CN104177089A - Process for preparing zirconium boride based conductive ceramic evaporation boat - Google Patents
Process for preparing zirconium boride based conductive ceramic evaporation boat Download PDFInfo
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- CN104177089A CN104177089A CN201410466727.9A CN201410466727A CN104177089A CN 104177089 A CN104177089 A CN 104177089A CN 201410466727 A CN201410466727 A CN 201410466727A CN 104177089 A CN104177089 A CN 104177089A
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- zirconium boride
- based conductive
- conductive ceramics
- evaporation boat
- boron nitride
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Abstract
The invention relates to a process for preparing a zirconium boride based conductive ceramic evaporation boat and belongs to the field of preparation of ceramic materials. The process is characterized by comprising the following steps: (1) mixing raw materials in percentage by weight, namely 40-50% of zirconium boride, 5-15% of silicon carbide, 35-45% of boron nitride and 2-5% of high-temperature sintering auxiliaries, adding anhydrous ethanol, and carrying out ball milling for 1-3 days, so as to obtain uniformly-mixed material slurry; (2) evaporating to dry the material slurry on a rotary evaporator, and then, grinding, so as to obtain a mixed powdery material; (3) loading the mixed powdery material into a graphite grinding tool, of which the surface is coated with boron nitride, carrying out hot-pressed sintering at the sintering temperature of 1,900-2,000 DEG C and the pressure of 20-40MPa under an argon atmosphere, and carrying out heat preservation for 0.5-2 hours, so as to obtain zirconium boride based conductive ceramics; (4) carrying out mechanical cutting, grinding and milling on the zirconium boride based conductive ceramics, thereby obtaining the zirconium boride based conductive ceramic evaporation boat. According to the process, the preparation process is simple, and the obtained material is strong in workability and long in service life, so that the process is applicable to large-scale production.
Description
Affiliated technical field
The preparation technology who the invention provides a kind of zirconium boride 99.5004323A8ure based conductive ceramics evaporation boat, belongs to field of ceramic material preparation.
Background technology
The vacuum-evaporation industry of aluminizing has proposed following many-sided requirement to boat material: suitable electrical resistivity range and temperature coefficient of resistance; Good thermotolerance; Good resistance to sudden heating; The good corrosion of resistance to aluminium; The wettability good with aluminium liquid under high temperature; Easily machining property; Enough physical strengths etc.
In early days, evaporation boat material is graphite, but it is easily corroded by liquid aluminium, and therefore the life-span is very short.At present, conductive ceramic evaporation boat mainly contains two constituent element evaporation boat (TiB
2-BN) and three constituent element evaporation boat (TiB
2-BN-AlN).This is due to TiB
2all there is special physics and chemistry performance: TiB with BN
2there is high-melting-point, high chemical stability, high rigidity, there is again good electroconductibility and thermal conductivity simultaneously; B N has good high-temperature electric insulativity and preventing corrosion from molten metals, and the most outstanding advantage is fabulous thermal shock resistance and easy machinability, therefore selects TiB
2-BN bis-constituent elements are prepared evaporation boat, because BN can react and generate AlN formation layer protecting film with liquid aluminium, also directly adopt TiB again
2-BN-AlN tri-components are prepared evaporation boat.
But, TiB
2oxidation-resistance is undesirable.Within the scope of 120～450 DEG C, TiB
2powder is measured in TG has slight weightening finish phenomenon to occur, repeatedly circulation in this temperature range, then occur without weightening finish phenomenon, illustrate that its surface has formed one deck protective oxide layer, avoid material internal to continue oxidation.Temperature exceedes after 900～1000 DEG C, TiB
2vigorous oxidation.TiB
2the undesirable TiB that reduced of oxidation-resistance
2the work-ing life of based conductive ceramics evaporation boat.
Zirconium boride 99.5004323A8ure has high fusing point, intensity, and resistivity is that 1 μ Ω cm is less than titanium boride (14 μ Ω cm), has good electroconductibility; Oxidation-resistance is good, at 800 DEG C, and ZrB
2powder is measured without weightening finish and weightlessness and is occurred in TG, and 800～1400 DEG C, weightening finish 40%, oxidation generates B
2o
3and ZrO
2.And zirconium boride 99.5004323A8ure based conductive ceramics evaporation boat there is no report.
Summary of the invention
The object of this invention is to provide a kind ofly can overcome above-mentioned defect, technique is simple, firing temperature is low, the preparation technology of the zirconium boride 99.5004323A8ure based conductive ceramics evaporation boat of long service life, its technical scheme is:
(1) by raw material zirconium boride 99.5004323A8ure, silicon carbide, boron nitride and high temperature sintering auxiliary agent be by weight percentage: 40～50%:5～15%:35～45%:2～5% mixes, the slip that adds dehydrated alcohol ball milling to obtain mixing for 1～3 day; (2) slip evaporates oven dry on rotatory evaporator, then grinds and obtains mixed powder; (3) again mixed powder is packed in the graphite grinding tool of surface-coated boron nitride, hot pressed sintering under argon gas atmosphere, sintering temperature is 1900～2000 DEG C, insulation 0.5～2h, pressure is 20～40 MPa, obtains zirconium boride 99.5004323A8ure based conductive ceramics; (4) zirconium boride 99.5004323A8ure based conductive ceramics obtains zirconium boride 99.5004323A8ure based conductive ceramics evaporation boat through cut mechanically, mill, milling.
