CN101704674A - Method for preparing titanium diboride ceramic micro powder by self-propagation high temperature synthesis - Google Patents
Method for preparing titanium diboride ceramic micro powder by self-propagation high temperature synthesis Download PDFInfo
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- CN101704674A CN101704674A CN200910095178A CN200910095178A CN101704674A CN 101704674 A CN101704674 A CN 101704674A CN 200910095178 A CN200910095178 A CN 200910095178A CN 200910095178 A CN200910095178 A CN 200910095178A CN 101704674 A CN101704674 A CN 101704674A
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- 239000000843 powder Substances 0.000 title claims abstract description 52
- 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
- 239000000919 ceramic Substances 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title claims abstract description 14
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 7
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 7
- 239000010936 titanium Substances 0.000 claims abstract description 19
- 238000002485 combustion reaction Methods 0.000 claims abstract description 18
- 239000011812 mixed powder Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000003595 mist Substances 0.000 claims description 11
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000000713 high-energy ball milling Methods 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
- 238000007670 refining Methods 0.000 claims description 2
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000001308 synthesis method Methods 0.000 abstract description 3
- 238000010891 electric arc Methods 0.000 abstract 1
- 235000019580 granularity Nutrition 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 7
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 239000004411 aluminium Substances 0.000 description 4
- 230000001902 propagating effect Effects 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000000694 effects Effects 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
- 230000002829 reductive effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 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
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-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
- 229910052799 carbon Inorganic materials 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
- 238000000748 compression moulding Methods 0.000 description 1
- 239000000470 constituent Substances 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
- 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
- 239000002305 electric material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a method for preparing titanium diboride ceramic micro powder by adopting a self-propagation high temperature synthesis method, which uses Ti powder and B powder of which granularities are less than 100 meshes and purities are more than 99 percent as raw materials and comprises the following steps: evenly mixing the Ti powder and the B powder in a molar ratio of 1:2, and then ball-milling the mixture with high energy for 3 to 10 hours at the room temperature and at the rotating speed of 1,000 to 2,000 revolutions per minute; then, cold-pressing and molding the ball-milled mixed powder; later, igniting the pressed blank by electric arc in a vacuum chamber to obtain a combustion product; and finally, crushing the combustion product to obtain a TiB2 micro powder ceramic material, wherein the average grain diameter of the powder is 2 to 8 mu m. The method for preparing the TiB2 micro powder ceramic material by using the pure Ti powder and the pure B powder as raw materials and adopting 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, providing a kind of is raw material with pure Ti powder and B powder, adopts the self propagating high temperature synthesis method to prepare TiB2 micro mist method of ceramic material.
Background technology
TiB2 molecular formula TiB
2, be a kind of new ceramic material, have than oxide ceramics, the more excellent physicochemical property of carbide ceramics, comprising: high-melting-point (3253 ℃), 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 ℃), its goods also have higher intensity and toughness, so TiB2 has structural ceramics and function ceramics dual purpose concurrently.At present, the Application Areas of TiB2 comprises: 1) conducting ceramic material is one of main raw material of vacuum plating conductive evaporation boat; 2) ceramic cutter and mould can be made finishing tool, wortle, overflow mould, sand spit, sealing element etc.; 3) composite ceramic material can be used as the important constituent element of multi-element composite material, with TiC, TiN, materials such as SiC are formed matrix material, make various high temperature resistant components and functional component, as high-temperature crucibles, engine components etc., also be one of preferred materials of making the armor facing material; 4) aluminium electrolytic cell cathode coated material is because TiB
2The wettability good with metal aluminium liquid used TiB
2As the aluminium electrolytic cell cathode coated material, the current consumption of aluminium cell is reduced, prolong bath life; 5) being made into PTC heating stupalith and flexible PCT material, having characteristics such as safety, power saving, reliable, easy machine-shaping, is the high-tech product of a kind of update of all kinds of thermo electric materials; 6) be the good reinforcers of metallic substance such as Al, Fe, Cu; 7) can be used as metal matrix surface refractory, corrosion-resistant coating material.But, high-purity Ti B
2Preparation comparatively the difficulty, cause it to cost an arm and a leg, strictness has limited the large-scale development and the application of this material.
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 the requirement of preparation starting material is more, and preparation process is still long, complicated.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, providing a kind of is raw material with pure Ti powder and B powder, adopts the self propagating high temperature synthesis method to prepare TiB2 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 micro mist stupalith is: with granularity all less than 100 orders, purity is raw material greater than 99% Ti powder and B powder all, Ti powder and B powder are carried out uniform mixing in the ratio of 1: 2 (mole), is 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, 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 in vacuum chamber; At last, broken products of combustion obtains TiB
2Micro mist stupalith, powder median size are 2～8 μ m.
The present invention is a raw material with pure Ti powder and pure B powder, adopts the synthetic preparation of ball milling and self propagating high temperature TiB
2The micro mist stupalith has that production technique is simple, cost is low, product production and a quality advantages of higher.The present invention utilizes the synthetic preparation of Ti powder and pure B powder TiB by the control to preparation technology parameter
2The micro mist stupalith shortens operational path, reduces production costs, and improves the quality of products, to realize TiB
2The extensive widespread use of stupalith.
