CN101704678A - Self-propagation high-temperature synthesizing preparation method of TiB2-TiC complex ceramic micropowder - Google Patents
Self-propagation high-temperature synthesizing preparation method of TiB2-TiC complex ceramic micropowder Download PDFInfo
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- CN101704678A CN101704678A CN200910095175A CN200910095175A CN101704678A CN 101704678 A CN101704678 A CN 101704678A CN 200910095175 A CN200910095175 A CN 200910095175A CN 200910095175 A CN200910095175 A CN 200910095175A CN 101704678 A CN101704678 A CN 101704678A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000919 ceramic Substances 0.000 title claims abstract description 14
- 230000002194 synthesizing effect Effects 0.000 title abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 51
- 238000002485 combustion reaction Methods 0.000 claims abstract description 18
- 239000011812 mixed powder Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000000498 ball milling Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 7
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 6
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 6
- 239000010936 titanium Substances 0.000 claims description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 239000003595 mist Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 claims description 6
- 229910033181 TiB2 Inorganic materials 0.000 claims description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 5
- 230000005611 electricity Effects 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 239000010959 steel Substances 0.000 claims description 5
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000003825 pressing Methods 0.000 abstract 2
- 238000010891 electric arc Methods 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 20
- 238000005516 engineering process Methods 0.000 description 11
- 238000000034 method Methods 0.000 description 9
- 239000002245 particle Substances 0.000 description 8
- 230000001902 propagating effect Effects 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229960005196 titanium dioxide Drugs 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052575 non-oxide ceramic Inorganic materials 0.000 description 3
- 239000011225 non-oxide ceramic Substances 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 238000000748 compression moulding Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- OTRAYOBSWCVTIN-UHFFFAOYSA-N OB(O)O.OB(O)O.OB(O)O.OB(O)O.OB(O)O.N.N.N.N.N.N.N.N.N.N.N.N.N.N.N Chemical compound OB(O)O.OB(O)O.OB(O)O.OB(O)O.OB(O)O.N.N.N.N.N.N.N.N.N.N.N.N.N.N.N OTRAYOBSWCVTIN-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- -1 cutting tool Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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Abstract
The invention discloses a self-propagation high-temperature synthesizing preparation method of TiB2-TiC complex ceramic micropowder, which comprises the following steps of: ; uniformly mixing Ti powder and B4C powder according to the mole proportion of 3:1 and then carrying out high-energy ball milling for 3-10 hours at room temperature at the rotating speed of 1,000-2,000rpm, wherein the Ti powder and the B4C powder, with granularity of smaller than 100 meshes and purity of larger than 99 percent, are used as raw materials; then coldly pressing and moulding the ball-milled mixed powder; igniting and pressing by an electric arc in a vacuum chamber to obtain a combustion product; and finally, breaking the combustion product to obtain a TiB2-TiC complex micropowder ceramic material with the powder average grain diameter of 2-8 microns. The TiB2-TiC complex micropowder ceramic material prepared by the pure Ti powder and the B4C powder as the raw materials through ball milling and self-propagation high-temperature synthesis has the advantages of simple production process, low cost, high product yield and quality, and the like.
Description
Technical field
The invention belongs to new ceramics powdered material preparing technical field, provide a kind of with pure Ti powder and B
4The C powder is a raw material, adopts the self propagating high temperature synthesis method to prepare TiB2-titanium carbide complex phase micro mist method of ceramic material.
Background technology
TiB2 (TiB
2) have high-melting-point (3253 ℃), a low density (4.52g/cm
3), high rigidity (HV=34GPa), fabulous chemical stability and good heat conduction, conduction, wear-resisting, resistance to high temperature oxidation performances such as (can resist the oxidation below 1100 ℃), have structural ceramics and function ceramics dual purpose concurrently, be mainly used in the making conducting ceramic material, ceramic cutter and mould, composite ceramic material, the aluminium electrolytic cell cathode coated material, PTC heating stupalith and flexible PCT material, the reinforcer of metallic substance such as Al, Fe, Cu, metal matrix surface refractory, corrosion-resistant coating material.Titanium carbide (TiC) has high rigidity (HV=30GPa), high-melting-point (3160 ℃), high elastic coefficient, low heat conductivity (21W/ (mk)), chemical stability is good and the low plurality of advantages such as (60 μ Ω cm (room temperature)) of resistivity, be widely used in making high-abrasive material, cutting tool, abrasive material, mould, the smelting metal crucible, numerous areas such as powder metallurgy.TiB2 (TiB
2) and titanium carbide (TiC) be combined into the complex phase ceramic particle, have TiB
2With the composite performance of TiC, in non-oxide ceramics, superhard alloy and high-strength highly-conductive metal-base composites,, be subjected to extensive concern often as main strengthening phase.
