CN105693252A - Hot-pressing technology for preparing boride sputtering target material - Google Patents

Hot-pressing technology for preparing boride sputtering target material Download PDF

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CN105693252A
CN105693252A CN201610045617.4A CN201610045617A CN105693252A CN 105693252 A CN105693252 A CN 105693252A CN 201610045617 A CN201610045617 A CN 201610045617A CN 105693252 A CN105693252 A CN 105693252A
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boride
graphite jig
temperature
target material
particle
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CN105693252B (en
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贾泽夏
庄志杰
顾宗慧
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Mike Material Technology (suzhou) Co Ltd
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Mike Material Technology (suzhou) Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/5805—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides
    • C04B35/58064—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides
    • C04B35/58071—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides based on titanium borides
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/5805—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides
    • C04B35/58064—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides
    • C04B35/58078—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides based on zirconium or hafnium borides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • C04B35/645—Pressure sintering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
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  • Organic Chemistry (AREA)
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Abstract

The invention relates to a hot-pressing technology for preparing a boride sputtering target material. A preparation method sequentially comprises the following process steps of pulverizing boride with the purity being larger than or equal to 99.9 percent and the particle size being less than or equal to 5mum to be boride particles with the diameter being 1 to 3mm; filling in a graphite jig; loading in a hot-pressing furnace; warming and pressurizing; after keeping warm for 5 to 10h, cooling to form a workblank; obtaining a finished product through machining, wherein the relative density is 85 percent to 90 percent, and the electrical resistivity is 1.0 to 3.5 ohm.cm; the boride powder forms compact blocks at high temperature and high pressure, so that the compact blocks are high in relative density, low in electrical resistivity, good in uniformity, high in stability and favorable in sputtering performance, and meets the usage requirements of the target material. The preparation method is simple and easy to implement, the complicated mold design required by adopting a traditional powder metallurgy pressing method is avoided, the molding efficiency is greatly improved, and the obtained target material is excellent in sputtering performance, less in impurities, and suitable for sputtering coatings.

