CN101701300B - Method for preparing titanium diboride dispersion-strengthened Cu-base composites by using mechanical alloying method - Google Patents
Method for preparing titanium diboride dispersion-strengthened Cu-base composites by using mechanical alloying method Download PDFInfo
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- CN101701300B CN101701300B CN2009100951769A CN200910095176A CN101701300B CN 101701300 B CN101701300 B CN 101701300B CN 2009100951769 A CN2009100951769 A CN 2009100951769A CN 200910095176 A CN200910095176 A CN 200910095176A CN 101701300 B CN101701300 B CN 101701300B
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- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 18
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229910033181 TiB2 Inorganic materials 0.000 title claims abstract description 16
- 238000005551 mechanical alloying Methods 0.000 title claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 66
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000011812 mixed powder Substances 0.000 claims abstract description 30
- 229910052786 argon Inorganic materials 0.000 claims abstract description 15
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007789 gas Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000005554 pickling Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000005245 sintering Methods 0.000 claims abstract description 6
- 239000010949 copper Substances 0.000 claims description 42
- 229910052802 copper Inorganic materials 0.000 claims description 24
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 20
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 5
- 239000010959 steel Substances 0.000 claims description 5
- 230000003014 reinforcing effect Effects 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 238000005516 engineering process Methods 0.000 abstract description 9
- 239000002253 acid Substances 0.000 abstract description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract 4
- 238000000227 grinding Methods 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 239000011159 matrix material Substances 0.000 description 14
- 238000002360 preparation method Methods 0.000 description 11
- 238000005275 alloying Methods 0.000 description 10
- 229910000881 Cu alloy Inorganic materials 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 238000013459 approach Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000011065 in-situ storage Methods 0.000 description 4
- 238000005728 strengthening Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000006104 solid solution Substances 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910017813 Cu—Cr Inorganic materials 0.000 description 1
- 229910017827 Cu—Fe Inorganic materials 0.000 description 1
- 229910017945 Cu—Ti Inorganic materials 0.000 description 1
- 229910017985 Cu—Zr Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
Abstract
The invention discloses a method for preparing titanium diboride dispersion-strengthened Cu-base composites by using a mechanical alloying method, taking Cu powder, TiO2 powder, B2O3 powder and Mg powder with the granularity less than 100 meshes and purity more than 99 percent as raw materials. The method comprises the following steps of: thoroughly mixing the Cu powder, the TiO2 powder, the B2O3 powder and the Mg powder; carrying out high-energy ball-grinding on the mixed powder for 3 to 15 hours at the revolution speed of 1000 to 2000 rpm at room temperature; acid pickling the powder for 2 to 15 hours at the temperature of 20 to 80 DEG C with 1 to 3 mol/L hydrochloric acid to get mixed powder of Cu and TiB2; drying the mixed powder of Cu and TiB2, and carrying out high-energy ball-grinding on mixed powder of Cu and TiB2 for 1 to 3 hours ; cold pressing the mixed powder of Cu and TiB2 for forming; and at last sintering the mixture of Cu and TiB2 for 1 to 3 hours in a resistance furnace with argon protection gas at the temperature of 800 to 1000 DEG C to get the TiB2 dispersion-strengthened Cu-base composites with granularity of 5 to 10 microns. The method for preparing the TiB2 dispersion-strengthened Cu-base composites by using the simple high-energy ball-milling mechanical alloying method has the advantages of simple technology, low production cost, high product yield and high product quality.
Description
Technical field
The invention belongs to the metal-base composites preparing technical field, a kind of method of mechanical alloying method preparing titanium diboride dispersion-strengthened Cu-base composites is provided.