In the traditional preparation process technology of non-oxide ceramics, superhard alloy and high-strength highly-conductive metal-base composites, all be to prepare independent TiB earlier
2With the TiC powder, by methods such as powder metallurgy these two kinds of powder are joined in the corresponding matrix then.
TiB
2The traditional preparation process technology of powder is: the mixture of titanium or titanium oxide and boron oxide or norbide and carbon is carried out the high temperature cabonization reduction, explained hereafter device complexity, temperature of reaction height, the time is long, energy consumption is huge, and the TiB2 crystal grain that obtains is thick, boron-containing quantity is low, product purity is poor.Be that reductive agent, ammonium pentaborate are that boron source and titanium dioxide are the titanium diboride ceramic powder charcoal reduction synthetic method in titanium source based on gac under Chinese patent CN105533A has reported 1450～1700 ℃, about product granularity 10 μ m, comparatively thick, and the synthesis temperature height, long reaction time.Chinese patent CN1341576A has reported that the synthetic reduction method of another kind of self propagating high temperature prepares TiB
2The method of ceramic is with TiO
2, B
2O
3With metal M g powder uniform mixing and compression molding, place the self-spreading high-temperature synthesizing device of argon shield then at normal temperatures and pressures, ignition, products of combustion obtains TiB after fragmentation, pickling
2Ceramic, median size are about 5 μ m, but preparation process is still long, complicated.
Traditional preparation technology of TiC powder is that the mixture with titanium or titanium dioxide and carbon places in the graphite tube furnace of vacuum, be heated to then and carry out carbonization more than 2200 ℃ under the high temperature, have shortcomings such as device complexity, long reaction time, energy consumption height, titanium carbide product carbon content are low, product purity difference.Many studies show that, self propagating high temperature synthesizing titanium carbide technology can overcome these shortcomings, production cost is reduced significantly, but gained titanium carbide powder particle thick (about 100 μ m), can not satisfy the commercialization titanium carbide to the requirement of particle, influence the competitive power of this technology smaller or equal to 10 μ m.1991, the Russian disclose spread certainly-hot pressing prepares the method for titanium carbide micro powder, gained titanium carbide granularity reaches 3～20 μ m, but influences suitability for industrialized production owing to process unit is too complicated.Chinese patent CN1135457A reported a kind of self propagating high temperature synthetic-chemical-reacting furnace prepares the method for titanium carbide micro powder, earlier with intermediate compound TiC
0.5The compression molding of+0.5C mixture is placed on the inside of (Ti+C) mixture; under the normal temperature and pressure argon shield, place self propagating high temperature to synthesize-chemical-reacting furnace then; ignition; make outer field (Ti+C) rapid reaction generate the TiC product of particle diameter 20～80 μ m, and utilize outer system to emit the (TiC that reaction heat makes internal layer simultaneously
0.5+ 0.5C) rapid reaction generates the TiC product of particle diameter＜10 μ m.The weak point of this technology is that preparation technology and device are complicated, and gained TiC particle is thicker, and particle is inhomogeneous.
In summary, existing TiB
2All there is technology and prepares complicated, higher, the not high weak point in various degree of quality product of cost with TiC powdered preparation technology, and all be to prepare a kind of powder separately, and then the two mixing made an addition in the body material, increased the production cost of non-oxide ceramics, superhard alloy and high-strength highly-conductive metal-base composites virtually.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, provide a kind of with pure Ti powder and B
4The C powder is a raw material, adopts the self propagating high temperature synthesis method to prepare TiB2-titanium carbide complex phase micro mist method of ceramic material, shortens operational path, reduces production costs, and improves the quality of products.
