CN102260803B - Nano TiC0.5 particle in situ reinforced Cu(Al) composite material and preparation method thereof - Google Patents
Nano TiC0.5 particle in situ reinforced Cu(Al) composite material and preparation method thereof Download PDFInfo
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- CN102260803B CN102260803B CN201110198183.9A CN201110198183A CN102260803B CN 102260803 B CN102260803 B CN 102260803B CN 201110198183 A CN201110198183 A CN 201110198183A CN 102260803 B CN102260803 B CN 102260803B
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- 239000002245 particle Substances 0.000 title claims abstract description 40
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002131 composite material Substances 0.000 title abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 28
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 229910052786 argon Inorganic materials 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000011159 matrix material Substances 0.000 claims description 33
- 239000002994 raw material Substances 0.000 claims description 18
- 229910052802 copper Inorganic materials 0.000 claims description 17
- 239000000758 substrate Substances 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 150000001298 alcohols Chemical class 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 229910017767 Cu—Al Inorganic materials 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 239000010949 copper Substances 0.000 abstract description 70
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 4
- 238000000498 ball milling Methods 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 230000006835 compression Effects 0.000 abstract 1
- 238000007906 compression Methods 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 239000000956 alloy Substances 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 125000004429 atom Chemical group 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000002787 reinforcement Effects 0.000 description 3
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- -1 form octahedra Chemical group 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 150000003624 transition metals Chemical group 0.000 description 1
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Abstract
The invention provides a nano TiC0.5 particle in situ reinforced Cu(Al) composite material and a preparation method thereof. The material comprises the following chemical components by weight percent: 0.37-25.22wt% of TiC0.5, 68.46-99.54 wt% of Cu and 0.09-6.32wt% of Al. The preparation method of the material comprises the following steps: proportionally burdening Ti2AlC powder and pure copper powder, wherein the proportion of Ti2AlC is 0.46-31.54wt%, and the proportion of Cu is 68.46-99.54wt%; carrying out ball milling and mixing materials, drying, and carrying out cold pressing and formation at the pressure of 140-180MPa; and carrying out constant pressure sintering at the temperature of 1100-1180 DEG C, protecting with argon, and insulating for 20-30 minutes so as to obtain the nano TiC0.5 particle in situ reinforced Cu(Al) composite material. With high compression strength, large deformation rate and high conductivity, the material can be widely used for preparing key devices of mechanical, electric, chemical and carrying tools.
Description
Technical field
The present invention relates to a kind of nano TiC
0.5particle in-situ Reinforced Cu (Al) matrix material and preparation method thereof.
Background technology
The matrix material being formed by one or more ceramic phases enhancing copper or copper alloy, the satisfactory electrical conductivity of existing copper and thermal conductivity, high intensity and toughness, there is again the characteristic such as high temperature resistant, corrosion-resistant, wear-resistant of pottery, have been widely used in fields such as electrician, chemical industry, traffic, machineries, be widely applied to the fields such as electrical contact, electric switch, heat exchanger.But the interface wet ability between copper and most of pottery is poor, make the preparation of ceramic Reinforced Cu-Base Composites more difficult.
In recent years, nano-particle reinforcement Cu-base composites, makes it reach excellent mechanics, tribological property, causes extensive concern.But, wild phase particle is directly added to the traditional preparation method in copper matrix, wild phase particle often can not be dispersed in copper matrix, and cost is higher.Therefore, can there is strong interface to be combined with copper, there is again nano-particle reinforcement effect, and the material of preparation process economy be that investigators pursue always.
