CN101613816A - Multiple dispersion strengthening copper-base composite material prepared in situ and preparation method thereof - Google Patents

Multiple dispersion strengthening copper-base composite material prepared in situ and preparation method thereof Download PDF

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Publication number
CN101613816A
CN101613816A CN200910055061A CN200910055061A CN101613816A CN 101613816 A CN101613816 A CN 101613816A CN 200910055061 A CN200910055061 A CN 200910055061A CN 200910055061 A CN200910055061 A CN 200910055061A CN 101613816 A CN101613816 A CN 101613816A
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powder
situ
prepared
base composite
dispersion strengthening
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甘可可
祁更新
陈晓
陈乐生
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Wenzhou Hongfeng Electrical Alloy Co Ltd
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Wenzhou Hongfeng Electrical Alloy Co Ltd
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Abstract

The present invention discloses a kind of multiple dispersion strengthening copper-base composite material prepared in situ and preparation method thereof, its wild phase comprises at least three kinds in the following material: 0.3%≤titanium carbide≤5%, 0.3%≤zirconium carbide≤5%, 0.3%≤aluminum oxide≤5%, 0.3%≤titanium boride≤5%, 0.1%≤aluminium carbide≤5%, 0.3%≤chromic oxide≤5%, 0.3%≤zirconium white≤5%, 0.1%≤graphite≤1%; Surplus is Cu.The granularity of wild phase material is respectively between 10nm-10 μ m.The preparation method adopts ball milling, compacting, sintering, extrusion process, in technological process processing parameter is carried out suitable optimal control to obtain polynary disperse enhanced Cu-base composites.Owing to adopt in-situ authigenic to become technology and in conjunction with the method for various reinforced phase, compare with the traditional ceramics granule reinforced copper base composite material, material of the present invention has higher hot strength, better conductivity and creep-resistant property.

Description

Multiple dispersion strengthening copper-base composite material prepared in situ and preparation method thereof
Technical field
The present invention relates to a kind of metal-base composites and preparation method thereof, be specially a kind of multiple dispersion strengthening copper-base composite material prepared in situ and preparation method thereof.
Background technology
Copper is owing to have high conduction, heat conductivility, good processing properties and cheap price, thereby be widely used in fields such as comprising navigation, aviation, electronics, for example electrical contact, brush, the friction materials of cooling component, electronic component, electrode, low-speed heave-load initiatively.But, limited its widespread use because fine copper metal strength and hardness are on the low side.Ceramic particle strengthens Cu-base composites, for example Cu-Al 2O 3, Cu-TiB 2In matrix material, when taking into account copper matrix excellent heat conductivity conductivity, can promote the hardness and the intensity of copper matrix greatly.The research to ceramic particle enhancing Cu-base composites abroad enters the practical stage in the 1950's, and can carry out suitability for industrialized production the seventies.KLF-1, MF202 dispersion strengthening copper alloy that Japanese Matsushita Electric Industrial is produced, the Cu-Al that German SIEMENS company, Korea S LKENG produce 2O 3Had considerable scale, and formulated relevant industry standard.Because this series products is classified patented product abroad as, production technology is in confidential state.
China starts late for the research that original position generates dispersion strengthening copper alloy, and 20 worlds begin project verification the seventies, and the end of the eighties is in succession relevant for the report of this type of material.To the mid-90, units such as Beijing Non-Ferrous Metal Research General Academy adopt means such as rapid solidification and isostatic cool pressing to carry out the research and development of this type of material.But because this type of material structure lack of homogeneity, density is not high, complicated process of preparation, and reasons such as production cost height, domestic unit fails large-scale production always; Therefore, every performance of this type of material all awaits further raising.
