of Cu, 1-1.5 wt% of CuO, 1-1.5 wt% of Ti and YH20.5-2 wt%, and the sum of the mass percentages of the components is 100%.
The invention discloses a preparation method of a nanocluster reinforced copper-based composite material, which is shown in a flow chart of figure 1 and is specifically implemented according to the following steps:
step 1, raw material proportioning:
cu with the purity of more than 99.9 percent, CuO with the purity of more than 99.99 percent, Ti with the purity of more than 99.99 percent and YH with the purity of more than 99.99 percent2Weighing the following components in percentage by mass:
Cu：95-97.5％；
CuO：1-1.5wt％；
Ti：1-1.5wt％；
YH2：0.5-2wt％；
step 2, high-energy ball milling:
CuO, Ti and YH weighed in the step 12Ball-milling in a high-energy ball mill, wherein a process control agent is absolute ethyl alcohol or stearic acid, and mixing the ball-milled composite powder with the Cu powder weighed in the step 1 to obtain uniformly-mixed powder;
and step 3, sintering:
sintering the uniformly mixed powder in a spark plasma sintering furnace, raising the furnace temperature, then preserving the heat, keeping constant pressure during the period, and cooling along with the furnace after the heat preservation is finished;
step 4, aging treatment:
and (3) preserving heat in an open type vacuum-atmosphere tubular furnace, wherein the protective atmosphere is Ar gas, and the cooling mode is furnace cooling.
Wherein, the rotation speed of the high-energy ball mill in the step 2 is 300-500 rpm.
And (3) controlling the time of the high-energy ball milling in the step (2) to be 2-8 h.
And in the step 2, the material mixing time is controlled to be 20-60 min.
In step 2, the process control agent is mixed with CuO, Ti and YH2The mass ratio of the total powder is 1: 5000-10000.
And 3, raising the temperature of the furnace to 700-850 ℃, and then preserving the heat for 10-15 min.
And 4, controlling the heat preservation temperature to be 300-600 ℃.
And 4, keeping the temperature for 1-8 h.
Example 1
Cu with the purity of more than 99.9 percent, CuO with the purity of more than 99.9 percent, Ti with the purity of more than 99.99 percent and YH with the purity of more than 99.99 percent2Weighing according to a certain mass ratio, wherein the components are as follows: cu: 95 percent; CuO: 1.5 wt%; ti: 1.5 wt%; YH2: 2 wt%. Will call CuO, Ti and YH2Ball milling is carried out in a high-energy ball mill at the rotating speed of 300rpm for 8h, the process control agent is absolute ethyl alcohol, and the ball-milled composite powder and Cu powder are mixed at the rotating speed of 100rpm for 20min to obtain uniformly mixed powder. Sintering the uniformly mixed powder in a discharge plasma sintering furnace, keeping the temperature for 15min after the furnace temperature is increased to 700 ℃, keeping the constant pressure at 30MPa, cooling along with the furnace after the temperature is kept, and finally keeping the temperature for 1h in an open type vacuum-atmosphere tubular furnace at 600 ℃, wherein the protective atmosphere is Ar gas, and the cooling mode is along with the furnace cooling. Thus obtaining the high-strength high-conductivity copper-based composite material. The alloy was tested to have a tensile strength, electrical conductivity and hardness of 570MPa, 48% IACS and 260HV, respectively.
Example 2
Cu with purity of more than 99.9 percent, CuO with purity of 99.99 percent, Ti with purity of 99.99 percent and YH with purity of 99.99 percent2Weighing according to a certain mass ratio, wherein the components are as follows: cu: 96 percent; CuO: 1.5wt％；Ti：1.5wt％；YH2: 1 wt%. Will call CuO, Ti and YH2Ball milling is carried out in a high-energy ball mill at the rotating speed of 400rpm for 5h, the process control agent is absolute ethyl alcohol, and the ball-milled composite powder and Cu powder are mixed at the rotating speed of 100rpm for 40min to obtain uniformly mixed powder. Sintering the uniformly mixed powder in a discharge plasma sintering furnace, keeping the temperature for 12min after the furnace temperature is increased to 800 ℃, keeping the constant pressure at 32MPa, cooling along with the furnace after the temperature is kept, and finally keeping the temperature for 8h in an open type vacuum-atmosphere tubular furnace at 300 ℃, wherein the protective atmosphere is Ar gas, and the cooling mode is along with the furnace cooling. Thus obtaining the high-strength high-conductivity copper-based composite material. The alloy was tested to have a tensile strength, electrical conductivity and hardness of 570MPa, 48% IACS and 260HV, respectively.
Example 3
Cu with purity of more than 99.9 percent, CuO with purity of 99.99 percent, Ti with purity of 99.99 percent and YH with purity of 99.99 percent2Weighing according to a certain mass ratio, wherein the components are as follows: cu: 97.5 percent; CuO: 1 wt%; ti: 1 wt%; YH2: 0.5 wt%. Will call CuO, Ti and YH2Ball milling is carried out in a high-energy ball mill at the rotating speed of 500rpm for 2h, the process control agent is absolute ethyl alcohol, and the ball-milled composite powder and Cu powder are mixed at the rotating speed of 100rpm for 60min to obtain uniformly mixed powder. Sintering the uniformly mixed powder in a discharge plasma sintering furnace, keeping the temperature for 10min after the furnace temperature is increased to 850 ℃, keeping the constant pressure at 35MPa, cooling along with the furnace after the temperature is kept, and finally keeping the temperature for 4h in an open type vacuum-atmosphere tubular furnace at 450 ℃, wherein the protective atmosphere is Ar gas, and the cooling mode is along with the furnace cooling. Thus obtaining the high-strength high-conductivity copper-based composite material. The tensile strength, the electric conductivity and the hardness of the alloy are respectively 580MPa, 52 percent IACS and 290HV after being tested.
The examples and copper alloy performance parameters are shown in Table 1
TABLE 1 comparison of examples with copper alloy Performance parameters
Sample name Tensile strength/MPa hardness/HV Conductivity/% IACS
Example 1 550 280 45
Example 2 570 260 48
Example 3 580 290 52
Copper alloy 560 280 16
It is apparent from examples 1 to 3 that the nanocluster reinforced copper-based composite material prepared by the method of the present invention has superior comprehensive properties compared with a certain copper alloy, and solves the contradiction between high strength and high conductivity of the copper alloy.