Background technology
Copper alloy with high strength and high conductivity is one type of structure function material that good comprehensive physicals and mechanical property are arranged; Irreplaceable effect is arranged in numerous industrial circles, be widely used in electric power, electrician, the mechanical manufacturing field such as electrode, power asynchronous traction motor of high rotor, electric railway contact wire, thermonuclear reactor experiment (ITER) divertor vertical target radiator element of the lead frame mouth of unicircuit, all kinds of spot welding and roll seam welding machine.But intensity in the copper alloy and electroconductibility are a pair of conflicting characteristics always, and this disappears and other rises, generally can only under the prerequisite of sacrificing specific conductivity and thermal conductivity, improve the mechanical property of copper, to obtain high intensity.How to solve this contradiction, be the key subject of copper alloy with high strength and high conductivity research always.
The approach that obtains copper alloy with high strength and high conductivity at present mainly contains two kinds: the one, and the alloying approach is promptly introduced alloying element and is strengthened to form copper alloy in copper; The 2nd, compoundization approach is promptly introduced second strengthening phase and is strengthened to form matrix material in the copper matrix.
Alloying is in copper, to add alloying element, and solute atoms can cause the lattice lattice distortion after dissolving in lattice, causes stress field, thereby intensity is improved.Traditional alloying is mainly strengthened the copper matrix through means such as solution strengthening and precipitation strengths.According to the alloy solid solution strengthening principle, solid solution alloy unit commonly used in the copper alloy have Sn, Cd, Ag etc.According to the precipitation strength principle, such copper alloy of having developed at present has Cu-Cr, Cu-Zr, Cu-Ti, Cu-Fe etc.The advantage of alloying is that technology is ripe, technology is simple, cost is lower, suitability for scale production.Its shortcoming is that distored dot matrix has reduced electroconductibility to the corresponding aggravation of the scattering process of moving electron in the crystal.Generally can only under the prerequisite of sacrificing specific conductivity, improve the mechanical property of copper.The copper alloy intensity of alloying preparation is between 350 ~ 650MPa, and specific conductivity generally is no more than 90%IACS, is difficult to satisfy electrical part of new generation to performance demands.
According to conductivity theory; A little less than the scattering process that second the scattering process of the electronics that causes in the copper matrix causes in the copper matrix than the solid solution atom many; So complex intensifying can not cause the obvious reduction of copper matrix electroconductibility; And wild phase can also improve the mechanical property of matrix, becomes the main means that obtain high-strength high-conductive copper alloy.Research data shows, the composite material strength such as Cu-Ta, Cu-Nd that utilizes the preparation of compoundization of material is greater than 1400MPa, and electric conductivity reaches more than the 90%IACS, and obtains practical applications.The difference that compoundization approach is introduced mode based on hardening constituent can be divided into artificial composite algorithm and in-situ compositing.
Artificial composite algorithm is strengthened the copper matrix through the whisker or the fiber that in copper, add second phase artificially, or dependence strengthening phase itself increases the method for the strength of materials, for example oxidation reinforcement, mechanical alloying method and thomel composite algorithm etc.The characteristics of artificial composite algorithm are part method comparative maturities, and its product has obtained practical applications, but complex process, production cost is high.In-situ compositing is in copper, to add a certain amount of alloying element; Through certain technology; Make the inner original position of copper generate wild phase, rather than strengthen body and two kinds of materials of matrix copper with regard to existing before the processing, comprise viscous deformation composite algorithm, reaction in composite algorithm and growth in situ composite algorithm.Contrast artificial composite algorithm, the matrix and the second phase interface consistency are better in the product that in-situ compositing obtained, and step of preparation process reduces, and production cost reduces.
TiB2 (TiB
2) have plurality of advantages such as HMP, low density, good heat conduction and electroconductibility, be widely used in fields such as conducting ceramic material, composite ceramic materials.In metallic substance such as Al, Fe, Cu, add TiB
2, can give full play to metallic matrix and TiB
2Wild phase advantage separately obtains high performance metal-base composites.Traditional T iB
2The preparation of dispersion-strengthened metal based composites need obtain TiB earlier
2Superfine powder passes through certain method then TiB
2Be distributed in the Cu matrix.But TiB
2The preparation technology of superfine powder is comparatively complicated, causes TiB
2The preparation section of dispersion-strengthened metal based composites is more, and production cost is higher.
