CN104844215A - High-density ZrC ceramic target preparation method - Google Patents
High-density ZrC ceramic target preparation method Download PDFInfo
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- CN104844215A CN104844215A CN201510222022.7A CN201510222022A CN104844215A CN 104844215 A CN104844215 A CN 104844215A CN 201510222022 A CN201510222022 A CN 201510222022A CN 104844215 A CN104844215 A CN 104844215A
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Abstract
The invention discloses a high-density ZrC ceramic target preparation method. The method comprises putting a graphite grinding tool containing ZrC micro powder in a cavity of a plasma activation sintering furnace, raising the temperature to be in a range of 1800 DEG C to 1900 DEG C at a temperature raising rate ranging from 150 DEG C/min to 300 DEG C/min, preserving the temperature for 4 minutes to 6 minutes, and applying axial pressure in a range of 10MPa to 30MPa; cooling samples in the furnace to the room temperature to obtain ZrC ceramic targets. According to the method, the produced ZrC ceramic targets are single in phase and large in size the density (> 94%) is still high without adding any sintering aids, and the application prospect is quite broad.
Description
Technical field
The present invention relates to a kind of preparation method of high fine and close ZrC ceramic target.
Background technology
The aerospace field that recent country greatly develops; the fuel oil atomizer of the heat-resisting protective material of supersonic plane, rocket and various high-speed aircraft, tub and aviation and rocket engine operationally usually will stand the effect of high temperature, and this also makes ultrahigh-temperature structured material have a very wide range of applications.ZrC is a kind of common superhigh temperature ceramics, have high-melting-point, high boiling point, high rigidity, high conductivity and excellent antiacid corrosive power, and ZrC has the price of relative moderate.ZrC pottery is considered to the superhigh temperature ceramic material very with application prospect.
Because ZrC has very high fusing point, fusing point is up to 3540 DEG C, and the preparation of pure ZrC stupalith is more difficult, needs very high sintering temperature, and high sintering pressure and for a long time insulation just can prepare dense material.All that powder stock is passed through hot pressed sintering in the last few years in current report, hot isostatic pressing and self-propagating high-temperature synthesis prepare ZrC pottery, but the density of these potteries is all very low, the ceramic dense degree utilizing the zirconium powder of many granularities and carbon dust reaction sintering to obtain only has 40%, and the ZrC ceramic dense degree utilizing self-propagating high-temperature synthesis to prepare can reach 92%, but sintering temperature is up to 2440 DEG C.The people such as Sciti add sintering aid MoSi in ZrC powder
2, with the addition of the MoSi of 9vol%
2during as sintering aid, ZrC-MoSi
2density reach 99.5%, but with the addition of more MoSi
2as sintering aid, greatly reduce the purity of ZrC pottery, greatly reduce the practical application area of ZrC pottery.The large-sized ceramic block of ZrC is usually used as the target required for magnetron sputtering plating deposition, but on the market sell the density very low (60% ~ 80%) being applicable to magnetron sputtering large size pure ZrC ceramic target, be therefore badly in need of that a kind of simple and effective preparation purity is high, the novel method of high-compactness, large-sized ZrC ceramic target.
Summary of the invention
Object of the present invention is just to provide a kind of preparation method of high fine and close ZrC ceramic target, and the ZrC ceramic target purity utilizing the method to prepare is high, density is high, size is large, and can reduce its sintering temperature as far as possible.
The present invention solves its technical problem and adopts following technical scheme:
The preparation method of the fine and close ZrC ceramic target of height provided by the invention, specifically: the cavity graphite grinding tool that ZrC micro mist is housed being put into plasma activated sintering stove, 1800 ~ 1900 DEG C are warming up under an argon atmosphere with the temperature rise rate of 150 ~ 300 DEG C/min, be incubated 4 ~ 6 minutes, apply the axle pressure of 10 ~ 30MPa; Then sample cools to room temperature with the furnace, obtains described ZrC ceramic target.
The size of the ZrC ceramic target obtained by present method is Φ 50 ~ Φ 80mm.