At present the major technique means of domestic production produced in situ dispersion strengthening copper alloy have: powder mixing machine method, chemical coprecipitation, mechanical alloying method, powder internal oxidation, sol-gel method prepare powdered alloy, finally obtain product by compacting, sintering, extruding, drawing, technology such as rolling again.Specific as follows:
(1) the composite electroforming preparing process CN1683601A of nano aluminium oxide particle reinforced copper base matrix material
(2) multiphase oxide particles enhanced copper-base composite material and preparation method thereof CN101168806A
(3) the preparation method CN1710124A of reactive hot-press in-situ autogenesis copper-base composite material
(4) a kind of chromic oxide and chromium dispersed and strengthened copper-based composite material and preparation method thereof CN1936056A
(5) a kind of in-situ produced titanium carbide dispersion strengthening copper based composite material and preparation method thereof CN1804077A
Adopt the method for nano alumina particles and the electroforming of copper common deposited to prepare the nano-copper base material in the document 1, can realize the good combination of nano particle and copper matrix, but material density is not enough, and wild phase is assembled thick, can not obtain the material of good mechanical property.Document 2 adopts the alloy reaction-injection moulding, and the method for oxidation obtains Cu-Al then 2O 3-La 2O 3Matrix material, its advantage can directly obtain the product of desired shape, and shortcoming is an apparatus expensive, and it is single to obtain disperse wild phase kind, can only obtain oxide compound and strengthen copper-based material.Document 3 adopts high-energy ball milling+hot-press method to prepare TiB enhancing copper-based material, and its advantage is easy to operate, and technology controlling and process is simple.Shortcoming is that hot-press equipment is not suitable for large-scale production, the production cost height, and wild phase is single.Document 4 adopts inner oxidation method, obtains Cr 2O 3The particle enhanced copper sill.Its advantage is to obtain higher electric conductivity, but its mechanical property is undesirable, and the wild phase kind is single.Document 5 adopts tin titanium carbide decomposition acquisition TiC enhancing copper-based material in mechanical milling process, and its advantage is simple to operate, and is easy to prepare, and shortcoming is that the starting material source is expensive, and electric conductivity is lower, and disperse phase forms difficulty.In sum, existing domestic material exists with production technique: (1) dispersion-strengthened is mutually thick, and the strengthening phase kind is single; (2) dispersion-strengthened forms difficulty mutually, the material property instability; (3) material preparation process technical sophistication, the difficult control of quality product, production cost is higher.Above factor causes original position to generate disperse strengthening the Cu-base composites over-all properties and have big gap with comparing abroad, and serious dependence on import is used in mass-producing.
Summary of the invention
The present invention is directed to deficiency and defective that above-mentioned prior art exists, a kind of multiple dispersion strengthening copper-base composite material prepared in situ and preparation method thereof is provided, the main method that adopts high-energy ball milling, in the high energy knockout process, generate the tiny polynary wild phase of disperse by various different element generation unbalance response original positions, solved the problem that the disperse phase kind is single, particle is thick, product has good mechanical performance and conductivity, and preparation technology is simple, and operation is with low cost easily.
For realizing above-mentioned purpose, the technical solution used in the present invention is:
The invention provides a kind of multiple dispersion strengthening copper-base composite material prepared in situ, its component comprises Cu and wild phase, and wherein wild phase is at least three kinds (weight percents) in the following material: 0.3%≤titanium carbide (TiC)≤5%, 0.3%≤zirconium carbide (ZrC)≤5%, 0.3%≤aluminum oxide (Al 2O 3)≤5%, 0.3%≤titanium boride (TiB 2)≤5%, 0.1%≤aluminium carbide (Al 4C 3)≤5%, 0.3%≤chromic oxide (Cr 2O 3)≤5%, 0.3%≤zirconium white (ZrO)≤5%, 0.1%≤graphite≤1%; Surplus is Cu.
Described titanium carbide, zirconium carbide, aluminum oxide, graphite, titanium boride, aluminium carbide, chromic oxide, zirconic mean particle size are respectively between 10nm-10 μ m.
The present invention also provides the preparation method of above-mentioned multiple dispersion strengthening copper-base composite material prepared in situ, may further comprise the steps:
The first step is at first with at least two kinds of powder in Cu powder and Ti powder, Zr powder, Al powder, the Cr powder and Graphite Powder 99, B powder, Cu 2At least a powder in the O powder is mixed in proportion ball milling;
Described ball milling, wherein ratio of grinding media to material is between 10: 1~100: 1, and the ball milling time, rotational speed of ball-mill was at 200~800 rev/mins between 2h~200h; Milling atmosphere is an inert atmosphere.