In recent years, ternary layered ceramic material Ti
2alC has been subject to Materials science worker's extensive attention.It has metal and ceramic advantage concurrently, the electroconductibility that like metal has equally had and thermal conductivity, and relatively soft, anti-thermal shock, show as plasticity under high temperature; As pottery, there is good oxidation-resistance, corrosion-resistant, under high temperature, can keep higher intensity.Ti
2the crystalline structure of AlC is measured by Jeitschko and Nowotny the earliest, and its crystalline structure is hexagonal system, and spacer is P63/mmc, and lattice parameter is a=0.307nm, c=1.769nm, and theoretical density is 4.11g/cm
3.Closelypacked Ti octahedral layer is separated by a plane layer Al atom, the octahedra center of Ti is carbon atom, and every two-layer one deck Al atomic shell that just has, between transition metal atoms Ti and C atom, form octahedra, C atom is positioned at octahedral center, between Ti atom and C atom, is combined into strong covalent bond; And be weak binding between Ti atom and Al family plane, therefore, perpendicular to easily sliding under the effect of shearing stress between layers of c-axis.(reference: Jeitschko W, Nowotny H et al.Monatash Chem.1963,94:672).So special structure is expected investigator, if Ti
2alC and Cu are compound, due to the strong molten power of Cu and Al, probably destroy Ti
2in AlC, compared with the Al atomic shell of weak binding, make its stripping and enter in Cu solution.Like this, Ti
2alC particle will be decomposed and form ultra-fine grain Reinforced Cu sill, this also just investigator to pursue.
Summary of the invention
The object of the present invention is to provide a kind of with Ti
2alC powder and pure copper powder are the nano TiC that raw material is made
0.5particle in-situ Reinforced Cu (Al) matrix material and preparation method thereof.Technology to be solved by this invention asks and is, a little less than existing ceramic particle is combined with the interface of copper, and the problem that particle scale is large.
Technical scheme of the present invention:
Nano TiC of the present invention
0.5particle in-situ Reinforced Cu (Al) matrix material, its composition is as follows:
TiC
0.5 0.37～25.22wt％，
Cu 68.46～99.54wt％，
Al 0.09～6.32wt％。
Nano TiC of the present invention
0.5particle in-situ Reinforced Cu (Al) matrix material, its microstructure is as follows:
The Ti of raw material
2alC particle breakdown, Al is extracted in Cu, forms Cu (Al) alloy.Ti
2alC is decomposed to form the TiC of 50～150nm
0.5particle, evenly Reinforced Cu (Al) alloy composite materials.
Nano TiC of the present invention
0.5particle in-situ Reinforced Cu (Al) matrix material, its mechanical property and electric property are as follows:
Incompressible intensity: 170～860MPa,
Maximum distortion rate: 8～37%,
Specific conductivity: 9～62%IACS.
Nano TiC of the present invention
0.5the preparation method of particle in-situ Reinforced Cu (Al) matrix material, comprises following steps:
Step 1 batching
By Ti
2alC powder and fine copper (Cu) powder is prepared burden in following ratio:
Ti
2AlC 0.46～31.54wt.％，
Cu 68.46～99.54wt.％；
Step 2 batch mixing
In every 100 grams of above-mentioned batchings, add the dehydrated alcohol of 70～120 milliliters and the agate ball of 200～400 grams, ball milling 2～4 hours, 60～70 DEG C of oven dry in baking oven, grind the mixing raw material of drying, and cross 80～200 mesh sieves;
Step 3 coldmoulding
Raw material after above-mentioned batch mixing is pressed under 140～180MPa pressure to the base substrate of any shape;
Step 4 sintering
The base substrate of above-mentioned coldmoulding is put into High Temperature Furnaces Heating Apparatus, under argon shield, by the temperature rise rate of 10～40 DEG C/min, furnace temperature is risen to 1100～1180 DEG C, insulation 20～30min, cooling with the speed of 10～15 DEG C/min, obtain nano TiC of the present invention
0.5particle in-situ Reinforced Cu (Al) matrix material.
The beneficial effect that the present invention has:
Nano TiC of the present invention
0.5particle in-situ Reinforced Cu (Al) matrix material, its intensity and specific conductivity are much higher than single-phase Ti
2alC material, also higher than common Cu alloy material.Its intensity, maximum distortion rate and specific conductivity are according to Ti
2the proportioning raw materials of AlC and copper and difference; Ti
2the larger made nano TiC of ratio of AlC
0.5the incompressible intensity of particle in-situ Reinforced Cu (Al) matrix material is larger and maximum distortion rate and specific conductivity are less.For nano TiC of the present invention
0.5the application of particle in-situ Reinforced Cu (Al) matrix material, can choose suitable Ti according to actual service requirements
2the proportioning raw materials of AlC and copper.