High-energy ball milling (high-energy ball milling) reaction mechanical alloying method is to utilize mechanical energy to come induced chemical reaction or induced material tissue, structure and changes of properties, has become a kind of important channel of preparation super-fine material and novel material.As a kind of new technology; High-energy ball milling machinery alloying has obvious reduction reaction activity, crystal grain thinning, greatly improves powder activity and improve even particle distribution property and strengthen combining of interface between body and the matrix; Promote the solid ionic diffusion; Bringing out cryochemistry reaction, thereby improved the performances such as degree of compactness, electricity, calorifics of material, is a kind of energy-conservation, material preparation technology efficiently.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of method that adopts the mechanical alloying method preparing titanium diboride dispersion-strengthened Cu-base composites is provided, shorten operational path, reduce production costs, improve the quality of products.
The technical scheme that the present invention prepares TiB2 micro mist stupalith is: all less than 100 orders, purity is all greater than 99% Cu powder, TiO with granularity
2Powder, B
2O
3Powder and Mg powder are raw material, with Cu powder, TiO
2Powder, B
2O
3Powder and Mg powder (Cu powder and TiO
2+ B
2O
3The mass ratio of+Mg powder is 80: 20 ~ 99: 1, wherein TiO
2, B
2O
3, Mg mol ratio be 1: 1: 5) uniform mixing; Is ball-to-powder weight ratio that 10: 1 ~ 100: 1 steel ball and mixed powder put into the high energy ball mill ball grinder in being full of the glove box of argon gas; Make the ball material mixture account for 10 ~ 50% of ball grinder cavity volume; At room temperature carried out high-energy ball milling 3 ~ 15 hours, make it in mechanical milling process, to take place alloying, grain refining and grain refine, form Cu, TiB with 1000 ~ 2000 rev/mins rotating speed
2With MgO admixed finepowder stupalith; Adopting concentration then is that the hydrochloric acid of 1 ~ 3mol/l carries out 2 ~ 15h pickling to mixed powder under 20 ~ 80 ℃ temperature, and flush away MgO obtains Cu+TiB
2Mixed powder; With Cu+TiB
2In being full of the glove box of argon gas, put into the high energy ball mill ball grinder once more after the mixed powder oven dry, at room temperature carried out high-energy ball milling 1 ~ 3 hour with 1000 ~ 2000 rev/mins rotating speed; With the Cu+TiB behind the ball milling once more
2Mixed powder coldmoulding; Sintering 1 ~ 3 hour in the argon shield atmosphere resistance furnace under 800 ~ 1000 ℃ of temperature obtains the TiB that particle diameter is 5 ~ 10 μ m at last
2The Cu-base composites of dispersion-strengthened.The present invention adopts simple high-energy ball milling machinery alloyage process, makes Cu powder, TiO
2Powder, B
2O
3The synthetic preparation of powder and Mg powder TiB
2Dispersed and strengthened copper-based composite material has that technology is simple, production cost is low, product production and a quality advantages of higher.Can be used for the production preparation of the high-strength highly-conductive Cu-base composites of field widespread uses such as power industry, national defense industry, unicircuit, welding set.The present invention utilizes Cu powder, TiO through to mechanical alloying and acid cleaning process parameter control
2Powder, B
2O
3The synthetic preparation of powder and Mg powder TiB
2Dispersed and strengthened copper-based composite material shortens operational path, reduces production costs, and improves the quality of products, to realize TiB
2The extensive widespread use of dispersed and strengthened copper-based composite material.
Embodiment
Further specify flesh and blood of the present invention with instance below, but content of the present invention is not limited to this.