Described ZrC ceramic target thing is mutually single.
Described ZrC ceramic target density reaches 94.4 ~ 97.5%.
Plasma activated sintering method is have employed as novel sintered technique in the present invention.Be compared to the major advantage of traditional hot-pressing sintering technique plasma activated sintering: the powder utilizing pulse high current to pass through to be applied with axle pressure makes it micro discharges occurs thus makes to have activated powder granule, next utilizes its temperature rise rate fast, the technical superiority that soaking time is short.Overcome the shortcoming that in conventional thermocompression sintering, sintering time is long, the sintering technology feature of plasma discharging can suppress the abnormal growth of crystal grain in sintering process very well and by putting a little further acceleration of sintering between particle, can obtain the fine and close ZrC ceramic block of the single height of crystal grain small structure.
ZrC ceramic target thing prepared in the present invention is mutually single, when not adulterating any sintering aid, sintering temperature is controlled in lower interval range, the ZrC pottery obtained still has very high density, as the high quality target required for deposition ZrC film, this has very important meaning for the research and development promoting ZrC film coating.
The present invention compared with prior art has following main advantage:
One. the sintering temperature adopting plasma activated sintering to prepare ZrC ceramic target decreases compared with the sintering temperature of other sintering process, and sintering temperature is only 1800 ~ 1900 DEG C, reduces power consumption required in sintering process.
They are two years old. and it is higher that preparation ZrC pottery causes target density, can reach 94.4 ~ 97.5%.
They are three years old. and do not need any sintering aid that adulterates in the ZrC ceramic target of preparation, purity reaches 99%.
Accompanying drawing explanation
Fig. 1 is that the thing of ZrC ceramic target in embodiment 1 ~ 5 is compared figure.
Fig. 2 is the micro-structure diagram of the ZrC pottery section obtained after plasma activated sintering in embodiment 1.
Fig. 3 is the micro-structure diagram of the ZrC pottery section obtained after plasma activated sintering in embodiment 2.
Fig. 4 is the micro-structure diagram of the ZrC pottery section obtained after plasma activated sintering in embodiment 3.
Fig. 5 is the micro-structure diagram of the ZrC pottery section obtained after plasma activated sintering in embodiment 4.
Fig. 6 is the micro-structure diagram of the ZrC pottery section obtained after plasma activated sintering in embodiment 5.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment.
Embodiment 1:
A preparation method for high fine and close ZrC ceramic target, it comprises the following steps:
(1) the ZrC ceramic of 39.4g is inserted in the graphite grinding tool of Φ 50mm, entirety moves in plasma activated sintering cavity, 1800 DEG C are warming up to the temperature rise rate of 150 DEG C/min in argon gas atmosphere, be incubated 4 minutes, be applied with the axle pressure of 10MPa, cool to room temperature with the furnace again, obtain ZrC ceramic target.
(2) detecting carrying out thing after ZrC ceramic target surface rubbing mutually and density test with ultra precision surface grinding machine, finally obtaining thing mutually single, density is 95.1%, ZrC ceramic target that diameter is 50mm.
Embodiment 2:
A preparation method for high fine and close ZrC ceramic target, it comprises the following steps:
(1) the ZrC ceramic of 56.8g is inserted in the graphite grinding tool of Φ 60mm, entirety moves in plasma activated sintering cavity, 1850 DEG C are warming up to the temperature rise rate of 200 DEG C/min in argon gas atmosphere, be incubated 5 minutes, be applied with the axle pressure of 10MPa, cool to room temperature with the furnace again, obtain ZrC ceramic target.
(2) detecting carrying out thing after ZrC ceramic target surface rubbing mutually and density test with ultra precision surface grinding machine, finally obtaining thing mutually single, density is 95.8%, ZrC ceramic target that diameter is 60mm.