Second the step, with powder behind the ball milling in the hydrogen atmosphere anneal;
Described anneal is meant at 200~600 ℃ of annealing 0.5-10h.
In the 3rd step, wait under the static pressure powder compression after the three-step annealing processing is become blank;
The described static pressure that waits, wherein pressure is 100MPa~500MPa.
In the 4th step, the blank to compression moulding in high temperature sintering furnace carries out sintering;
Described sintering, wherein sintering temperature is 750~1000 ℃, sintering time is 1~10h, hydrogen atmosphere or inert atmosphere protection.
In the 5th step, the blank behind the sintering is carried out hot pressing;
Described hot pressing, wherein hot pressing temperature is 500~1000 ℃, and hot pressing pressure is between 100~800MPa, and the hot pressing soaking time is 5~60min.
The 6th step, the base substrate after the hot pressing is carried out resintering, processing parameter is with the 5th step;
Described resintering, wherein sintering temperature is 750~1000 ℃, sintering time is 1~10h, hydrogen atmosphere or inert atmosphere protection.
In the 7th step, the base substrate behind the resintering is carried out hot extrusion.
Described hot extrusion is to carry out on hydropress.
Described hot extrusion, wherein blank heating temperature is at 300~900 ℃, 200~700 ℃ of extrusion mould preheating temperatures, extrusion speed is 5~12cm/min, extrusion ratio is 10~400.
The present invention adopts in-situ authigenic to become technology, produces above-mentioned wild phase by the high-energy ball milling mode.In the high-energy ball milling process because huge energy impact, can be so that under proper technical conditions, produce reaction between each element, this type of reaction in is as follows:
Ti+C=TiC?Zr+C=ZrC?Ti+2B=TiB 2?4Al+3C=Al 4C 3
Al+Cu 2O=Al 2O 3+Cu?2Cr+3Cu 2O=Cr 2O 3+6Cu?Zr+O 2=ZrO 2
Simultaneously because the existence of C element, the C element will with the unnecessary O in the ball milling environment 2Realization response, thereby the stability of assurance ball milling environment, this will help the stable of explained hereafter and product performance.The C element has in material and is beneficial to the raising that increases the material antifriction performance, the work-ing life that helps to improve material simultaneously.
The polynary disperse that the present invention prepares strengthens Cu-base composites, has disperse distribution crystal grain tiny desirable weave construction, excellent mechanical property and conductive performance, and wild phase generates easily, advantages such as stable processing technique.Adopt the prepared material wear ability of the present invention obviously to be better than the C18150 copper zirconium alloy, recrystallization temperature is 650~900 ℃, and tensile strength reaches 500~750MPa, and electric conductivity is between 70~90%IACS.
Description of drawings
Fig. 1 is the schema of preparation method in the embodiment of the invention
Embodiment
Below in conjunction with accompanying drawing technical scheme of the present invention is further described, below description just is used to understand the present invention, and is not used in the scope of the present invention that limits.
As shown in Figure 1, the preparation method in following examples of the present invention implements according to the flow process shown in Fig. 1.Unspecified all can the employing has the proven technique realization now in following examples.
Embodiment one
With preparation Cu-0.3TiC-0.3TiB 2-0.3ZrC multi-element Cu-base matrix material is an example
1, at first with 99.2wt%Cu powder, 0.2wt%Ti powder, 0.2wt%Zr, 0.1wt%B and 0.3wt%C mixing and ball milling 50h, ratio of grinding media to material is 30: 1, and rotational speed of ball-mill is 500 rev/mins, and milling atmosphere is an argon gas;
2, then that ball milling is good powder is at 400 ℃ of following hydrogen annealing 3h;
3, be to be pressed into base substrate under the 200MPa with the powder after the anneal waiting static pressure then;
4, with pressed compact 900 ℃ of sintering 5h under hydrogen atmosphere;
5, subsequently sintered compact is carried out hot pressing, hot pressing temperature is 800 ℃, and hot pressing pressure is 400MPa, pressurize 10 minutes;
6, then according to original sintering process resintering once with base substrate after the hot pressing; Processing parameter is with the 5th step;
7, again the base substrate behind the resintering is hot extruded into wire rod or sheet material on hydropress, extrusion temperature is 650 ℃, and hot extrusion speed is 5cm/min, and mold preheating temperature is 350 ℃, and extrusion ratio is 200.To push back bar or sheet material at last and make the finished product through after the deformation process.