Description

Heat pressing process prepares boride sputtering target material
Technical field
The present invention relates to the C04B pottery in IPC classification or C23C sputtering method coating technology, especially heat pressing process prepares boride sputtering target material。
Background technology
Boride and corresponding carbide, in field of new, receive publicity and try hard to these materials for producing cemented tungsten carbide cutters coating, and to reach wear-resisting purpose, the achievement up to the present obtained is still very limited。
Owing in boride, boron atom covalence key-like becomes network, the electron transfer of boron atom has arrived in metal lattice, make boride inertia very strong, stable chemical performance, and therefore in protective coating etc., show the excellent application effect such as high rigidity, high-melting-point, low-resistivity。Most of boride coating are that CVD is produced, but adopt direct evaporation method, reactive sputtering and direct sputtering method also can produce boride film。Boride film is coated on different matrix surfaces, has broad application prospects in the field such as wear-resisting, anti-corrosion, high temperature resistance, microelectronics。
Typical several boride has titanium boride (TiB2), zirconium boride (ZrB2), boronation thallium (TaB2) etc.。Wherein, PVD method and CVD the ZrB produced2All have been reported, TaB2Coating is only capable of adopting CVD to produce, blocks TaB2Hardness number be 2500kgf mm-2。The ZrB produced by CVD2The hardness number of film and the hardness number of block materials are very close to, but, ZrB2Compare TiB2Slightly soft, and corrosion resistance is better。For cavitation erosion, seriously corroded, operating temperature is significantly high, and working condition requires harsh engineer applied operating mode, TiB2The physicochemical property of a series of excellences such as have hardness height, fusing point is high, conductivity high and thermal conductivity is high, chemical stability is excellent, is a kind of compound-material with better prospect。
The technique that boride sputtering target material is prepared in current research is less, and restriction boride target is fast-developing。
In prior art, existing a kind of TiB2Preparation of coatings technology, namely with diborane for raw material, by CVD, is adopted direct evaporation legal system to take TiB by fusing agglomerate2Coating, this TiB2Coating is for the face coat of HSC Milling Tools and screw tool, although, there is good Wear vesistance, but technique is more backward, coating quality and performance efficiency are restricted。
One of technology as the exhibition of newly setting out, hot-pressing technique is also improved in research and development。Published Chinese patent application there is a small amount of document record relevant knowledge。
Chinese patent application 200510109055.7 discloses the Thermocompressed sintering and forming method of a kind of large size ceramic sputtering target material, and its method step is as follows: A) weigh the powder material making target；B) by the selected mould with diameter of the diametric requirements making target；C) mould is put in the hot pressing furnace body of heater of upper pressurization, fixing push-down head datum level；D) adopt the charging of Vibrating funnel method, measure and ensure that in mould, the powder body piling height of each local is identical；E) hot pressing supplementary protection atmosphere, starts press, starts pressurization, makes seaming chuck start to move down, and heat-insulation pressure keeping 20MIN-60MIN under temperature 650 DEG C～2100 DEG C, pressure 15～40MPA environment, until target relative density reaches design load；F) adopt additional pressurize technique pressurize, prepare the sintered body of sputtering target material further。
Chinese patent application 200680054798.1 disperses the reflectance coating by least one Compound Phase formed in aluminum, magnesium, stannum, zinc, indium, titanium, zirconium, manganese, the nitride of silicon, oxide, composite oxides, nitrogen oxides, carbide, sulfide, chloride, silicide except silicon, fluoride, boride, hydride, phosphide, selenides, tellurides or the thin film of transflective film in by silver or the substrate that formed of silver alloy。Except aluminum etc., this thin film can also comprise at least one in silver, gallium, palladium, the nitride of copper, oxide, composite oxides, nitrogen oxides, carbide, sulfide, chloride, silicide, fluoride, boride, hydride, phosphide, selenides, tellurides。
The boride powder possessing above character can prepare into sputtering target material by heat pressing process。Heat pressing process is to utilize High Temperature High Pressure by powder briquet so that it is molding and have high relative density, meets target performance requirement。Experiments verify that; boride sputtering target material is prepared by boride powder; being formed boride coating by boride target as sputter, wherein, boride powder realizes high temperature high pressure process under vacuum or inert gas shielding environment; the isolation layer of shaped cavity inner surface plating 0.2mm; but mould of getting along well under the high temperature of 2000 DEG C～2400 DEG C reacts, and boride powder obtains the pottery of densification under 30～100MPa, and its relative density is more than 85%; and, do not produce adhesion with mould。But, the deficiency existed based on existing process aspect is still difficult to overcome, including: the boride powder cost of raw material is high, and is difficult to sintering densification, and the target relative density prepared is relatively low；Simultaneously, it is impossible to the target that preparation size is relatively larger, large area target easily ftractures in preparation process, and, target unstable properties, the thermal shock resistance under thermal shock environments is poor。
Summary of the invention
It is an object of the invention to provide a kind of heat pressing process and prepare boride sputtering target material, it is proposed to a kind of defect for prior art existence and not enough solution so that boride powder obtains compact block at high temperature under high pressure, and not easily reacts with other moulds。
The purpose of the present invention will be realized by techniques below measure: the preparation method process step of boride sputtering target material is followed successively by: the boride powder of purity >=99.9%, granularity≤5 μm is made the boride particle that diameter is 1～3mm；Inserting in graphite jig, reinstall hot pressing furnace, heat up pressurization, and after insulation 5～10h, then blank is made in cooling, prepares finished product after machining, and relative density is 85%～90%, and resistivity is 1.0～3.5 Ω；Specifically comprise the steps of
