CN101468918A - 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 PDF

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CN101468918A
CN101468918A CNA2007103044656A CN200710304465A CN101468918A CN 101468918 A CN101468918 A CN 101468918A CN A2007103044656 A CNA2007103044656 A CN A2007103044656A CN 200710304465 A CN200710304465 A CN 200710304465A CN 101468918 A CN101468918 A CN 101468918A
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powder
boride
purity
temperature
zirconium
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CN101468918B (en
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储茂友
王星明
邓世斌
韩沧
张碧田
段华英
张明贤
龚述荣
潘德明
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GRINM Resources and Environment Technology Co Ltd
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Beijing General Research Institute for Non Ferrous Metals
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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

The preparation method of boride with high purity zirconium/hafnium boride powder and superhigh temperature ceramic target material thereof
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 class pottery: because they have high-melting-point, high strength, high rigidity, good unique characteristics such as anti-oxidant and flame retardant properties, be widely used in technical fields such as aerospace, this class 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 have all been obtained in actual applications 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, at present the industrial ZrB that makes 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 high strength.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 metal oxide, 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, the product component complexity, and byproduct 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 byproduct to be difficult to remove in the product that utilizes this method to prepare equally, reduced the purity of product.
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
At the deficiencies in the prior art and defective, 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 as follows: 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, adopt the self propagating high temperature synthesis technique again, make boride with high purity zirconium (ZrB 2)/hafnium boride (HfB 2) powder.
The described boride with high purity zirconium ZrB that makes 2/ hafnium boride HfB 2The purity of powder is greater than 99.5%.
The performing step of described 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, with the repressed slightly formation blank of mixed powder, 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, and question response takes out reaction product after finishing the system cooling, 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 as follows: with the described zirconium boride 99.5004323A8ure of making/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 described method are as follows:
(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) described target blank is carried out machinery and electromachining, cleaning, obtain superhigh temperature ceramic target material.
The relative density of the boride with high purity zirconium/hafnium boride superhigh temperature ceramic target material of described 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 mixing poor effect because B powder and metal powder density differ too big, 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, the purity height, 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 relative 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, provide assurance.
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 as follows:
(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, and high-purity B powder (purity is 99%) is pressed the ratio weighing in Hf:B atomic ratio 1.01:2 of Zr:B atomic ratio 1.03:2 and wet Hf powder with wet Zr powder respectively.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, with the repressed slightly formation blank of mixed powder, 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, and question response takes out reaction product after finishing the system cooling, 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; 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, 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 example summary of the invention is further elaborated
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 1.03:2 wet mixing, dry 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 question response takes out reaction product after finishing the system cooling, 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, relative 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, relative 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 1.01:2 wet mixing, dry 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 question response takes out reaction product after finishing the system cooling, 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, relative 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, relative density is near 98%.
Above embodiment sets forth principle of the present invention and embodiment with specific case, 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 all can change in specific embodiments and applications, in sum, this description should not be construed as limitation of the present invention.

Claims (6)

1. the preparation method of boride with high purity zirconium/hafnium boride powder, the process of its realization is as follows: 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, adopt the self propagating high temperature synthesis technique again, make boride with high purity zirconium ZrB2/ hafnium boride HfB2 powder.
2. according to the preparation method of right 1 described boride with high purity zirconium, hafnium boride powder, it is characterized in that the described boride with high purity zirconium ZrB that makes 2/ hafnium boride HfB 2The purity of powder is higher than 99.5%.
3. according to the preparation method of right 1 described boride with high purity zirconium and hafnium boride powder, it is characterized in that the performing step of described method is specific as follows:
(1) to press atomic ratio respectively 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, with the repressed slightly formation blank of mixed powder, is positioned in the plumbago crucible;
(3) 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, and question response takes out reaction product after finishing the system cooling, and the product fragmentation is promptly obtained required zirconium boride 99.5004323A8ure ZrB 2/ hafnium boride HfB 2Powder.
4. the preparation method of a superhigh temperature ceramic target material, it is characterized in that, the process of its realization is as follows: with the described zirconium boride 99.5004323A8ure of making/hafnium boride powder is raw material, adopt hot-pressing sintering technique, do not add any additives in the described hot-pressing sintering technique, and adopt the two-part temperature in this heat pressing process, 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.
5. method according to claim 4 is characterized in that, the realization concrete steps of described method are as follows:
(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) described target blank is carried out machinery and electromachining, cleaning, obtain superhigh temperature ceramic target material.
6. method according to claim 4 is characterized in that, the relative density of the boride with high purity zirconium/hafnium boride superhigh temperature ceramic target material of described densification reaches 95~99%.
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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
CN115151358A (en) * 2019-12-24 2022-10-04 俄罗斯国立科技大学莫斯科钢铁合金研究所 Method for manufacturing ultrahigh-temperature ceramic material based on hafnium carbide and hafnium carbonitride
CN115151358B (en) * 2019-12-24 2024-05-24 俄罗斯国立科技大学莫斯科钢铁合金研究所 Method for manufacturing superhigh temperature ceramic material based on hafnium carbide and 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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