CN101468918B - High purity zirconium boride / hafnium boride and preparation of superhigh temperature ceramic target material - Google Patents
High purity zirconium boride / hafnium boride and preparation of superhigh temperature ceramic target material Download PDFInfo
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- CN101468918B CN101468918B CN2007103044656A CN200710304465A CN101468918B CN 101468918 B CN101468918 B CN 101468918B CN 2007103044656 A CN2007103044656 A CN 2007103044656A CN 200710304465 A CN200710304465 A CN 200710304465A CN 101468918 B CN101468918 B CN 101468918B
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Abstract
The invention discloses a method for preparing a high-purity ultrahigh-temperature ceramic target material which belongs to the technical field of ceramic target materials, and in particular provides a method for preparing high-purity zirconium/hafnium boride powder and a ceramic target material thereof. The method comprises the steps of taking high-purity Zr powder, Hf powder and high-purity B powder as raw materials, adopting a self-propagating method to prepare high-purity ZrB2 and HfB2 powder respectively and then adopting a high-temperature high-pressure hot-pressing molding process to prepare a high-purity dense zirconium/hafnium boride ultrahigh-temperature ceramic target material, wherein the relative density of the target material reaches 95 to 99 percent. Relative to the prior art, metal powder in the method is slightly excessive when the materials are mixed, so as to make up for the metal loss during self-propagating reaction and further guarantee the component unicity of products. Relative to pressureless sintering, the sintering temperature needed in the method is greatly lowered; in addition, as the hot-pressing process adopts two-stage temperature, blank is uniform in temperature field, so as to ensure that the target material with uniform density can be obtained in the late hot-pressing process.
Description
Technical field
The invention belongs to a kind of preparation method of high-purity superhigh temperature ceramic target material, be specially boride with high purity zirconium ZrB
2/ hafnium boride HfB
2The hot pressing preparation method of superhigh temperature ceramic target material belongs to the ceramic target technical field.
Background technology
Ultrahigh-temperature pottery (Ultra-High Temperature Ceramics; UHTCS) be such one type of pottery: because they have HMP, HS, high firmness, good unique characteristics such as anti-oxidant and flame retardant properties; Be widely used in technical fields such as aerospace, this type pottery mainly comprises ZrB
2, HfB
2, ZrC, HfC and be the composite ceramic material of principal constituent with them.Continuous progress along with modern industry; Thin film technique and thin-film material have obtained development at full speed; Still great successes in practical application, have all been obtained academicly; And become most active research field in contemporary vacuum science and technology and the Materials science, in new high-tech industry, have very important effect.ZrB
2And HfB
2The applied research of ultrahigh-temperature ceramic membrane has also obtained continuous expansion in recent years, makes ZrB in the industry at present
2And HfB
2The method of film mainly is a sputtering method, and this method need be used ZrB
2And HfB
2Target is as the raw material of plated film.
Want to make the uniform high performance thin film of composition, just require target to have high homogeneity of ingredients, high purity, high-density and HS.Simultaneously density and the high target of intensity have advantages such as conduction, thermal conductivity are good, use this target plated film, and the sputtering power of needs is little, and the rate of film build height is not easy to crack, the target long service life.
At present about preparation ZrB
2And HfB
2The report of target is also few.Traditional ZrB
2And HfB
2The preparation method of powder mainly is to be raw material with the MOX, and adopting C or B4C is reductive agent, utilizes solid state reaction, makes ZrB
2And HfB
2Powder.Though this method cost is low, technology is simple, and long reaction time, transformation efficiency are not high, and product component is complicated, and sub product is difficult to separate.Because long reaction time, the product particle can be looked bigger in addition, and powder active low is unfavorable for the preparation of later stage ceramic body.There is report to adopt metal (Zr or Hf)+B recently
2O
3+ Mg (perhaps C) is a raw material, utilizes self propagating high temperature synthetic (Self-propagating high temperature synthesis, SHS) technology, preparation ZrB
2And HfB
2Powder, this method can overcome long, shortcomings such as energy consumption is high, its lytic activity difference of industrial preparative method time.But exist the part sub product to be difficult to remove in the product that utilizes this method to prepare equally, reduced product gas purity.