The implementation result of present embodiment: tensile strength: 550MPa; Recrystallization temperature: 650 ℃; Electric conductivity 90%IACS.
Embodiment two
With preparation Cu-1Al 2O 3-0.5ZrC-0.3ZrO 2The multi-element Cu-base matrix material is an example
1, at first with 96.4wt%Cu powder, 0.8wt%Al powder, 0.1wt%Zr, 0.5wt%C, 1.3wt%Cu 2O mixing and ball milling 100h, ratio of grinding media to material is 50: 1, and rotational speed of ball-mill is 600 rev/mins, and milling atmosphere is an argon gas;
2, then that ball milling is good powder is at 400 ℃ of following hydrogen annealing 3h;
3, be to be pressed into base substrate under the 400MPa with the powder after the anneal waiting static pressure then;
4, with pressed compact 900 ℃ of sintering 5h under hydrogen atmosphere;
5, subsequently sintered compact is carried out hot pressing, hot pressing temperature is 850 ℃, and hot pressing pressure is 300MPa, pressurize 10 minutes;
6, then according to original sintering process resintering once with base substrate after the hot pressing; Processing parameter is with the 5th step;
7, again the base substrate behind the resintering is hot extruded into bar or sheet material on hydropress, extrusion temperature is 750 ℃, and hot extrusion speed is 5cm/min, and mold preheating temperature is 350 ℃, and extrusion ratio is 240.To push back wire rod or sheet material at last and make the finished product through after the deformation process.
The implementation result of present embodiment: tensile strength: 650MPa; Recrystallization temperature: 900 ℃; Electric conductivity 88%IACS.
Embodiment three
With preparation Cu-3TiC-1TiB-0.3ZrC multi-element Cu-base matrix material is example
1, at first with 95wt%Cu powder, 2.0wt%Ti powder, 1.5wt%Zr, 0.5wt%B and 1.0wt%C mixing and ball milling 75h, ratio of grinding media to material is 80: 1, and rotational speed of ball-mill is 400 rev/mins, and milling atmosphere is an argon gas;
2, then that ball milling is good powder is at 400 ℃ of following hydrogen annealing 3h;
3, be to be pressed into base substrate under the 400MPa with the powder after the anneal waiting static pressure then;
4, with pressed compact 900 ℃ of sintering 8h under hydrogen atmosphere;
5, subsequently sintered compact is carried out hot pressing, hot pressing temperature is 850 ℃, and hot pressing pressure is 600MPa, pressurize 10 minutes;
6, then according to original sintering process resintering once with base substrate after the hot pressing; Processing parameter is with the 5th step;
7, again the base substrate behind the resintering is hot extruded into bar or sheet material on hydropress, extrusion temperature is 650 ℃, and hot extrusion speed is 6cm/min, and mold preheating temperature is 450 ℃, and extrusion ratio is 100.To push back bar or sheet material at last and make the finished product through after the deformation process.
The implementation result of present embodiment: tensile strength: 750MPa; Recrystallization temperature: 860 ℃; Electric conductivity 75%IACS.
Embodiment four
With preparation Cu-5Al 2O 3-0.5Cr 2O 3-0.1Al 4C 3-0.1C multi-element Cu-base matrix material is an example
1, at first with 91.4wt%Cu powder, 3wt%Al powder, 0.3wt%Cr powder, 5wt%Cu 2O powder, 0.3wt%C powder mixing and ball milling 80h, ratio of grinding media to material is 60: 1, and rotational speed of ball-mill is 700 rev/mins, and milling atmosphere is an argon gas;
2, then that ball milling is good powder is at 400 ℃ of following hydrogen annealing 3h;
3, be to be pressed into base substrate under the 250MPa with the powder after the anneal waiting static pressure then;
4, with pressed compact 850 ℃ of sintering 8h under hydrogen atmosphere;
5, subsequently sintered compact is carried out hot pressing, hot pressing temperature is 850 ℃, and hot pressing pressure is 600MPa, pressurize 10 minutes;
6, then according to original sintering process resintering once with base substrate after the hot pressing; Processing parameter is with the 5th step;
7, again the base substrate behind the resintering is hot extruded into wire rod or sheet material, extrusion temperature is 700 ℃, and hot extrusion speed is 5cm/min, and mold preheating temperature is 450 ℃, and extrusion ratio is 220.To push back wire rod or sheet material at last and make the finished product through after the deformation process.