1. granulate: by the boride powder of purity >=99.9%, granularity≤5 μm, after quality inspection is qualified, re-uses Granulation Equipments and powder body is made the boride particle that diameter is 1～3mm；
2. die-filling: resistant to elevated temperatures graphite jig is arranged in plant equipment, boride particle is inserted in graphite jig, and uses machinery jolt ramming；
3. shove charge: the graphite jig of boride particle jolt ramming will be filled from taking off plant equipment and loading in vacuum hotpressing stove；
4. heat up pressurization: vacuum hotpressing stove carries out the pressurization that heats up, and when temperature is 0～1500 DEG C, programming rate is 5～10 DEG C/min, and after temperature reaches 1500 DEG C, programming rate is 1～4 DEG C/min, and maximum temperature is 2000 DEG C, applies pressure 30～100MPa；The a small amount of boride powder parsed from boride particle plates the isolation layer of 0.2mm at High Temperature High Pressure shaped cavity inner surface, stops boride particle and mould to react and adhesion；
5. after insulation 5～10h, then the 10～15h that lowers the temperature, after being brought down below 200 DEG C from the highest temperature, graphite jig is taken out from vacuum hotpressing stove, stand and be cooled to room temperature, from graphite jig, take out in type boride target blank；
6. boride target blank is carried out surface finish class machining, obtain boride sputtering target material finished product。
Advantages of the present invention and effect: make boride powder obtain compact block at high temperature under high pressure so that it is to have high relative density, low-resistivity, and uniformity good, stability is high, has good sputtering performance, meets target user demand。This preparation method is simple, it is to avoid adopting the complicated die design that prior powder metallurgy drawing method needs, drastically increase shaping efficiency, gained target as sputter function admirable, impurity is few, it is adaptable to sputter coating。
Accompanying drawing explanation
Fig. 1 is the preparation method step schematic diagram in the embodiment of the present invention 1。
Detailed description of the invention
The present invention prepares the preparation method process step of boride sputtering target material by heat pressing process be followed successively by: granulate, die-filling, load hot pressing furnace, heat up pressurization, blank, machining, finished product；Specifically comprise the steps of
7. granulate: by the boride powder of purity >=99.9%, granularity≤5 μm, after quality inspection is qualified, re-uses Granulation Equipments and powder body is made the boride particle that diameter is 1～3mm；
8. die-filling: resistant to elevated temperatures graphite jig is arranged in plant equipment, boride particle is inserted in graphite jig, and uses machinery jolt ramming；
9. shove charge: the graphite jig of boride particle jolt ramming will be filled from taking off plant equipment and loading in vacuum hotpressing stove；
10. heat up pressurization: vacuum hotpressing stove carries out the pressurization that heats up, and when temperature is 0～1500 DEG C, programming rate is 5～10 DEG C/min, and after temperature reaches 1500 DEG C, programming rate is 1～4 DEG C/min, and maximum temperature is 2000 DEG C, applies pressure 30～100MPa；The a small amount of boride powder parsed from boride particle plates the isolation layer of 0.2mm at High Temperature High Pressure shaped cavity inner surface, stops boride particle and mould to react and adhesion；
After 11 insulation 5～10h, then the 10～15h that lowers the temperature, after being brought down below 200 DEG C from the highest temperature, graphite jig is taken out from vacuum hotpressing stove, stand and be cooled to room temperature, from graphite jig, take out in type boride target blank；
12 pairs of boride target blanks carry out surface finish class machining, obtain boride sputtering target material finished product。
Below in conjunction with drawings and Examples, the invention will be further described。
Embodiment 1: as shown in Figure 1, is 99.95% by purity, and granularity is the TiB of 4 μm2Powder, after quality inspection is qualified, re-uses Granulation Equipments by TiB2Powder body makes the TiB that diameter is 2mm2Particle；Resistant to elevated temperatures graphite jig is arranged in plant equipment, by TiB2Particle is inserted in graphite jig, and graphite jig is sized to 106 × 96 × 220mm, and die head is sized to 104 × 94 × 220mm, and uses machinery jolt ramming；TiB will be filled2The graphite jig of particle jolt ramming takes off plant equipment and loads in vacuum hotpressing stove；Vacuum hotpressing stove carries out the pressurization that heats up, and arranging maximum temperature is 2000 DEG C, and when temperature is 0～1500 DEG C, programming rate is 5 DEG C/min, and when temperature is after 1500 DEG C～2000 DEG C, programming rate is 2 DEG C/min, applies pressure 50MPa；After insulation 5h, lowering the temperature 10h with the cooling rate of 2 DEG C/min again, is taken out by graphite jig after being down to 200 DEG C from vacuum hotpressing stove, standing is cooled to room temperature, takes out molded TiB from graphite jig2Target blank；To TiB2Target blank is machined out, and obtains TiB2Sputtering target material finished product；Test to obtain TiB2Sputtering target material finished product relative density is 86.7%, and resistivity is 3.31 Ω。
Embodiment 2: be 99.9% by purity, granularity is the ZrB of 3 μm2Re-use Granulation Equipments after powder quality inspection is qualified and make the particle that diameter is 3mm；Resistant to elevated temperatures graphite jig is arranged in plant equipment, by ZrB2Particle is inserted in graphite jig, and uses machinery jolt ramming；ZrB will be filled2The graphite jig of particle jolt ramming takes off plant equipment and loads in vacuum hotpressing stove；Vacuum hotpressing stove carries out the pressurization that heats up, and arranging maximum temperature is 1800 DEG C, and when temperature is 0～1500 DEG C, programming rate is 6 DEG C/min, and when temperature is after 1500 DEG C～1800 DEG C, programming rate is 1 DEG C/min, applies pressure 60MPa；After insulation 6h, lowering the temperature 15h with the cooling rate of 1 DEG C/min again, is taken out by graphite jig after being down to 200 DEG C from vacuum hotpressing stove, standing is cooled to room temperature, takes out molded ZrB from graphite jig2Target blank；To molded ZrB2Target blank is machined out, and obtains ZrB2Sputtering target material finished product；Test to obtain ZrB2Sputtering target material finished product relative density is 88%, and resistivity is 1.35 Ω。
The above is the preferred embodiment of the present invention, and it is not intended that limiting the scope of the invention。