The technical scheme that the present invention prepares TiB2-titanium carbide complex phase micro mist stupalith is: all less than 100 orders, purity is all greater than 99% Ti powder and B with granularity
4The C powder is a raw material, with Ti powder and B
4The C powder carries out uniform mixing in the ratio of 3: 1 (mole), be ratio of grinding media to material 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 then, make the ball material mixture account for 10～50% of ball grinder cavity volume, at room temperature carried out high-energy ball milling 3～10 hours then with 1000～2000 rev/mins rotating speed, make mixed powder that grain refine and grain refining take place in the process in ball milling, improve even particle distribution, greatly improve powder activity, reduce reaction activity; Subsequently, with the mixed powder coldmoulding behind the ball milling; Then, electricity consumption acnode combustion pressed compact obtains products of combustion; At last, broken products of combustion obtains TiB
2-TiC complex phase micro mist stupalith, powder median size are 2～8 μ m.
The present invention is with pure Ti powder and B
4The C powder is a raw material, adopts the synthetic preparation of ball milling and self propagating high temperature TiB
2-TiC complex phase micro mist stupalith by the control to preparation technology parameter, utilizes Ti powder and pure B
4The synthetic preparation of C powder TiB
2-TiC complex phase micro mist stupalith shortens operational path, reduces production costs, and improves the quality of products, to realize TiB
2The extensive widespread use of-TiC diphase ceramic material.
Embodiment
Further specify flesh and blood of the present invention with example below, but content of the present invention is not limited to this.
Embodiment 1: be 150 orders with granularity, purity is 99.9% Ti powder and B
4The C powder is a raw material, with Ti powder and B
4The C powder is that 3: 1 ratio is carried out uniform mixing in molar ratio, be ratio of grinding media to material 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 then, make the ball material mixture account for 15% of ball grinder cavity volume, at room temperature carried out high-energy ball milling 3 hours with 1000 rev/mins rotating speed; Subsequently, the mixed powder behind the ball milling is cold-pressed into the cylindrical blank of Φ 30mm * 30mm; Then, electricity consumption acnode combustion pressed compact obtains products of combustion in vacuum chamber; At last, broken products of combustion obtains TiB
2-TiC complex phase micro mist stupalith, the powder median size is about 7.5 μ m.
Embodiment 2: be 200 orders with granularity, purity is 99.9% Ti powder and B
4The C powder is a raw material, with Ti powder and B
4The C powder carries out uniform mixing in the ratio of 3: 1 (mole), be ratio of grinding media to material 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 then, make the ball material mixture account for 25% of ball grinder cavity volume, at room temperature carried out high-energy ball milling 6 hours with 1500 rev/mins rotating speed; Subsequently, the mixed powder behind the ball milling is cold-pressed into the cylindrical blank of Φ 30mm * 30mm; Then, electricity consumption acnode combustion pressed compact obtains products of combustion in vacuum chamber; At last, broken products of combustion obtains TiB
2-TiC complex phase micro mist stupalith, the powder median size is about 4.5 μ m.
Embodiment 3: be 300 orders with granularity, purity is 99.9% Ti powder and B
4The C powder is a raw material, with Ti powder and B
4The C powder carries out uniform mixing in the ratio of 3: 1 (mole), be ratio of grinding media to material 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 then, make the ball material mixture account for 35% of ball grinder cavity volume, at room temperature carried out high-energy ball milling 9 hours with 2000 rev/mins rotating speed; Subsequently, the mixed powder behind the ball milling is cold-pressed into the cylindrical blank of Φ 30mm * 30mm; Then, electricity consumption acnode combustion pressed compact obtains products of combustion in vacuum chamber; At last, broken products of combustion obtains TiB
2-TiC complex phase micro mist stupalith, the powder median size is about 2.5 μ m.
Claims (3)
1. the self-propagating high temperature synthesis preparation method of TiB2-titanium carbide complex-phase ceramic micropowder: it is characterized in that: all less than 100 orders, purity is all greater than 99% Ti powder and B with granularity
4The C powder is a raw material, with Ti powder and B
4The C powder by behind 3: 1 mol ratio uniform mixing at room temperature the rotating speed with 1000～2000 rev/mins carried out high-energy ball milling 3～10 hours; Then, with the mixed powder coldmoulding behind the ball milling; Subsequently, electricity consumption acnode combustion pressed compact obtains products of combustion in vacuum chamber; At last, broken products of combustion obtains TiB
2-TiC complex phase micro mist stupalith.
2. the self-propagating high temperature synthesis preparation method of a kind of TiB2 according to claim 1-titanium carbide complex-phase ceramic micropowder, it is characterized in that: during described high-energy ball milling, is ratio of grinding media to material that 20～80: 1 steel ball and mixed powder are put into ball grinder in being full of the glove box of argon gas, makes the ball material mixture account for 15～35% of ball grinder cavity volume.