Traditional ZrB
2And HfB
2The preparation method of ceramic body mainly is with ZrB
2And HfB
2Powder is a raw material, adds an amount of sintering aid, adopts high temperature pressureless sintering.The ceramic body that these class methods make because need add sintering agent, has reduced the purity of material; Because pressureless sintering is difficult to obtain the very high ceramic body of density, the intensity of ceramic body and density uniformity are all poor, are difficult to be applied to sputtering technology in addition.
Summary of the invention
To the deficiency and the defective of prior art, the purpose of this invention is to provide a kind of high-purity ZrB
2, HfB
2The preparation method of powder and target thereof.
The preparation method of a kind of boride with high purity zirconium/hafnium boride powder; The process of its realization is following: is raw material greater than high-purity zirconium powder/hafnium powder of 99.9% and purity greater than 99% high purity boron powder with purity; Zirconium powder/hafnium powder and high purity boron powder are pressed atomic ratio respectively be (1.03～1.05): 1; (1.01～1.02): 1 mixes, and adopts the self propagating high temperature synthesis technique again, processes boride with high purity zirconium (ZrB
2)/hafnium boride (HfB
2) powder.
The said boride with high purity zirconium ZrB that processes
2/ hafnium boride HfB
2The purity of powder is greater than 99.5%.
The performing step of said method is specific as follows:
(1) to press atomic ratio with boron powder (purity is greater than 99%) be (1.03～1.05) to high-purity (purity is greater than 99.9%) wet zirconium powder/wet hafnium powder: 1/ (1.01～1.02): 1 weighing;
(2) above-mentioned mixing raw material is positioned in the ball grinder, ball milling is after 3～10 hours, and it is air-dry that the starting material that mix are positioned in the drying room room temperature, behind the complete drying, mixed powder formed blank through compacting slightly, is positioned in the plumbago crucible;
(3) blank one end is connected with the W silk of portfire, puts into the vacuum reaction synthesizer, vacuum tightness is higher than 1 * 10
-1Begin during Pa to heat up, reach between 700 ℃～1000 ℃, the self propagating high temperature building-up reactions promptly takes place in the starting ignition device, after the cooling of question response completion system, takes out reaction product, and the product fragmentation is promptly obtained required zirconium boride 99.5004323A8ure ZrB
2/ hafnium boride HfB
2Powder.
A kind of preparation method of superhigh temperature ceramic target material; The process of its realization is following: with the said zirconium boride 99.5004323A8ure of processing/hafnium boride powder is raw material; Adopt hot-pressing sintering technique, do not add any additives in the described hot-pressing sintering technique, and in this heat pressing process, adopt the two-part temperature; Cryogenic vacuum sintering, pressure are 1 * 10
-1Pa, high temperature Ar protects sintering, makes fine and close boride with high purity zirconium/hafnium boride superhigh temperature ceramic target material.
The realization concrete steps of said method are following:
(1) is raw material with zirconium boride 99.5004323A8ure/hafnium boride powder, in the graphite jig of packing into, graphite jig is positioned in the hot pressing furnace, be evacuated down to 1 * 10
-1Begin during Pa to heat up, temperature reaches 1200～1300 ℃, and insulation 30min keeps system vacuum tightness to remain on about 100Pa, does not pressurize;
(2) subsequently in temperature-rise period, applying argon gas, constantly pressurization of beginning in temperature-rise period; When temperature rises between 1750～1900 ℃, pressure reaches 10～30MPa, the beginning heat-insulation pressure keeping; Behind the heat-insulation pressure keeping 1～1.5 hour; Close heating power supply and begin cooling, equitemperature is reduced to 1200～1700 ℃, the gradual slow pressure release;
(3) etc. after hot pressing furnace cools off fully, obtain zirconium boride 99.5004323A8ure/hafnium boride target blank;
(4) said target blank is carried out machinery and electromachining, cleaning, obtain superhigh temperature ceramic target material.
The specific density of the boride with high purity zirconium/hafnium boride superhigh temperature ceramic target material of said densification reaches 95～99%.
The present invention compared with prior art has following outstanding advantage:
1., the wet metal powder (Zr powder or Hf powder) that adopts the B powder and have certain moisture mixes, and can guarantee the security of mixing process, can avoid simultaneously causing doing the drawback of mixed poor effect because the B powder differs too big with metal powder density, improved mixing efficiency.
2., the metal powder ratio excessive slightly, remedied the loss of metal in the self-propagating reaction process, further guaranteed the unicity of product component.