The implementation result of present embodiment: tensile strength: 750MPa; Recrystallization temperature: 850 ℃; Electric conductivity 80%IACS.
Embodiment five
With preparation Cu-5TiC-0.5ZrC-1TiB 2The multi-element Cu-base matrix material is an example
1, at first with 95wt%Cu powder, 3.5wt%Ti powder, 0.3wt%Zr powder, 1.2wt%C powder, 1wt%B powder mixing and ball milling 120h, ratio of grinding media to material is 45: 1, and rotational speed of ball-mill is 350 rev/mins, and milling atmosphere is an argon gas;
2, then that ball milling is good powder is at 400 ℃ of following hydrogen annealing 3h;
3, be to be pressed into base substrate under the 200MPa with the powder after the anneal waiting static pressure then;
4, with pressed compact 900 ℃ of sintering 5h under hydrogen atmosphere;
5, subsequently sintered compact is carried out hot pressing, hot pressing temperature is 800 ℃, and hot pressing pressure is 400MPa, pressurize 10 minutes;
6, then according to original sintering process resintering once with base substrate after the hot pressing; Processing parameter is with the 5th step;
7, again the base substrate behind the resintering is hot extruded into bar or sheet material, extrusion temperature is 500 ℃, and hot extrusion speed is 7cm/min, and mold preheating temperature is 350 ℃, and extrusion ratio is 100.To push back bar or sheet material at last and make the finished product through after the deformation process.
The implementation result of this enforcement: tensile strength: 680MPa; Recrystallization temperature: 900 ℃; Electric conductivity 75%IACS
Embodiment six
With preparation Cu-3Al 2O 3-1Cr 2O 3-0.1Al 4C 3-0.1C multi-element Cu-base matrix material is an example
1, at first with 91.4wt%Cu powder, 2wt%Al powder, 0.7wt%Cr powder, 5wt%Cu 2O powder, 0.3wt%C powder mixing and ball milling 150h, ratio of grinding media to material is 100: 1, and rotational speed of ball-mill is 500 rev/mins, and milling atmosphere is an argon gas;
2, then that ball milling is good powder is at 400 ℃ of following hydrogen annealing 3h;
3, be to be pressed into base substrate under the 500MPa with the powder after the anneal waiting static pressure then;
4, with pressed compact 900 ℃ of sintering 5h under hydrogen atmosphere;
5, subsequently sintered compact is carried out hot pressing, hot pressing temperature is 850 ℃, and hot pressing pressure is 400MPa, pressurize 10 minutes;
6, then according to original sintering process resintering once with base substrate after the hot pressing; Processing parameter is with the 5th step;
7, again the base substrate behind the resintering is hot extruded into bar or sheet material, extrusion temperature is 850 ℃, and hot extrusion speed is 5cm/min, and mold preheating temperature is 550 ℃, and extrusion ratio is 300.To push back bar or sheet material at last and make the finished product through after the deformation process.
The implementation result of present embodiment: tensile strength: 650MPa; Recrystallization temperature: 860 ℃; Electric conductivity 80%IACS.
As can be seen from the above embodiments, the present invention mainly adopts the method for high-energy ball milling, in the high energy knockout process, generate the tiny polynary wild phase of disperse by various different element generation unbalance response original positions, solved the problem that the disperse phase kind is single, particle is thick, product has good mechanical performance and conductivity, and preparation technology is simple, operation is with low cost easily.The prepared material wear ability of the present invention obviously is better than the C18150 copper zirconium alloy, and recrystallization temperature is 650~900 ℃, and tensile strength reaches 500~800MPa, and electric conductivity is between 70~90%IACS.