Embodiment 1: be 150 orders with granularity, purity is 99.9% Cu powder, TiO
2Powder, B
2O
3Powder and Mg powder are raw material, with Cu powder, TiO
2Powder, B
2O
3Powder and Mg powder (Cu powder and TiO
2+ B
2O
3The mass ratio of+Mg powder is 95: 5, wherein TiO
2, B
2O
3, Mg mol ratio be 1: 1: 5) uniform mixing; Is ball-to-powder weight ratio that 20: 1 steel ball and mixed powder put into the high energy ball mill ball grinder in being full of the glove box of argon gas; Make the ball material mixture account for 15% of ball grinder cavity volume; At room temperature carried out high-energy ball milling 3 hours, form Cu, TiB with 1000 rev/mins rotating speed
2With MgO admixed finepowder stupalith; Adopting concentration then is that the hydrochloric acid of 3mol/l carries out the 12h pickling to mixed powder under 30 ℃ temperature, and flush away MgO obtains Cu+TiB
2Mixed powder; With Cu+TiB
2In being full of the glove box of argon gas, put into the high energy ball mill ball grinder once more after the mixed powder oven dry, at room temperature carried out high-energy ball milling 1 hour with 1000 rev/mins rotating speed; With the Cu+TiB behind the ball milling once more
2Mixed powder coldmoulding; Sintering is 3 hours in the last argon shield atmosphere resistance furnace under 800 ℃ of temperature, obtains the TiB that particle diameter is about 9.5 μ m
2The Cu-base composites of dispersion-strengthened.
Embodiment 2: be 200 orders with granularity, purity is 99.9% Cu powder, TiO
2Powder, B
2O
3Powder and Mg powder are raw material, with Cu powder, TiO
2Powder, B
2O
3Powder and Mg powder (Cu powder and TiO
2+ B
2O
3The mass ratio of+Mg powder is 85: 15, wherein TiO
2, B
2O
3, Mg mol ratio be 1: 1: 5) uniform mixing; Is ball-to-powder weight ratio that 40: 1 steel ball and mixed powder put into the high energy ball mill ball grinder in being full of the glove box of argon gas; Make the ball material mixture account for 25% of ball grinder cavity volume; At room temperature carried out high-energy ball milling 9 hours, form Cu, TiB with 1500 rev/mins rotating speed
2With MgO admixed finepowder stupalith; Adopting concentration then is that the hydrochloric acid of 2mol/l carries out the 9h pickling to mixed powder under 55 ℃ temperature, and flush away MgO obtains Cu+TiB
2Mixed powder; With Cu+TiB
2In being full of the glove box of argon gas, put into the high energy ball mill ball grinder once more after the mixed powder oven dry, at room temperature carried out high-energy ball milling 2 hours with 1500 rev/mins rotating speed; With the Cu+TiB behind the ball milling once more
2Mixed powder coldmoulding; Sintering is 2 hours in the last argon shield atmosphere resistance furnace under 900 ℃ of temperature, obtains the TiB that particle diameter is about 7 μ m
2The Cu-base composites of dispersion-strengthened.
Embodiment 3: be 300 orders with granularity, purity is 99.9% Cu powder, TiO
2Powder, B
2O
3Powder and Mg powder are raw material, with Cu powder, TiO
2Powder, B
2O
3Powder and Mg powder (Cu powder and TiO
2+ B
2O
3The mass ratio of+Mg powder is 80: 20, wherein TiO
2, B
2O
3, Mg mol ratio be 1: 1: 5) uniform mixing; Is ball-to-powder weight ratio that 80: 1 steel ball and mixed powder put into the high energy ball mill ball grinder in being full of the glove box of argon gas; Make the ball material mixture account for 35% of ball grinder cavity volume; At room temperature carried out high-energy ball milling 15 hours, form Cu, TiB with 2000 rev/mins rotating speed
2With MgO admixed finepowder stupalith; Adopting concentration then is that the hydrochloric acid of 1mol/l carries out the 3h pickling to mixed powder under 75 ℃ temperature, and flush away MgO obtains Cu+TiB
2Mixed powder; With Cu+TiB
2In being full of the glove box of argon gas, put into the high energy ball mill ball grinder once more after the mixed powder oven dry, at room temperature carried out high-energy ball milling 1 hour with 2000 rev/mins rotating speed; With the Cu+TiB behind the ball milling once more
2Mixed powder coldmoulding; Sintering is 1 hour in the last argon shield atmosphere resistance furnace under 1000 ℃ of temperature, obtains the TiB that particle diameter is about 5.5 μ m
2The Cu-base composites of dispersion-strengthened.
