CN104178657A - Nano copper-silver composite material and preparation method thereof - Google Patents
Nano copper-silver composite material and preparation method thereof Download PDFInfo
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- CN104178657A CN104178657A CN201410449326.2A CN201410449326A CN104178657A CN 104178657 A CN104178657 A CN 104178657A CN 201410449326 A CN201410449326 A CN 201410449326A CN 104178657 A CN104178657 A CN 104178657A
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Abstract
The invention relates to a nano copper-silver composite material which is composed of following components in percentage by mass: 70-90% of copper powder and 10-30% of silver powder. The particle size of the copper powder is 15-20nm, and the particle size of the silver powder is 5-10 mu m. The preparation method comprises the following steps: proportioning, evenly mixing and pressing. The yield strength of the nano copper-silver composite material is 450-530 MPa, and the elongation percentage can reach 40-50%. On the basis of the excellent comprehensive mechanical properties of the composite nano material, the preparation method solves the contradiction between strength and elongation percentage of the existing nanocrystal metal material, implements unification of high strength and high plasticity, and widens the engineering application fields of the nanocrystal metal material. The method has the advantages of low cost, high yield, simple technique and no bubbling or caking, and can well control the particle size and distribution of the material; and the prepared nanocrystal material has high density and high purity, and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of material and preparation method, particularly a kind of nanometer copper-silver matrix material and preparation method, metal nanometer material technical field.
Background technology
Nanocrystalline material refers to other crystalline material of nanosized level, because the superfine little crystal grain of nanocrystalline material makes it have the incomparable excellent properties of other material, thereby having obtained extensive attention and deep development, it has become one of the most promising material in this century.The hardness of nano crystal metal material and intensity are greater than hardness and the intensity of congruent coarse grain material, the plasticity of nanocrystalline metal can show higher plasticity and toughness under compressive stress state, but under action of pulling stress, compare with congruent coarse grained metal, its plasticity, toughness decline to a great extent, the ductility that is nano crystal metal material is lower, and unit elongation does not reach 5% conventionally, and this has also hindered the application of nano crystal metal material in engineering.How to address this problem and become the key issue that promotes Application of micron.Theoretically, can set up a kind of nano composite material, with nanometer close grain, provide the intensity that material is high, with coarse grain, improve good ductility and the toughness of material, thereby when keeping nano crystal metal material higher-strength, improve its ductility.But in actual use, metal nanometer composite material and technology of preparing are still in the research trial stage, and method, particularly nanometer copper-silver matrix material and preparation method that shortage is applicable to suitability for industrialized production still belong to blank.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of nanometer copper-silver matrix material that has good strength and plasticity concurrently is provided;
Another object of the present invention is to provide the preparation method of described nanometer copper-silver matrix material.
The alleged problem of the present invention solves by the following technical programs:
A nanometer copper-silver matrix material material, is comprised of copper powder and silver powder, and the particle diameter of described copper powder is 15-20nm, and the particle diameter of described silver powder is 5-10
, wherein the mass percent of copper powder is 70%-90%, the mass percent of silver powder is 10%-30%.
A preparation method for nanometer copper-silver matrix material, carries out according to following step:
A. according to proportional quantity, take copper powder and silver powder;
B. the copper powder of proportional quantity and silver powder are mixed;
C. the copper powder mixing, silver powder are inserted in vacuum oven, hydrogen reducing 30-40 minute under the temperature condition of 400 ℃ of temperature is then protected under argon shield environment, treats that temperature is cooled to room temperature;
D. the copper silver powder through c step process is carried out to High Temperature High Pressure compacting under the condition of the temperature of 700 ~ 800 ℃ and 5GPa pressure, obtain lumpy nanometer copper silver composite material.
The preparation method of above-mentioned nanometer copper-silver matrix material, in described d step, nanometer copper-silver matrix material pressing process is: boost 15 minutes; Pressurize 30 minutes, heats at packing stage: wherein heat up 5 minutes, be incubated 20 minutes, lower the temperature 5 minutes.