The preparation technology of described zirconium boride 99.5004323A8ure based conductive ceramics evaporation boat, the particle diameter of raw material zirconium boride 99.5004323A8ure is 1～5 μ m, the particle diameter of silicon carbide is 0.5～2 μ m.
The preparation technology of described zirconium boride 99.5004323A8ure based conductive ceramics evaporation boat, raw material boron nitride is sheet, and particle diameter is 0.5～5 μ m, and thickness is 50～200nm.
The preparation technology of described zirconium boride 99.5004323A8ure based conductive ceramics evaporation boat, middle high temperature sintering auxiliary agent is by Al powder and Y
2o
3in one or both mixing.
the present invention compared with prior art, has the following advantages:
1, major ingredient zirconium boride 99.5004323A8ure oxidation-resistance of the present invention is better than titanium boride, and can obviously be improved the work-ing life of zirconium boride 99.5004323A8ure based conductive ceramics evaporation boat;
2, major ingredient zirconium boride 99.5004323A8ure of the present invention has good electroconductibility, under the resistivity that meets conductive ceramic evaporation boat requires, makes the proportioning raw materials regulation range of zirconium boride 99.5004323A8ure based conductive ceramics evaporation boat large;
3, material carbon SiClx of the present invention add the sintering temperature that can reduce zirconium boride 99.5004323A8ure based conductive ceramics evaporation boat, improve the densification of material, and the anti-aluminium corrosion of the raising energy strongthener of compactness;
4, silicon carbide has good anti-aluminium liquid aggressiveness, and high temperature oxidation can generate fine and close silicon dioxide protective film, and can be improved the work-ing life of zirconium boride 99.5004323A8ure based conductive ceramics evaporation boat.
Embodiment
Embodiment 1
1, be 0.5 μ m by the silicon carbide of the zirconium boride 99.5004323A8ure of 4000 gram of 1 μ m of raw material, 1500 gram of 0.5 μ m, 4000 gram particle footpaths, the sheet boron nitride that thickness is 200nm and 500 grams of Al powder mix, the slip that adds dehydrated alcohol ball milling to obtain mixing for 1 day;
2, slip evaporates oven dry on rotatory evaporator, then grinds and obtains mixed powder;
3, again mixed powder is packed in the graphite grinding tool of surface-coated boron nitride, hot pressed sintering under argon gas atmosphere, sintering temperature is 1900 DEG C, insulation 2h, pressure is 20 MPa, obtains zirconium boride 99.5004323A8ure based conductive ceramics;
4, zirconium boride 99.5004323A8ure based conductive ceramics obtains zirconium boride 99.5004323A8ure based conductive ceramics evaporation boat through cut mechanically, mill, milling.
Embodiment 2
1, be 5 μ m by the silicon carbide of the zirconium boride 99.5004323A8ure of 5000 gram of 5 μ m of raw material, 1300 gram of 2 μ m, 3500 gram particle footpaths, the sheet boron nitride that thickness is 200nm and 200 grams of Al powder mix, the slip that adds dehydrated alcohol ball milling to obtain mixing for 3 days;
2, slip evaporates oven dry on rotatory evaporator, then grinds and obtains mixed powder;
3, again mixed powder is packed in the graphite grinding tool of surface-coated boron nitride, hot pressed sintering under argon gas atmosphere, sintering temperature is 2000 DEG C, insulation 0.5h, pressure is 40 MPa, obtains zirconium boride 99.5004323A8ure based conductive ceramics;
4, zirconium boride 99.5004323A8ure based conductive ceramics obtains zirconium boride 99.5004323A8ure based conductive ceramics evaporation boat through cut mechanically, mill, milling.
Embodiment 3
1, be 2 μ m by the silicon carbide of the zirconium boride 99.5004323A8ure of 4200 gram of 2 μ m of raw material, 1000 gram of 1 μ m, 4500 gram particle footpaths, the sheet boron nitride that thickness is 100nm, 100 grams of Al powder and 200 grams of Y
2o
3powder, mixing, the slip that adds dehydrated alcohol ball milling to obtain mixing for 2 days;
2, slip evaporates oven dry on rotatory evaporator, then grinds and obtains mixed powder;
3, again mixed powder is packed in the graphite grinding tool of surface-coated boron nitride, hot pressed sintering under argon gas atmosphere, sintering temperature is 1950 DEG C, insulation 1h, pressure is 30 MPa, obtains zirconium boride 99.5004323A8ure based conductive ceramics;
4, zirconium boride 99.5004323A8ure based conductive ceramics obtains zirconium boride 99.5004323A8ure based conductive ceramics evaporation boat through cut mechanically, mill, milling.