Claims (10)

1. A nanocluster reinforced copper-based composite material is characterized in that,including Cu, CuO, Ti and YH2The four components comprise, by mass, 95-97.5 wt% of Cu, 1-1.5 wt% of CuO, 1-1.5 wt% of Ti and YH20.5-2 wt%, and the sum of the mass percentages of the components is 100%.
2. The preparation method of the nanocluster reinforced copper-based composite material is characterized by comprising the following steps:
step 1, raw material proportioning:
cu with the purity of more than 99.9 percent, CuO with the purity of more than 99.99 percent, Ti with the purity of more than 99.99 percent and YH with the purity of more than 99.99 percent2Weighing the following components in percentage by mass:
Cu：95-97.5％；
CuO：1-1.5wt％；
Ti：1-1.5wt％；
YH2：0.5-2wt％；
step 2, high-energy ball milling:
CuO, Ti and YH weighed in the step 12Ball-milling in a high-energy ball mill, wherein a process control agent is absolute ethyl alcohol or stearic acid, and mixing the ball-milled composite powder with the Cu powder weighed in the step 1 to obtain uniformly-mixed powder;
and step 3, sintering:
sintering the uniformly mixed powder in a spark plasma sintering furnace, raising the furnace temperature, then preserving the heat, keeping constant pressure during the period, and cooling along with the furnace after the heat preservation is finished;
step 4, aging treatment:
and (3) preserving heat in an open type vacuum-atmosphere tubular furnace, wherein the protective atmosphere is Ar gas, and the cooling mode is furnace cooling.
3. The method for preparing a nanocluster reinforced copper-based composite material according to claim 2, wherein the high energy ball milling speed in the step 2 is 300-500 rpm.
4. The method for preparing a nanocluster reinforced copper-based composite material according to claim 2, wherein the time for high energy ball milling in the step 2 is controlled to be 2-8 hours.
5. The method for preparing a nanocluster reinforced copper-based composite material according to claim 2, wherein the material mixing time in the step 2 is controlled to be 20-60 min.
6. The method as claimed in claim 2, wherein the process control agent is mixed with CuO, Ti, YH in the step 22The mass ratio of the total powder is 1: 5000-10000.
7. The method for preparing a nanocluster reinforced copper-based composite material according to claim 2, wherein the temperature of the furnace in the step 3 is increased to 700-850 ℃, and then the temperature is kept for 10-15 min.
8. The method for preparing a nanocluster reinforced copper-based composite material according to claim 2, wherein in the step 3, the pressure in a sintering furnace is kept at 30-35 MPa.
9. The method for preparing a nanocluster reinforced copper-based composite material according to claim 2, wherein the temperature in the step 4 is controlled to be 300-600 ℃.
10. The method for preparing a nanocluster reinforced copper-based composite material according to claim 2, wherein the temperature preservation time in the step 4 is 1-8 hours.
CN202011246367.3A 2020-11-10 2020-11-10 Nanocluster reinforced copper-based composite material and preparation method thereof Pending CN112359245A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2015005576A (en) * 2013-06-19 2015-01-08 田中電子工業株式会社 Cross-section structure of pure-copper alloy wire for ultrasonic bonding
CN108559866A (en) * 2018-05-15 2018-09-21 西安理工大学 A kind of high-strength high-conductivity Cu-Ti alloys and preparation method thereof
CN110331325A (en) * 2019-07-19 2019-10-15 西安理工大学 A kind of nano-alumina reinforcing copper-based composite and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2015005576A (en) * 2013-06-19 2015-01-08 田中電子工業株式会社 Cross-section structure of pure-copper alloy wire for ultrasonic bonding
CN108559866A (en) * 2018-05-15 2018-09-21 西安理工大学 A kind of high-strength high-conductivity Cu-Ti alloys and preparation method thereof
CN110331325A (en) * 2019-07-19 2019-10-15 西安理工大学 A kind of nano-alumina reinforcing copper-based composite and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
张克立 等: "《无机合成化学（第二版）》", 31 January 2012, 武汉大学出版社 *
朱秀秀: "《纳米氧化物弥散强化Cu-3Ti合金的制备及组织性能研究》", 《中国优秀硕士论文工程科技1辑》 *

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Application publication date: 20210212