The present invention is directed to the low problem of solution nano crystal metal material unit elongation and improve, a kind of nanometer copper-silver matrix material is provided.It is raw material that described matrix material be take a certain proportion of nano level copper powder and micron order silver powder, through steps such as mixing, reduction, compactings, makes lumpy nanometer copper silver composite material.This matrix material be take nanosized copper crystal grain as matrix; micro nanometer silver uniform crystal particles is distributed on nanosized copper crystal grain matrix; by nanosized copper crystal grain, provide good intensity for described matrix material, by micro nanometer silver crystal grain, provide good unit elongation for described matrix material.After testing, the yield strength of stretching of nanometer copper-silver matrix material of the present invention is 450-530MPa, is more or less the same with the brilliant copper of receiving of same grain-size, and unit elongation can reach 40-50%, and the brilliant copper of receiving of same grain-size seldom surpasses 10%.Based on the good comprehensive mechanical property of composite nano materials of the present invention, intensity and these those long contradictions that disappear of unit elongation of existing nano crystal metal material have been broken through, realize the unification of high strength, high-ductility, high tenacity, expanded the engineering Application Areas of nano crystal metal material.The inventive method production cost is low, output is large, technique is simple, does not have pore and caking, and grain-size and distribution that can fine control material, and the nano-crystal material density of preparation is high, purity is high, is suitable for suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the XRD(X ray diffraction of embodiment 1 nanometer copper-silver matrix material) figure;
Fig. 2 is the electron-microscope scanning figure of embodiment 1 nanometer copper-silver matrix material;
Fig. 3 is the energy spectrum analysis of the EDS(X ray of Fig. 2 mid point 1) spectrogram;
Fig. 4 is the energy spectrum analysis of the EDS(X ray of Fig. 2 mid point 2) spectrogram.
Embodiment
The raw material of nanometer copper-silver matrix material of the present invention is selected from nano level copper powder and micron order silver powder, and the particle diameter of copper powder is controlled at 15-20nm, and the particle diameter of silver powder is controlled at 5-10
.Nano level copper powder size value is set and can be avoided when hot pressing, and grain growth surpasses 100 nanometers and causes the strength of materials to reduce.In raw material, the mass percent of copper powder is 70%-90%, and surplus is silver powder.Micron order silver powder adds as coarse crystal, main in order to improve the unit elongation of material, if the ratio of silver powder is too low, described matrix material unit elongation improves not obvious, with the increase of silver powder ratio, described matrix material intensity when unit elongation improves can decrease, and when silver-colored mass percent surpasses 40%, the strength of materials can obviously reduce, consider the requirement of composite material strength and plasticity, the present invention determines the mass percent of micron order silver powder at 10%-30%.
The preparation method of nanometer copper-silver matrix material of the present invention carries out according to following step:
1, according to proportional quantity, prepare nano level copper powder and micron order silver powder;
2, the copper powder of proportional quantity and silver powder are mixed, mixing process can adopt three-dimensional material mixer evenly to mix, and need guarantee, in mixing process, not mix impurity;
3, mixed copper silver powder in being set to the vacuum oven of 400 ℃, temperature setting is carried out to hydrogen reducing 30-40 minute, the cupric oxide that may contain in mixed powder is reduced, then under ar gas environment, protected, oxidized to prevent mixed powder, treat that temperature is cooled to room temperature; The operating process of this step is: first pass into nitrogen by vacuum oven the inside Bas Discharged, then pass into hydrogen and heat, to inserting mixed powder in vacuum oven, reduce, pass into argon gas protected and be cooled to room temperature after having reduced.
4, adopt six-plane piercer to carry out High Temperature High Pressure compacting under 700 ℃-800 ℃ of temperature and pressure 5GPa condition the mixed powder of processing through above-mentioned steps, pressing process: boost 15 minutes, pressurize 30 minutes, in pressure maintaining period, heat: heat up 5 minutes, be incubated 20 minutes, lower the temperature 5 minutes, then step-down is 20 minutes, is finally pressed into shape lumpy nanometer copper silver composite material.
With German Brooker X-ray diffractometer, nanometer copper-silver matrix material of the present invention is carried out to the thing identification of phases and show, matrix material of the present invention is nanocrystal bimodal material, nano level Cu and micron order Ag, consists of, and chemical reaction does not occur.
Below provide several specific embodiment of the present invention:
Embodiment 1: 70 grams of the copper powders, the particle diameter that take particle diameter and be 15-20nm are 5-10
30 grams, silver powder; Adopt three-dimensional material mixer that copper powder and silver powder are mixed; Mixed copper silver powder is carried out to hydrogen reducing 30 minutes in temperature setting is set to the vacuum oven of 400 ℃, then under ar gas environment, protected, treat that temperature is cooled to room temperature; Adopt six-plane piercer to carry out High Temperature High Pressure compacting under 750 ℃ of temperature and pressure 5GPa condition in the mixed copper silver powder of processing through above-mentioned steps, pressing process: boost 15 minutes, pressurize 30 minutes, in pressure maintaining period, heat: heat up 5 minutes, be incubated 20 minutes, lower the temperature 5 minutes, then step-down is 20 minutes, is finally pressed into shape lumpy nanometer copper silver composite material.The yield strength 460.3MPa of the present embodiment nanometer copper-silver matrix material after testing, unit elongation is 45.2%.