Claims (10)

1. multiple dispersion strengthening copper-base composite material prepared in situ, it is characterized in that, comprise Cu and wild phase, wherein wild phase is that wild phase is at least three kinds (weight percents) in the following material: 0.3%≤titanium carbide (TiC)≤5%, 0.3%≤zirconium carbide (ZrC)≤5%, 0.3%≤aluminum oxide (Al 2O 3)≤5%, 0.3%≤titanium boride (TiB 2)≤5%, 0.1%≤aluminium carbide (Al 4C 3)≤5%, 0.3%≤chromic oxide (Cr 2O 3)≤5%, 0.3%≤zirconium white (ZrO)≤5%, 0.1%≤graphite≤1%; Surplus is Cu.
2. multiple dispersion strengthening copper-base composite material prepared in situ as claimed in claim 1 is characterized in that, described titanium carbide, zirconium carbide, aluminum oxide, graphite, titanium boride, aluminium carbide, chromic oxide, zirconic mean particle size are respectively between 10nm-10 μ m.
3. the preparation method of a multiple dispersion strengthening copper-base composite material prepared in situ as claimed in claim 1 is characterized in that, may further comprise the steps:
The first step is at first with at least two kinds of powder in Cu powder and Ti powder, Zr powder, Al powder, the Cr powder and Graphite Powder 99, B powder, Cu 2At least a powder mixes ball milling in the O powder;
Second the step, with powder behind the ball milling in the hydrogen atmosphere anneal;
In the 3rd step, wait under the static pressure powder compression after the three-step annealing processing is become blank;
In the 4th step, the blank to compression moulding in high temperature sintering furnace carries out sintering;
In the 5th step, the blank behind the sintering is carried out hot pressing;
The 6th step, the base substrate after the hot pressing is carried out resintering, processing parameter is with the 5th step;
In the 7th step, the base substrate behind the resintering is carried out hot extrusion.
4. the preparation method of multiple dispersion strengthening copper-base composite material prepared in situ as claimed in claim 3 is characterized in that, in the first step, described ball milling, wherein ratio of grinding media to material is between 10: 1~100: 1, and the ball milling time, rotational speed of ball-mill was at 200~800 rev/mins between 2h~200h; Milling atmosphere is an inert atmosphere.
5. the preparation method of multiple dispersion strengthening copper-base composite material prepared in situ as claimed in claim 3 is characterized in that, in second step, described anneal is meant at 200-600 ℃ of annealing 0.5~10h and handles.
6. the preparation method of multiple dispersion strengthening copper-base composite material prepared in situ as claimed in claim 3 is characterized in that, in the 3rd step, and the described static pressure that waits, wherein pressure is 100MPa~500MPa.
7. the preparation method of multiple dispersion strengthening copper-base composite material prepared in situ as claimed in claim 3 is characterized in that, in the 4th step, and described sintering, wherein sintering temperature is 750~1000 ℃, sintering time is 1-10h, hydrogen atmosphere or inert atmosphere protection.
8. the preparation method of multiple dispersion strengthening copper-base composite material prepared in situ as claimed in claim 3 is characterized in that, in the 5th step, described hot pressing, wherein hot pressing temperature is 500~1000 ℃, and hot pressing pressure is between 100~800MPa, and the hot pressing soaking time is 5~60min.
9. the preparation method of multiple dispersion strengthening copper-base composite material prepared in situ as claimed in claim 3 is characterized in that, in the 6th step, and described resintering, wherein sintering temperature is 750~1000 ℃, sintering time is 1~10h, hydrogen atmosphere or inert atmosphere protection.
10. the preparation method of multiple dispersion strengthening copper-base composite material prepared in situ as claimed in claim 3, it is characterized in that, in the 7th step, described hot extrusion, wherein blank heating temperature is at 300~900 ℃, 200~700 ℃ of extrusion mould preheating temperatures, extrusion speed are 5~12cm/min, and extrusion ratio is 10~400.
CN200910055061A 2009-07-20 2009-07-20 Multiple dispersion strengthening copper-base composite material prepared in situ and preparation method thereof Pending CN101613816A (en)

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