3. the self-propagating high temperature synthesis preparation method of a kind of TiB2 according to claim 1-titanium carbide complex-phase ceramic micropowder is characterized in that obtaining TiB
2The powder median size of-TiC complex phase micro mist stupalith is 2～8 μ m.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200910095175A CN101704678A (en) | 2009-11-11 | 2009-11-11 | Self-propagation high-temperature synthesizing preparation method of TiB2-TiC complex ceramic micropowder |
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| CN200910095175A CN101704678A (en) | 2009-11-11 | 2009-11-11 | Self-propagation high-temperature synthesizing preparation method of TiB2-TiC complex ceramic micropowder |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212729A (en) * | 2011-04-17 | 2011-10-12 | 山东科技大学 | TiB2-TiC-TiN-NiAl porous composite material with combined hole pattern and preparation method thereof |
| CN102430757A (en) * | 2011-11-25 | 2012-05-02 | 天津大学 | Method for preparing TiB2/TiC (titanium diboride/titanium carbide) ultrafine powder for surface spraying of engine piston ring by means of high energy ball milling |
| CN106431416A (en) * | 2016-09-22 | 2017-02-22 | 铜仁学院 | Zirconium carbide-zirconium diboride complex-phase ceramic powder synthesized through thermal explosion and preparation method thereof |
| CN108610052A (en) * | 2018-05-17 | 2018-10-02 | 广东工业大学 | A kind of titanium diboride base complex phase ceramic and its preparation method and application |
| CN109956754A (en) * | 2017-12-25 | 2019-07-02 | 南京理工大学 | Graphene nanometer sheet toughening TiB2Base ceramic cutting tool material and its preparation process |
| CN110592426A (en) * | 2019-08-27 | 2019-12-20 | 江苏大学 | High-hardness high-temperature-resistant TiC + TiB reinforced titanium-based composite material generated by solid-phase in-situ reaction and preparation method thereof |
| CN113880585A (en) * | 2021-10-29 | 2022-01-04 | 武汉科技大学 | Titanium boride-boron carbide composite ceramic having complex shape and method for producing same |
-
2009
- 2009-11-11 CN CN200910095175A patent/CN101704678A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212729A (en) * | 2011-04-17 | 2011-10-12 | 山东科技大学 | TiB2-TiC-TiN-NiAl porous composite material with combined hole pattern and preparation method thereof |
| CN102212729B (en) * | 2011-04-17 | 2012-10-03 | 山东科技大学 | TiB2-TiC-TiN-NiAl porous composite material with combined hole pattern and preparation method thereof |
| CN102430757A (en) * | 2011-11-25 | 2012-05-02 | 天津大学 | Method for preparing TiB2/TiC (titanium diboride/titanium carbide) ultrafine powder for surface spraying of engine piston ring by means of high energy ball milling |
| CN106431416A (en) * | 2016-09-22 | 2017-02-22 | 铜仁学院 | Zirconium carbide-zirconium diboride complex-phase ceramic powder synthesized through thermal explosion and preparation method thereof |
| CN109956754A (en) * | 2017-12-25 | 2019-07-02 | 南京理工大学 | Graphene nanometer sheet toughening TiB2Base ceramic cutting tool material and its preparation process |
| CN108610052A (en) * | 2018-05-17 | 2018-10-02 | 广东工业大学 | A kind of titanium diboride base complex phase ceramic and its preparation method and application |
| CN110592426A (en) * | 2019-08-27 | 2019-12-20 | 江苏大学 | High-hardness high-temperature-resistant TiC + TiB reinforced titanium-based composite material generated by solid-phase in-situ reaction and preparation method thereof |
| CN110592426B (en) * | 2019-08-27 | 2021-11-23 | 江苏大学 | High-hardness high-temperature-resistant TiC + TiB reinforced titanium-based composite material generated by solid-phase in-situ reaction and preparation method thereof |
| CN113880585A (en) * | 2021-10-29 | 2022-01-04 | 武汉科技大学 | Titanium boride-boron carbide composite ceramic having complex shape and method for producing same |
| CN113880585B (en) * | 2021-10-29 | 2023-10-27 | 武汉科技大学 | Titanium boride-boron carbide composite ceramic with complex shape and manufacturing method thereof |
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Application publication date: 20100512 |