Embodiment 3:
A preparation method for high fine and close ZrC ceramic target, it comprises the following steps:
(1) the ZrC micro mist of 77.1g is inserted in the graphite grinding tool of Φ 70mm, entirety moves in plasma activated sintering cavity, 1870 DEG C are warming up to the temperature rise rate of 300 DEG C/min in argon gas atmosphere, be incubated 6 minutes, be applied with the axle pressure of 30MPa, sample cools to room temperature with the furnace, obtains ZrC ceramic target.
(2) detecting carrying out thing after ZrC ceramic target surface rubbing mutually and density test with ultra precision surface grinding machine, finally obtaining thing mutually single, density is 97.1%, ZrC ceramic target that diameter is 70mm.
Embodiment 4:
A preparation method for high fine and close ZrC ceramic target, it comprises the following steps:
(1) the ZrC ceramic of 90.4g is inserted in the graphite grinding tool of Φ 80mm, entirety moves in plasma activated sintering cavity, 1900 DEG C are warming up to the temperature rise rate of 200 DEG C/min in argon gas atmosphere, be incubated 4 minutes, be applied with the axle pressure of 20MPa, cool to room temperature with the furnace again, obtain ZrC ceramic target.
(2) detecting carrying out thing after ZrC ceramic target surface rubbing mutually and density test with ultra precision surface grinding machine, finally obtaining thing mutually single, density is 96.4%, ZrC ceramic target that diameter is 80mm.
Embodiment 5:
A preparation method for high fine and close ZrC ceramic target, it comprises the following steps:
(1) the ZrC ceramic of 39.1g is inserted in the graphite grinding tool of Φ 50mm, entirety moves in plasma activated sintering cavity, 1900 DEG C are warming up to the temperature rise rate of 200 DEG C/min in argon gas atmosphere, be incubated 6 minutes, be applied with the axle pressure of 30MPa, cool to room temperature with the furnace again, obtain ZrC ceramic target.
(2) detecting carrying out thing after ZrC ceramic target surface rubbing mutually and density test with ultra precision surface grinding machine, finally obtaining thing mutually single, density is 97.5%, ZrC ceramic target that diameter is 50mm.
Claims (4)
1. the preparation method of one kind high fine and close ZrC ceramic target, it is characterized in that: the cavity graphite grinding tool that ZrC micro mist is housed being put into plasma activated sintering stove, 1800 ~ 1900 DEG C are warming up under an argon atmosphere with the temperature rise rate of 150 ~ 300 DEG C/min, be incubated 4 ~ 6 minutes, apply the axle pressure of 10 ~ 30MPa; Then sample cools to room temperature with the furnace, obtains described ZrC ceramic target.
2. the preparation method of the fine and close ZrC ceramic target of height according to claim 1, is characterized in that: the size of obtained ZrC ceramic target is Φ 50 ~ Φ 80mm.
3. the preparation method of the fine and close ZrC ceramic target of height according to claim 1, is characterized in that: described ZrC ceramic target thing is mutually single.
4. the preparation method of the fine and close ZrC ceramic target of height according to claim 1, is characterized in that: described ZrC ceramic target density reaches 94.4 ~ 97.5%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510222022.7A CN104844215A (en) | 2015-05-04 | 2015-05-04 | High-density ZrC ceramic target preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111548162A (en) * | 2020-04-17 | 2020-08-18 | 西安理工大学 | Method for preparing ZrC ceramic by compression molding of precursor |
| CN116023127A (en) * | 2022-12-28 | 2023-04-28 | 松山湖材料实验室 | YBCO target manufacturing method and target mold |
-
2015
- 2015-05-04 CN CN201510222022.7A patent/CN104844215A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111548162A (en) * | 2020-04-17 | 2020-08-18 | 西安理工大学 | Method for preparing ZrC ceramic by compression molding of precursor |
| CN111548162B (en) * | 2020-04-17 | 2022-06-07 | 西安理工大学 | Method for preparing ZrC ceramic by compression molding of precursor |
| CN116023127A (en) * | 2022-12-28 | 2023-04-28 | 松山湖材料实验室 | YBCO target manufacturing method and target mold |
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Application publication date: 20150819 |