3., the powder that utilizes this self propagating high temperature synthesis method to obtain: component is single, all is ZrB
2Or HfB
2, purity is high, ZrB
2Or HfB
2Content surpass 99.5%, powder active big, help the later stage to obtain high-purity, high fine and close ZrB
2And HfB
2Target, the target specific density reaches 95～99%.
4., adopt heat pressing process to prepare ZrB
2And HfB
2Target helps obtaining the uniform high densification of density, high-intensity ZrB
2And HfB
2Target, simultaneously with respect to pressureless sintering, needed sintering temperature also reduces greatly.
5., this heat pressing process adopts the two-part temperature; 1200～1300 ℃ of low temperature do not have the pressure vacuum heat-preserving, help further removing gas and light metal impurity in the blank, and the even temperature field of blank; For obtaining the uniform target of density in the later stage hot pressing, assurance is provided.
6., the pressurize technology in pyroprocess technology and the temperature-fall period subsequently can further improve the density of target; And can prevent in order to obtain the target of high-compactness; Raising sintering temperature simply and prolongation soaking time, and cause the excessive drawback of target grain fineness number.This technology can reach highdensity target, and the grain fineness number of target also is unlikely to excessive simultaneously.
7., the target cleaning in later stage, can remove because the water-soluble impurity of bringing in the target course of processing also can be removed the unsintered free state loose powder of part in the target, these all can destroy film quality in coating process.
Embodiment
Technological method step of the present invention is following:
(1) common high-purity Zr powder (purity is 99.9%) and Hf powder (purity is 99.9%) are to be stored in the pure water; High-purity B powder (purity is 99%) is pressed Zr with wet Zr powder respectively: B atomic ratio 1.03: 2 and wet Hf powder are in Hf: 1.01: 2 ratio weighing of B atomic ratio.Be positioned over then in the ball grinder, ball milling is after 3～10 hours, and it is air-dry that the starting material that mix are positioned in the drying room room temperature, behind the complete drying, mixed powder formed blank through compacting slightly, is positioned in the plumbago crucible.Blank one end is connected with the tungsten filament of portfire, puts into the vacuum reaction synthesizer, vacuum tightness is higher than 1 * 10
-1Begin during Pa to heat up, reach between 700 ℃～1000 ℃, the self propagating high temperature building-up reactions promptly takes place in the starting ignition device, after the cooling of question response completion system, takes out reaction product, and the product fragmentation is promptly obtained required ZrB
2And HfB
2Powder.
(2) take by weighing the resulting ZrB of a certain amount of step (1) respectively
2And HfB
2Powder in the graphite jig of the certain size specification of packing into, is positioned over graphite jig in the hot pressing furnace, is evacuated down to 1 * 10
-1Begin during Pa to heat up, temperature reaches 1200～1300 ℃, insulation 30min.This moment, system vacuum tightness remained on about 100Pa, did not pressurize; In temperature-rise period, applying argon gas begins constantly pressurization in temperature-rise period subsequently; When temperature rises between 1750～1900 ℃, pressure reaches 10～30MPa, the beginning heat-insulation pressure keeping; Behind the heat-insulation pressure keeping 1～1.5 hour; Close heating power supply and begin cooling, equitemperature is reduced to 1200～1700 ℃, the gradual slow pressure release.
(3) etc. after hot pressing furnace cools off fully, take out the ZrB that obtains
2And HfB
2Target blank carries out machinery (grinding) and electromachining (line cutting) subsequently, obtains meeting the target of dimensional requirement; Put it into again in the pure water that contains clean-out system, carry out ultrasonic cleaning, clean after 1～2 hour, change pure water and carry out ultrasonic cleaning 1～2 hour once more; After cleaning target is put into vacuum drying oven and dry, obtain the target that plated film is used at last.
Below in conjunction with instance summary of the invention is done further elaboration
Embodiment one
1. be the Zr powder (purity is 99.9%) of 30 μ m and the B powder (purity is 99%) that median size is 8 μ m with median size, it is even to press atomic ratio wet mixing in 1.03: 2, dries the back pressed compact; Put into plumbago crucible, place vacuum oven, utilize the tungsten filament igniting; The self propagating high temperature building-up reactions takes place, and after the cooling of question response completion system, takes out reaction product; After the Mechanical Crushing, obtain purity is about 50 μ m near 99.8% median size ZrB
2Powder.