Nano TiC of the present invention
0.5the preparation method of particle in-situ Reinforced Cu (Al) matrix material, its main benefit be formula and preparation technology simple; By implementation step of the present invention, Ti in sintering process
2al in AlC is dissolved, Ti
2alC decomposes, and laminate structure is destroyed, forms the TiC of 50～150nm
0.5the microstructure of Particles Reinforced Cu (Al) alloy, and this special in-situ nano particle enhancement method makes prepared nano TiC
0.5and between Cu (Al) alloy, have good interface bond strength, this is also the fundamental cause that made matrix material has higher-strength, larger deformation rate and higher specific conductivity.
The present invention and denomination of invention " a kind of Ti
3c
2/ Cu-Al metallic substance and preparation method thereof ", the patent of invention that the patent No. is ZL200510012150.5 is compared, nano TiC of the present invention
0.5its wild phase difference of particle in-situ Reinforced Cu (Al) matrix material, wild phase microstructure form difference.Wild phase TiC of the present invention
0.5and compare Ti between Cu (Al)
3c
2and between Cu (Al), there is better interface wet ability and interface bond strength, thereby there is higher specific conductivity and compressive strength; Nano-particle reinforcement compares Ti uniformly simultaneously
3c
2in/Cu (Al) sintering metal, long plate shape particle has larger deformation rate.Therefore the present invention is more suitable for needs higher-strength and specific conductivity, needs to have the field of moderate finite deformation rate simultaneously.
Nano TiC of the present invention
0.5particle in-situ Reinforced Cu (Al) matrix material can be widely used in the fields such as machinery, electrician, traffic, chemical industry, for example, for the manufacture of contact, the slide block etc. of various high performance rollers, ring header, resistance soldering tip, various high power switch or contactor.
Nano TiC of the present invention
0.5particle in-situ Reinforced Cu (Al) matrix material sintering under normal pressure just can obtain, and is well suited for the suitability for industrialized production of the device of large-sized or complicated shape.
Brief description of the drawings
Fig. 1 and Fig. 2 are different content nano TiCs of the present invention
0.5the microstructural scanning electronic microscope of particle in-situ Reinforced Cu (Al) matrix material (SEM) photo.
Embodiment
Embodiment one
Step 1 batching
Take purity and be 98.5% Ti
2159.00 grams, the Cu powder that 0.74 gram, AlC powder, purity are 99.9%.
Step 2 batch mixing
The batching of step 1 is mixed, add 110 milliliters of dehydrated alcohols and 320 grams of agate balls, ball mill mixing 2 hours, with 60 DEG C of oven dry, by the mixing raw material grinding of drying, mistake 100 mesh sieves.
Step 3 coldmoulding
The mixing raw material of step 2, under 140MPa pressure, is cold-pressed into bar shaped base substrate.
Step 4 sintering
Bar shaped base substrate prepared by step 3 is put into the graphite jig of High Temperature Furnaces Heating Apparatus, under argon shield, is warming up to 1100 DEG C with the speed of 40 DEG C/min, and insulation 20min, is down to 60 DEG C with the speed of 10 DEG C/min by furnace temperature, obtains nano TiC of the present invention
0.5particle in-situ Reinforced Cu (Al) matrix material; Wherein TiC
0.5content be about 0.59 gram, all the other are Cu and Al (Cu content is 159.00 grams, and Al content is about 0.15 gram).
By above-mentioned nano TiC 0.5 particle in-situ Reinforced Cu (Al) matrix material, be processed into the sample of Φ 10mm × 30mm, carry out incompressible strength test; The compressive strength recording is 173.30MPa, and maximum distortion rate is 36.5%, and electric conductivity is 61.8%IACS.
Embodiment two
Step 1 batching
Take purity and be 99.0% Ti
225.64 grams, the Cu powder that 2.96 grams, AlC powder, purity are 99.9%.
Step 2 batch mixing
The batching of step 1 is mixed, add 20 milliliters of dehydrated alcohols and 60 grams of agate balls, ball mill mixing 2 hours, with 60 DEG C of oven dry, by the mixing raw material grinding of drying, mistake 80 mesh sieves.
Step 3 coldmoulding
The mixing raw material of step 2, under 160MPa pressure, is cold-pressed into bar shaped base substrate.