Referring to Fig. 1-4, Fig. 1 is the XRD(X ray diffraction of the obtained nanometer copper-silver matrix material of embodiment 1) scheme (to illustrate: X-ray diffraction spectrum is that X-ray diffractometer is with 2
the whole diffraction region of angle scanning, angle changes the X-coordinate as X-ray diffraction spectrum, ordinate zou is at different diffraction angle 2
descend to obtain diffraction peak intensity).As can be seen from Figure 1, in described nanometer copper-silver matrix material, only have copper and money kind elementary composition, after thermo compression, do not have other impurity, also do not have oxide compound to generate.Fig. 2 is the electron-microscope scanning figure of the obtained nanometer copper-silver matrix material of embodiment 1, and in figure, light areas is that silver-colored phase, darker regions are copper phase, from electron-microscope scanning figure, can find out by hot extrusion, and copper silver powder is successfully pressed into nanometer copper-silver matrix material.Fig. 3 and 4 is respectively the EDS spectrum analysis figure of the electron-microscope scanning of the prepared nanometer copper-silver matrix material of embodiment 1, can record atomic percent and the weight percent of Fig. 2 mid point 1 and point 2.Show that by analysis the weight percent at point 1 Cu of place and Ag is respectively 4.18%, 95.82%, its atomic percent is respectively 6.89%, 93.11%; Weight percent at point 2 Cu of place and Ag is respectively 94.45%, 5.55%, and its atomic percent is respectively 96.65%, 3.35%.
Embodiment 2: 80 grams of the copper powders, the particle diameter that take particle diameter and be 15-20nm are 5-10
20 grams, silver powder; Adopt three-dimensional material mixer that copper powder and silver powder are mixed; Mixed copper silver powder is carried out to hydrogen reducing 35 minutes in temperature setting is set to the vacuum oven of 400 ℃, then under ar gas environment, protected, treat that temperature is cooled to room temperature; Adopt six-plane piercer to carry out High Temperature High Pressure compacting under 700 ℃ of temperature and pressure 5GPa condition in the mixed copper silver powder of processing through above-mentioned steps, pressing process: boost 15 minutes, pressurize 30 minutes, in pressure maintaining period, heat: heat up 5 minutes, be incubated 20 minutes, lower the temperature 5 minutes, then step-down is 20 minutes, is finally pressed into shape lumpy nanometer copper silver composite material.The yield strength 481.4MPa of the present embodiment nanometer copper-silver matrix material after testing, unit elongation is 42.8%.
Embodiment 3: 90 grams of the copper powders, the particle diameter that take particle diameter and be 15-20nm are 5-10
10 grams, silver powder; Adopt three-dimensional material mixer that copper powder and silver powder are mixed; Mixed copper silver powder is carried out to hydrogen reducing 30 minutes in temperature setting is set to the vacuum oven of 400 ℃, then under ar gas environment, protected, treat that temperature is cooled to room temperature; Adopt six-plane piercer to carry out High Temperature High Pressure compacting under 750 ℃ of temperature and pressure 5GPa condition in the mixed copper silver powder of processing through above-mentioned steps, pressing process: boost 15 minutes, pressurize 30 minutes, in pressure maintaining period, heat: heat up 5 minutes, be incubated 20 minutes, lower the temperature 5 minutes, then step-down is 20 minutes, is finally pressed into shape lumpy nanometer copper silver composite material.The yield strength 506.5MPa of the present embodiment nanometer copper-silver matrix material after testing, unit elongation is 40.4%.
Embodiment 4: 70 grams of the copper powders, the particle diameter that take particle diameter and be 15-20nm are 5-10
30 grams, silver powder; Adopt three-dimensional material mixer that copper powder and silver powder are mixed; Mixed copper silver powder is carried out to hydrogen reducing 36 minutes in temperature setting is set to the vacuum oven of 400 ℃, then under ar gas environment, protected, treat that temperature is cooled to room temperature; Adopt six-plane piercer to carry out High Temperature High Pressure compacting under 800 ℃ of temperature and pressure 5GPa condition in the mixed copper silver powder of processing through above-mentioned steps, pressing process: boost 15 minutes, pressurize 30 minutes, in pressure maintaining period, heat: heat up 5 minutes, be incubated 20 minutes, lower the temperature 5 minutes, then step-down is 20 minutes, is finally pressed into shape lumpy nanometer copper silver composite material.The yield strength 471.5MPa of the present embodiment nanometer copper-silver matrix material after testing, unit elongation is 48.7%.
Embodiment 5: 80 grams of the copper powders, the particle diameter that take particle diameter and be 15-20nm are 5-10
20 grams, silver powder; Adopt three-dimensional material mixer that copper powder and silver powder are mixed; Mixed copper silver powder is carried out to hydrogen reducing 32 minutes in temperature setting is set to the vacuum oven of 400 ℃, then under ar gas environment, protected, treat that temperature is cooled to room temperature; Adopt six-plane piercer to carry out High Temperature High Pressure compacting under 750 ℃ of temperature and pressure 5GPa condition in the mixed copper silver powder of processing through above-mentioned steps, pressing process: boost 15 minutes, pressurize 30 minutes, in pressure maintaining period, heat: heat up 5 minutes, be incubated 20 minutes, lower the temperature 5 minutes, then step-down is 20 minutes, is finally pressed into shape lumpy nanometer copper silver composite material.The yield strength 485.2MPa of the present embodiment nanometer copper-silver matrix material after testing, unit elongation is 43.5%.