2. take by weighing a certain amount of above ZrB
2Powder is positioned in the graphite jig that workpiece size is 100 * 100mm, after colding pressing, is positioned in the hot pressing furnace.Be evacuated to 1 * 10
-1Behind the Pa, begin to heat up, to 1200 ℃, insulation 30min; Heat up, fill Ar gas, pressurization subsequently simultaneously, be warming up to 1750 ℃, pressure is 20 tons, and heat-insulation pressure keeping was closed heating power supply after 2 hours, begins cooling, and temperature is reduced to 1500 ℃, and the beginning pressure release was cooled off after 12 hours, and temperature is reduced to 70 ℃, discharging in the stove.Subsequently blank is carried out ground finish, clean vacuum drying.The purity check of target is greater than 99.5%, and density is 5.5g/cm
3, specific density is greater than 90%.
Embodiment two
Take by weighing the ZrB that same amount embodiment one makes
2Powder is positioned in the graphite jig that workpiece size is 100 * 100mm, after colding pressing, is positioned in the hot pressing furnace.Be evacuated to 1 * 10
-1Behind the Pa, begin to heat up, to 1200 ℃, insulation 30min; Heat up, fill Ar gas, pressurization subsequently simultaneously, be warming up to 1850 ℃, pressure is 30 tons, and heat-insulation pressure keeping was closed heating power supply after 2 hours, begins cooling, and temperature is reduced to 1400 ℃, and the beginning pressure release was cooled off after 13 hours, and temperature is reduced to 70 ℃, discharging in the stove.Subsequently blank is carried out ground finish, clean vacuum drying.The purity check of target is greater than 99.5%, and density is greater than 6.0g/cm
3, specific density is greater than 98%.
Embodiment three
1. be the Hf powder (purity is 99.9%) of 50 μ m and the B powder (purity is 99%) of 8 μ m with median size, it is even to press atomic ratio wet mixing in 1.01: 2, dries the back pressed compact; Put into plumbago crucible, place vacuum oven, utilize the igniting of W silk; The self propagating high temperature building-up reactions takes place, and after the cooling of question response completion system, takes out reaction product; After the Mechanical Crushing, obtain purity is about 70 μ m near 99.8% median size HfB
2Powder.
2. take by weighing a certain amount of above HfB
2Powder is positioned in the graphite jig that workpiece size is 100 * 100mm, after colding pressing, is positioned in the hot pressing furnace.Be evacuated to 1 * 10
-1Behind the Pa, begin to heat up, to 1300 ℃, insulation 30min; Heat up, fill Ar gas, pressurization subsequently simultaneously, be warming up to 1800 ℃, pressure is 20 tons, and heat-insulation pressure keeping was closed heating power supply after 2 hours, begins cooling, and temperature is reduced to 1500 ℃, and the beginning pressure release was cooled off after 12 hours, and temperature is reduced to 70 ℃, discharging in the stove.Subsequently blank is carried out ground finish, clean vacuum drying.The purity check of target is greater than 99.5%, and density is 10.1g/cm
3, specific density is greater than 90%.
Embodiment four
Take by weighing the HfB that same amount embodiment three makes
2Powder is positioned in the graphite jig that workpiece size is 100 * 100mm, after colding pressing, is positioned in the hot pressing furnace.Be evacuated to 1 * 10
-1Behind the Pa, begin to heat up, to 1300 ℃, insulation 30min; Heat up, fill Ar gas, pressurization subsequently simultaneously, be warming up to 1900 ℃, pressure is 30 tons, and heat-insulation pressure keeping was closed heating power supply after 2 hours, begins cooling, and temperature is reduced to 1400 ℃, and the beginning pressure release was cooled off after 13 hours, and temperature is reduced to 70 ℃, discharging in the stove.Subsequently blank is carried out ground finish, clean vacuum drying.The purity check of target is greater than 99.5%, and density is greater than 11.0g/cm
3, specific density is near 98%.
Above embodiment sets forth principle of the present invention and embodiment with concrete example, just is used for helping to understand method of the present invention and core concept thereof; Simultaneously, for one of ordinary skill in the art, according to thought of the present invention, the part that on embodiment and range of application, all can change, in sum, this description should not be construed as limitation of the present invention.