Step 4 sintering
Bar shaped base substrate prepared by step 3 is put into the graphite jig of High Temperature Furnaces Heating Apparatus, under argon shield, is warming up to 1130 DEG C with the speed of 30 DEG C/min, and insulation 20min, is down to 60 DEG C with the speed of 10 DEG C/min by furnace temperature, obtains nano TiC of the present invention
0.5particle in-situ Reinforced Cu (Al) matrix material; Wherein TiC
0.5content be about 2.37 grams, all the other are Cu and Al (Cu content is 25.64 grams, and Al content is about 0.59 gram).
By above-mentioned nano TiC
0.5particle in-situ Reinforced Cu (Al) matrix material, is processed into the sample of Φ 10mm × 30mm, carries out incompressible strength test; The compressive strength recording is 332.40MPa, and maximum distortion rate is 28.6%, and specific conductivity is 47.1%IACS.
Embodiment three
Step 1 batching
Take purity and be 99.0% Ti
222.43 grams, the Cu powder that 4.44 grams, AlC powder, purity are 99.9%.
Step 2 batch mixing
The batching of step 1 is mixed, add 20 milliliters of dehydrated alcohols and 60 grams of agate balls, ball mill mixing 3 hours, with 70 DEG C of oven dry, by the mixing raw material grinding of drying, mistake 110 mesh sieves.
Step 3 coldmoulding
The mixing raw material of step 2, under 160MPa pressure, is cold-pressed into bar shaped base substrate.
Step 4 sintering
Bar shaped base substrate prepared by step 3 is put into the graphite jig of High Temperature Furnaces Heating Apparatus, under argon shield, is warming up to 1150 DEG C with the speed of 30 DEG C/min, and insulation 30min, is down to 60 DEG C with the speed of 15 DEG C/min by furnace temperature, obtains nano TiC of the present invention
0.5particle in-situ Reinforced Cu (Al) matrix material; Wherein TiC
0.5content be about 3.55 grams, all the other are Cu and Al (Cu content is 22.43 grams, and Al content is about 0.89 gram).
By above-mentioned nano TiC
0.5particle in-situ Reinforced Cu (Al) matrix material, is processed into the sample of Φ 10mm × 30mm, carries out incompressible strength test; The compressive strength recording is 587.65MPa, and maximum distortion rate is 18.18%, and electric conductivity is 24.2%IACS.
Embodiment four
Step 1 batching
Take purity and be 99.2% Ti
219.22 grams, the Cu powder that 5.92 grams, AlC powder, purity are 99.9%.
Step 2 batch mixing
The batching of step 1 is mixed, add 30 milliliters of dehydrated alcohols and 100 grams of agate balls, ball mill mixing 3 hours, with 70 DEG C of oven dry, by the mixing raw material grinding of drying, mistake 180 mesh sieves.
Step 3 coldmoulding
The mixing raw material of step 2, under 180MPa pressure, is cold-pressed into bar shaped base substrate.
Step 4 sintering
Bar shaped base substrate prepared by step 3 is put into the graphite jig of High Temperature Furnaces Heating Apparatus, under argon shield, is warming up to 1160 DEG C with the speed of 30 DEG C/min, and insulation 30min, is down to 60 DEG C with the speed of 15 DEG C/min by furnace temperature, obtains nano TiC of the present invention
0.5particle in-situ Reinforced Cu (Al) matrix material; Wherein TiC
0.5content be about 4.73 grams, all the other are Cu and Al (Cu content is 19.22 grams, and Al content is about 1.19 grams).
By above-mentioned nano TiC
0.5particle in-situ Reinforced Cu (Al) matrix material, is processed into the sample of Φ 10mm × 30mm, carries out incompressible strength test; The compressive strength recording is 773.85MPa, and maximum distortion rate is 8.62%, and electric conductivity is 12.1%IACS.
Embodiment five
Step 1 batching
Take purity and be 99.2% Ti
216.43 grams, the Cu powder that 7.57 grams, AlC powder, purity are 99.9%.
Step 2 batch mixing
The batching of step 1 is mixed, add 20 milliliters of dehydrated alcohols and 60 grams of agate balls, ball mill mixing 4 hours, with 70 DEG C of oven dry, by the mixing raw material grinding of drying, mistake 200 mesh sieves.