Embodiment 6: 90 grams of the copper powders, the particle diameter that take particle diameter and be 15-20nm are 5-10
10 grams, silver powder; Adopt three-dimensional material mixer that copper powder and silver powder are mixed; Mixed copper silver powder is carried out to hydrogen reducing 40 minutes in temperature setting is set to the vacuum oven of 400 ℃, then under ar gas environment, protected, treat that temperature is cooled to room temperature; Adopt six-plane piercer to carry out High Temperature High Pressure compacting under 800 ℃ of temperature and pressure 5GPa condition in the mixed copper silver powder of processing through above-mentioned steps, pressing process: boost 15 minutes, pressurize 30 minutes, in pressure maintaining period, heat: heat up 5 minutes, be incubated 20 minutes, lower the temperature 5 minutes, then step-down is 20 minutes, is finally pressed into shape lumpy nanometer copper silver composite material.The yield strength 515MPa of the present embodiment nanometer copper-silver matrix material after testing, unit elongation is 40.8%.
From the detected result of above-described embodiment, can find out, nanometer copper-silver matrix material of the present invention has possessed high strength and good ductility simultaneously, has changed the shortcoming of nano crystal metal material high strength inductile, toughness.Coarse-grain silver plays the effect that improves matrix material unit elongation, and thin brilliant copper plays the effect that improves matrix material yield strength, and along with the minimizing of the increasing of coarse-grain silver, thin brilliant copper, the intensity of described matrix material decreases, and unit elongation increases to some extent.Under the condition of same proportioning, with the rising of press temperature, the intensity of described matrix material presents increase trend, but press temperature impact is little.
Claims (3)
1. a nanometer copper-silver matrix material, is characterized in that: it is comprised of copper powder and silver powder, and the particle diameter of described copper powder is 15-20nm, and the particle diameter of described silver powder is 5-10
, wherein the mass percent of copper powder is 70%-90%, the mass percent of silver powder is 10%-30%.
2. a preparation method for nanometer copper-silver matrix material, is characterized in that: according to following step, carry out:
A. according to proportional quantity, take copper powder and silver powder;
B. the copper powder of proportional quantity and silver powder are mixed;
C. the copper powder mixing, silver powder are inserted in vacuum oven, hydrogen reducing 30-40 minute under the temperature condition of 400 ℃ of temperature is then protected under argon shield environment, treats that temperature is cooled to room temperature;
D. the copper silver powder through c step process is carried out to High Temperature High Pressure compacting under the condition of the temperature of 700 ~ 800 ℃ and 5GPa pressure, obtain lumpy nanometer copper silver composite material.
3. according to the preparation method of the nanometer copper-silver matrix material described in claim 2, it is characterized in that: in described d step, nanometer copper-silver matrix material pressing process is: boost 15 minutes; Pressurize 30 minutes, heats at packing stage: wherein heat up 5 minutes, be incubated 20 minutes, lower the temperature 5 minutes.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104741615A (en) * | 2015-04-08 | 2015-07-01 | 华北电力大学（保定） | Super-fine grain twin-peak copper preparing method |
| CN111101008A (en) * | 2019-12-26 | 2020-05-05 | 浙江杭机新型合金材料有限公司 | High-strength high-conductivity copper-silver alloy material and preparation method thereof |
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| CN102383014A (en) * | 2011-11-11 | 2012-03-21 | 华中科技大学 | Method for preparing diamond-copper composite material by virtue of metallization of high-temperature blending surface |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102383014A (en) * | 2011-11-11 | 2012-03-21 | 华中科技大学 | Method for preparing diamond-copper composite material by virtue of metallization of high-temperature blending surface |
Non-Patent Citations (2)
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| FANG FANG ET AL: "Mechanical Alloying of Ag-Cu Immiscible Alloy System", 《JOURNAL OF SHANG HAI JIAO TONG UNIVERSITY (SCIENCE)》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104741615A (en) * | 2015-04-08 | 2015-07-01 | 华北电力大学（保定） | Super-fine grain twin-peak copper preparing method |
| CN111101008A (en) * | 2019-12-26 | 2020-05-05 | 浙江杭机新型合金材料有限公司 | High-strength high-conductivity copper-silver alloy material and preparation method thereof |
| CN111101008B (en) * | 2019-12-26 | 2021-08-17 | 浙江杭机新型合金材料有限公司 | High-strength high-conductivity copper-silver alloy material and preparation method thereof |
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Application publication date: 20141203 |