Claims (1)
1. the preparation method of a high-purity superhigh temperature ceramic target material is characterized in that, concrete preparation technology is following:
1) be that 99.9% high-purity Zr powder or purity are that 99.9% Hf powder is stored in the pure water with purity, with purity be high-purity B powder of 99% respectively with wet Zr powder in Zr: B atomic ratio 1.03: 2 or wet Hf powder are in Hf: 1.01: 2 ratio weighing of B atomic ratio; Be positioned over then in the ball grinder, ball milling is after 3～10 hours, and it is air-dry that the starting material that mix are positioned in the drying room room temperature, behind the complete drying, mixed powder formed blank through compacting slightly, is positioned in the plumbago crucible; Blank one end is connected with the tungsten filament of portfire, puts into the vacuum reaction synthesizer, vacuum tightness is higher than 1 * 10
-1Begin during Pa to heat up, reach between 700 ℃～1000 ℃, the self propagating high temperature building-up reactions promptly takes place in the starting ignition device, after the cooling of question response completion system, takes out reaction product, and the product fragmentation is promptly obtained required ZrB
2Powder or HfB
2Powder;
2) take by weighing the resulting ZrB of a certain amount of step (1)
2Powder or HfB
2Powder in the graphite jig of the certain size specification of packing into, is positioned over graphite jig in the hot pressing furnace, is evacuated down to 1 * 10
-1Begin during Pa to heat up, temperature reaches 1200～1300 ℃, insulation 30min; This moment, system vacuum tightness remained on 100Pa, did not pressurize; In temperature-rise period, applying argon gas begins constantly pressurization in temperature-rise period subsequently; When temperature rises between 1750～1900 ℃, pressure reaches 10～30MPa, the beginning heat-insulation pressure keeping; Behind the heat-insulation pressure keeping 1～1.5 hour; Close heating power supply and begin cooling, equitemperature is reduced to 1200～1700 ℃, the gradual slow pressure release;
3) after etc. hot pressing furnace cools off fully, take out the ZrB that obtains
2Target blank or HfB
2Target blank carries out the cutting of mechanical grinding and electromachining line subsequently, obtains meeting the target of dimensional requirement; Put it into again in the pure water that contains clean-out system, carry out ultrasonic cleaning, clean after 1～2 hour, change pure water and carry out ultrasonic cleaning 1～2 hour once more; After cleaning target is put into vacuum drying oven and dry, obtain the target that plated film is used at last.
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|---|---|---|---|
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Families Citing this family (14)
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| US9266782B2 (en) | 2010-10-29 | 2016-02-23 | Corning Incorporated | Large xenotime ceramic block and dry process for making the same |
| CN102115331B (en) * | 2011-03-14 | 2013-07-03 | 大连博恩坦科技有限公司 | 10B zirconium diboride and preparation method thereof |
| CN103205721B (en) * | 2013-03-19 | 2015-10-28 | 昆山海普电子材料有限公司 | A kind of production method of titanium-aluminium alloy target material |
| CN104418595B (en) * | 2013-08-22 | 2016-12-28 | 宁波江丰电子材料股份有限公司 | A kind of manufacture method of Sialon ceramics target |
| CN105693252B (en) * | 2016-01-22 | 2018-06-19 | 基迈克材料科技（苏州）有限公司 | Heat pressing process prepares boride sputtering target material |
| CN107879743B (en) * | 2017-09-28 | 2020-06-09 | 中国空间技术研究院 | Low-temperature sintering method of ultrahigh-temperature ceramic |
| CN108997016B (en) * | 2018-06-25 | 2021-03-26 | 广东工业大学 | Zirconium boride ceramic with high thermal conductivity and preparation method and application thereof |
| CN108546130B (en) * | 2018-07-19 | 2022-02-15 | 广东工业大学 | Ultrahigh-temperature ceramic and preparation method thereof |
| 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 |
| CN110698205B (en) * | 2019-11-19 | 2022-03-01 | 中国核动力研究设计院 | Preparation method of graphene-toughened silicon carbide ceramic |
| RU2729277C1 (en) * | 2019-12-24 | 2020-08-05 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский технологический университет "МИСиС" | Method of producing ultrahigh-temperature ceramic material based on hafnium carbonitride |
| CN113716965A (en) * | 2021-08-19 | 2021-11-30 | 中山市气相科技有限公司 | Binary eutectic target material and preparation method thereof |
| CN113814402A (en) * | 2021-10-13 | 2021-12-21 | 杭州润福春科技有限公司 | Preparation method of brake disc of heavy engineering machinery vehicle |
| CN116079055A (en) * | 2023-02-08 | 2023-05-09 | 苏州六九新材料科技有限公司 | CrAlFe-based alloy target and preparation method thereof |
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