Step 3 coldmoulding
The mixing raw material of step 2, under 180MPa pressure, is cold-pressed into bar shaped base substrate.
Step 4 sintering
Bar shaped base substrate prepared by step 3 is put into the graphite jig of High Temperature Furnaces Heating Apparatus, under argon shield, is warming up to 1180 DEG C with the speed of 30 DEG C/min, and insulation 30min, is down to 60 DEG C with the speed of 15 DEG C/min by furnace temperature, obtains nano TiC of the present invention
0.5particle in-situ Reinforced Cu (Al) matrix material; Wherein TiC
0.5content be about 6.05 grams, all the other are Cu and Al (Cu content is 16.43 grams, and Al content is about 1.52 grams).
By above-mentioned nano TiC
0.5particle in-situ Reinforced Cu (Al) matrix material, is processed into the sample of Φ 10mm × 30mm, carries out incompressible strength test; The compressive strength recording is 859.67MPa, and maximum distortion rate is 4.73%, and electric conductivity is 9.8%IACS.
Claims (1)
1. a nano TiC
0.5the preparation method of particle in-situ Reinforced Cu-Al matrix material, is characterized in that, the method comprises the following steps:
Step 1 batching
Take purity and be 98.5% Ti
2159.00 grams, the Cu powder that 0.74 gram, AlC powder, purity are 99.9%;
Step 2 batch mixing
The batching of step 1 is mixed, add 110 milliliters of dehydrated alcohols and 320 grams of agate balls, ball mill mixing 2 hours, with 60 DEG C of oven dry, by the mixing raw material grinding of drying, mistake 100 mesh sieves;
Step 3 coldmoulding
The mixing raw material of step 2, under 140MPa pressure, is cold-pressed into bar shaped base substrate;
Step 4 sintering
Bar shaped base substrate prepared by step 3 is put into the graphite jig of High Temperature Furnaces Heating Apparatus, under argon shield, is warming up to 1100 DEG C with the speed of 40 DEG C/min, and insulation 20min, is down to 60 DEG C with the speed of 10 DEG C/min by furnace temperature, obtains nano TiC
0.5particle in-situ Reinforced Cu-Al matrix material; Wherein TiC
0.5content be 0.59 gram, all the other are Cu and Al;
By above-mentioned nano TiC
0.5particle in-situ Reinforced Cu-Al matrix material, is processed into the sample of Φ 10mm × 30mm, carries out incompressible strength test; The compressive strength recording is 173.30MPa, and maximum distortion rate is 36.5%, and electric conductivity is 61.8%IACS.
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| CN114182098A (en) * | 2016-11-02 | 2022-03-15 | 洛阳铜一金属材料发展有限公司 | Separation method of copper-aluminum composite material |
| CN107217187B (en) * | 2017-06-09 | 2019-05-28 | 北京交通大学 | A kind of TiCxThe preparation method of/Cu co-continuous cermet material |
| CN108793166B (en) * | 2018-07-10 | 2020-06-19 | 中国科学院宁波材料技术与工程研究所 | Composite material of subgroup metal composite MXenes, preparation method and application thereof |
| CN109355528A (en) * | 2018-12-18 | 2019-02-19 | 江西理工大学 | A kind of TiCx-Al2O3/Cu based composites and its preparation method and application |
| CN113481399A (en) * | 2021-07-05 | 2021-10-08 | 北京交通大学 | With Ti2In-situ TiC generation by using AlC as precursorxReinforced titanium-based composite material and preparation method thereof |
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| CN1733955A (en) * | 2005-07-12 | 2006-02-15 | 北京交通大学 | Ti3C2/Cu-Al ceramet material and its preparation method |
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| CN1733955A (en) * | 2005-07-12 | 2006-02-15 | 北京交通大学 | Ti3C2/Cu-Al ceramet material and its preparation method |
Non-Patent Citations (1)
| Title |
|---|
| 黄振莺等.原位热压反应制备高性能亚微米层状Ti3C2/（Cu-Al）金属陶瓷.《稀有金属材料与工程》.2009,第38卷(第增刊2期),第487-490页. * |
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