Claims (2)
1. the method for a mechanical alloying preparing titanium diboride dispersion-strengthened Cu-base composites is characterized in that: all less than 100 orders, purity is all greater than 99% Cu powder, TiO with granularity
2Powder, B
2O
3Powder and Mg powder are raw material, with Cu powder, TiO
2Powder, B
2O
3Powder and Mg powder uniform mixing; Is ball-to-powder weight ratio that 10: 1～100: 1 steel ball and mixed powder put into the high energy ball mill ball grinder in being full of the glove box of argon gas; Make the ball material mixture account for 10～50% of ball grinder cavity volume; At room temperature carried out high-energy ball milling 3～15 hours with 1000～2000 rev/mins rotating speed, pickling then obtains Cu+TiB
2Mixed powder; With Cu+TiB
2High-energy ball milling 1～3 hour once more after the mixed powder oven dry; With the Cu+TiB behind the ball milling once more
2Mixed powder coldmoulding; Sintering is 1～3 hour in the last argon shield atmosphere resistance furnace under 800～1000 ℃ of temperature, obtains TiB
2The Cu-base composites of dispersion-strengthened;
Described with Cu powder, TiO
2Powder, B
2O
3When powder and Mg powder uniform mixing, Cu powder and TiO
2+ B
2O
3The mass ratio of+Mg powder is 80: 20～99: 1, wherein TiO
2, B
2O
3, Mg mol ratio be 1: 1: 5;
Described pickling is that to adopt concentration be that the hydrochloric acid of 1～3mol/L carries out 2～15h to mixed powder under 20～80 ℃ temperature.
2. the method for mechanical alloying preparing titanium diboride dispersion-strengthened Cu-base composites according to claim 1 is characterized in that: TiB
2The reinforcing particle median size of dispersed and strengthened copper-based composite material is 5～10 μ m.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009100951769A CN101701300B (en) | 2009-11-11 | 2009-11-11 | Method for preparing titanium diboride dispersion-strengthened Cu-base composites by using mechanical alloying method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100951769A CN101701300B (en) | 2009-11-11 | 2009-11-11 | Method for preparing titanium diboride dispersion-strengthened Cu-base composites by using mechanical alloying method |
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| CN101701300A CN101701300A (en) | 2010-05-05 |
| CN101701300B true CN101701300B (en) | 2012-01-11 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018017581A1 (en) * | 2016-07-18 | 2018-01-25 | Board Of Regents, University Of Texas System | Nano/micro scale porous structured alloys using selective alloying process based on elemental powders |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101956094B (en) * | 2010-10-15 | 2011-11-30 | 哈尔滨工业大学深圳研究生院 | Preparation method of high-strength and high-conductivity dispersion-strengthened alloy |
| CN102703746B (en) * | 2012-06-12 | 2014-06-25 | 嵊州德庆机械有限公司 | Method for preparing Y2O3-strengthened copper by acid-base copper etching waste solution |
| CN102703749B (en) * | 2012-06-12 | 2014-07-02 | 嵊州德庆机械有限公司 | Preparation method of Y2O3-strengthened copper |
| CN106916992B (en) * | 2017-03-31 | 2018-11-09 | 江西理工大学 | A kind of Al2O3- TiC Cu-base composites and preparation method thereof |
| CN107675009B (en) * | 2017-08-03 | 2019-07-23 | 西安理工大学 | Three-dimensional net structure titanium diboride enhances Cu-base composites and preparation method thereof |
| CN114210982B (en) * | 2021-11-16 | 2023-05-12 | 陕西斯瑞新材料股份有限公司 | Method for preparing Cu-Cr2Nb alloy with nano structure |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2018017581A1 (en) * | 2016-07-18 | 2018-01-25 | Board Of Regents, University Of Texas System | Nano/micro scale porous structured alloys using selective alloying process based on elemental powders |
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