Embodiment 4
1, be 1 μ m by the silicon carbide of the zirconium boride 99.5004323A8ure of 5000 gram of 3 μ m of raw material, 500 gram of 0.5 μ m, 4000 gram particle footpaths, the sheet boron nitride that thickness is 50nm and 500 grams of Y
2o
3powder mixes, the slip that adds dehydrated alcohol ball milling to obtain mixing for 1 day;
2, slip evaporates oven dry on rotatory evaporator, then grinds and obtains mixed powder;
3, again mixed powder is packed in the graphite grinding tool of surface-coated boron nitride, hot pressed sintering under argon gas atmosphere, sintering temperature is 1950 DEG C, insulation 0.5h, pressure is 30 MPa, obtains zirconium boride 99.5004323A8ure based conductive ceramics;
4, zirconium boride 99.5004323A8ure based conductive ceramics obtains zirconium boride 99.5004323A8ure based conductive ceramics evaporation boat through cut mechanically, mill, milling.
Claims (4)
1. the preparation technology of a zirconium boride 99.5004323A8ure based conductive ceramics evaporation boat, it is characterized in that adopting following steps: (1) by raw material zirconium boride 99.5004323A8ure, silicon carbide, boron nitride and high temperature sintering auxiliary agent is by weight percentage: 40～50%:5～15%:35～45%:2～5% mixes, the slip that adds dehydrated alcohol ball milling to obtain mixing for 1～3 day; (2) slip evaporates oven dry on rotatory evaporator, then grinds and obtains mixed powder; (3) again mixed powder is packed in the graphite grinding tool of surface-coated boron nitride, hot pressed sintering under argon gas atmosphere, sintering temperature is 1900～2000 DEG C, insulation 0.5～2h, pressure is 20～40 MPa, obtains zirconium boride 99.5004323A8ure based conductive ceramics; (4) zirconium boride 99.5004323A8ure based conductive ceramics obtains zirconium boride 99.5004323A8ure based conductive ceramics evaporation boat through cut mechanically, mill, milling.
2. the preparation technology of zirconium boride 99.5004323A8ure based conductive ceramics evaporation boat as claimed in claim 1, is characterized in that: the particle diameter of step (1) Raw zirconium boride 99.5004323A8ure is 1～5 μ m, and the particle diameter of silicon carbide is 0.5～2 μ m.
3. the preparation technology of zirconium boride 99.5004323A8ure based conductive ceramics evaporation boat as claimed in claim 1, is characterized in that: step (1) Raw boron nitride is sheet, and particle diameter is 0.5～5 μ m, and thickness is 50～200nm.
4. the preparation technology of zirconium boride 99.5004323A8ure based conductive ceramics evaporation boat as claimed in claim 1, is characterized in that: in step (1), high temperature sintering auxiliary agent is by Al powder and Y
2o
3in one or both mixing.
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| CN201410466727.9A CN104177089A (en) | 2014-09-15 | 2014-09-15 | Process for preparing zirconium boride based conductive ceramic evaporation boat |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107746263A (en) * | 2017-11-15 | 2018-03-02 | 石婷 | A kind of Compound Ceramic Evaporator and its manufacture method |
| CN108264355A (en) * | 2018-02-05 | 2018-07-10 | 合肥市大卓电力有限责任公司 | A kind of new and effective evaporation boat semiconductive ceramic |
| CN113474313A (en) * | 2018-12-27 | 2021-10-01 | 迈图高新材料石英股份有限公司 | Ceramic composite heater including boron nitride and titanium diboride |
Citations (1)
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|---|---|---|---|---|
| CN102173831A (en) * | 2010-12-30 | 2011-09-07 | 山东理工大学 | Method for preparing lamellar zirconium boride ultrahigh-temperature ceramic through casting method |
-
2014
- 2014-09-15 CN CN201410466727.9A patent/CN104177089A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102173831A (en) * | 2010-12-30 | 2011-09-07 | 山东理工大学 | Method for preparing lamellar zirconium boride ultrahigh-temperature ceramic through casting method |
Non-Patent Citations (2)
| Title |
|---|
| HAITANGWU等: "Fabrication and properties of ZrB2–SiC–BN machinable ceramics", 《JOURNAL OF THE EUROPEAN CERAMIC SOCIETY》 * |
| 宋杰光等: "《二硼化锆陶瓷材料的研究及展望》", 《材料导报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107746263A (en) * | 2017-11-15 | 2018-03-02 | 石婷 | A kind of Compound Ceramic Evaporator and its manufacture method |
| CN108264355A (en) * | 2018-02-05 | 2018-07-10 | 合肥市大卓电力有限责任公司 | A kind of new and effective evaporation boat semiconductive ceramic |
| CN113474313A (en) * | 2018-12-27 | 2021-10-01 | 迈图高新材料石英股份有限公司 | Ceramic composite heater including boron nitride and titanium diboride |
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Application publication date: 20141203 |
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