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, it is raw material that purity is 99.9% Ti powder and B powder, Ti powder and B powder are carried out uniform mixing in the ratio of 1: 2 mole (mole), is 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, make the ball material mixture account for 15% of ball grinder cavity volume, at room temperature carried out high-energy ball milling 3 hours then 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
2Micro mist stupalith, powder median size are 7.5 μ m.
Embodiment 2: be 200 orders with granularity, it is raw material that purity is 99.9% Ti powder and B powder, Ti powder and B powder are carried out uniform mixing in the ratio of 1: 2 (mole), is 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, make the ball material mixture account for 25% of ball grinder cavity volume, at room temperature carried out high-energy ball milling 6 hours then 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
2Micro mist stupalith, powder median size are 4.5 μ m.
Embodiment 3: be 300 orders with granularity, it is raw material that purity is 99.9% Ti powder and B powder, Ti powder and B powder are carried out uniform mixing in the ratio of 1: 2 (mole), is 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, make the ball material mixture account for 35% of ball grinder cavity volume, at room temperature carried out high-energy ball milling 9 hours then 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
2Micro mist stupalith, powder median size are 2.5 μ m.
Claims (3)
1. the method for a preparing titanium diboride ceramic micro powder by self-propagation high temperature synthesis, it is characterized in that containing following steps: with granularity all less than 100 orders, purity is raw material greater than 99% Ti powder and B powder all, Ti powder and B powder are carried out uniform mixing by 1: 2 molar ratio, is 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, make the ball material mixture account for 10～50% of ball grinder cavity volume, carry out high-energy ball milling in room temperature then, make mixed powder that grain refine and grain refining take place in the process in ball milling, subsequently, with the mixed powder coldmoulding behind the ball milling, electricity consumption acnode combustion pressed compact obtains products of combustion in vacuum chamber; At last, broken products of combustion obtains TiB
2The micro mist stupalith.
2. the method for a kind of preparing titanium diboride ceramic micro powder by self-propagation high temperature synthesis according to claim 1 is characterized in that: during described high-energy ball milling, rotating speed is 1000～2000 rev/mins, and the time is 3～10 hours.
3. the method for a kind of preparing titanium diboride ceramic micro powder by self-propagation high temperature synthesis according to claim 1 is characterized in that: described TiB
2The powder median size of micro mist stupalith is 2～8 μ m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910095178A CN101704674A (en) | 2009-11-11 | 2009-11-11 | Method for preparing titanium diboride ceramic micro powder by self-propagation high temperature synthesis |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910095178A CN101704674A (en) | 2009-11-11 | 2009-11-11 | Method for preparing titanium diboride ceramic micro powder by self-propagation high temperature synthesis |
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|---|---|
| CN101704674A true CN101704674A (en) | 2010-05-12 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891215A (en) * | 2010-07-15 | 2010-11-24 | 武汉工程大学 | Method for preparing nano titanium diboride polycrystalline powder |
| CN103265048A (en) * | 2013-06-14 | 2013-08-28 | 兰州理工大学 | Preparation method of TiB2 ultrafine powder material |
| CN104609865A (en) * | 2015-02-09 | 2015-05-13 | 广东工业大学 | Preparation method of silicon nitride-based conductive ceramic and molding method of silicon nitride-based conductive ceramic cutting tool |
| CN105439161A (en) * | 2015-07-29 | 2016-03-30 | 洛阳新巨能高热技术有限公司 | Preparation method for titanium diboride nanoparticles |
| CN109607557A (en) * | 2019-02-18 | 2019-04-12 | 北京镭硼科技有限责任公司 | A kind of high-purity titanium diboride raw powder's production technology |
| CN109896861A (en) * | 2019-04-11 | 2019-06-18 | 哈尔滨工业大学 | A kind of high-purity, the small grain size hafnium boride raw powder's production technology of resistance to ablation |
| WO2024187358A1 (en) * | 2023-03-14 | 2024-09-19 | 昆明理工大学 | Rapid preparation method for transition metal boride |
-
2009
- 2009-11-11 CN CN200910095178A patent/CN101704674A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891215A (en) * | 2010-07-15 | 2010-11-24 | 武汉工程大学 | Method for preparing nano titanium diboride polycrystalline powder |
| CN101891215B (en) * | 2010-07-15 | 2011-12-28 | 武汉工程大学 | Method for preparing nano titanium diboride polycrystalline powder |
| CN103265048A (en) * | 2013-06-14 | 2013-08-28 | 兰州理工大学 | Preparation method of TiB2 ultrafine powder material |
| CN104609865A (en) * | 2015-02-09 | 2015-05-13 | 广东工业大学 | Preparation method of silicon nitride-based conductive ceramic and molding method of silicon nitride-based conductive ceramic cutting tool |
| CN105439161A (en) * | 2015-07-29 | 2016-03-30 | 洛阳新巨能高热技术有限公司 | Preparation method for titanium diboride nanoparticles |
| CN109607557A (en) * | 2019-02-18 | 2019-04-12 | 北京镭硼科技有限责任公司 | A kind of high-purity titanium diboride raw powder's production technology |
| CN109896861A (en) * | 2019-04-11 | 2019-06-18 | 哈尔滨工业大学 | A kind of high-purity, the small grain size hafnium boride raw powder's production technology of resistance to ablation |
| WO2024187358A1 (en) * | 2023-03-14 | 2024-09-19 | 昆明理工大学 | Rapid preparation method for transition metal boride |
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Application publication date: 20100512 |