Claims (3)

1. heat pressing process prepares boride sputtering target material, it is characterised in that the preparation method process step of boride sputtering target material is followed successively by: the boride powder of purity >=99.9%, granularity≤5 μm is made the boride particle that diameter is 1～3mm；Inserting in graphite jig, reinstall hot pressing furnace, heat up pressurization, and after insulation 5～10h, then blank is made in cooling, prepares finished product after machining, and relative density is 85%～90%, and resistivity is 1.0～3.5 Ω；Specifically comprise the steps of
1. granulate: by the boride powder of purity >=99.9%, granularity≤5 μm, after quality inspection is qualified, re-uses Granulation Equipments and powder body is made the boride particle that diameter is 1～3mm；
2. die-filling: resistant to elevated temperatures graphite jig is arranged in plant equipment, boride particle is inserted in graphite jig, and uses machinery jolt ramming；
3. shove charge: the graphite jig of boride particle jolt ramming will be filled from taking off plant equipment and loading in vacuum hotpressing stove；
4. heat up pressurization: vacuum hotpressing stove carries out the pressurization that heats up, and when temperature is 0～1500 DEG C, programming rate is 5～10 DEG C/min, and after temperature reaches 1500 DEG C, programming rate is 1～4 DEG C/min, and maximum temperature is 2000 DEG C, applies pressure 30～100MPa；The a small amount of boride powder parsed from boride particle plates the isolation layer of 0.2mm at High Temperature High Pressure shaped cavity inner surface, stops boride particle and mould to react and adhesion；
5. after insulation 5～10h, then the 10～15h that lowers the temperature, after being brought down below 200 DEG C from the highest temperature, graphite jig is taken out from vacuum hotpressing stove, stand and be cooled to room temperature, from graphite jig, take out in type boride target blank；
6. boride target blank is carried out surface finish class machining, obtain boride sputtering target material finished product。
2. heat pressing process as claimed in claim 1 prepares boride sputtering target material, it is characterised in that be 99.95% by purity, and granularity is the TiB of 4 μm2Powder, after quality inspection is qualified, re-uses Granulation Equipments by TiB2Powder body makes the TiB that diameter is 2mm2Particle；Resistant to elevated temperatures graphite jig is arranged in plant equipment, by TiB2Particle is inserted in graphite jig, and graphite jig is sized to 106 × 96 × 220mm, and die head is sized to 104 × 94 × 220mm, and uses machinery jolt ramming；TiB will be filled2The graphite jig of particle jolt ramming takes off plant equipment and loads in vacuum hotpressing stove；Vacuum hotpressing stove carries out the pressurization that heats up, and arranging maximum temperature is 2000 DEG C, and when temperature is 0～1500 DEG C, programming rate is 5 DEG C/min, and when temperature is after 1500 DEG C～2000 DEG C, programming rate is 2 DEG C/min, applies pressure 50MPa；After insulation 5h, lowering the temperature 10h with the cooling rate of 2 DEG C/min again, is taken out by graphite jig after being down to 200 DEG C from vacuum hotpressing stove, standing is cooled to room temperature, takes out molded TiB from graphite jig2Target blank；To TiB2Target blank is machined out, and obtains TiB2Sputtering target material finished product；Test to obtain TiB2Sputtering target material finished product relative density is 86.7%, and resistivity is 3.31 Ω。
3. heat pressing process as claimed in claim 1 prepares boride sputtering target material, it is characterised in that be 99.9% by purity, and granularity is the ZrB of 3 μm2Re-use Granulation Equipments after powder quality inspection is qualified and make the particle that diameter is 3mm；Resistant to elevated temperatures graphite jig is arranged in plant equipment, by ZrB2Particle is inserted in graphite jig, and uses machinery jolt ramming；ZrB will be filled2The graphite jig of particle jolt ramming takes off plant equipment and loads in vacuum hotpressing stove；Vacuum hotpressing stove carries out the pressurization that heats up, and arranging maximum temperature is 1800 DEG C, and when temperature is 0～1500 DEG C, programming rate is 6 DEG C/min, and when temperature is after 1500 DEG C～1800 DEG C, programming rate is 1 DEG C/min, applies pressure 60MPa；After insulation 6h, lowering the temperature 15h with the cooling rate of 1 DEG C/min again, is taken out by graphite jig after being down to 200 DEG C from vacuum hotpressing stove, standing is cooled to room temperature, takes out molded ZrB from graphite jig2Target blank；To molded ZrB2Target blank is machined out, and obtains ZrB2Sputtering target material finished product；Test to obtain ZrB2Sputtering target material finished product relative density is 88%, and resistivity is 1.35 Ω。
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CN106222618A (en) * 2016-08-29 2016-12-14 基迈克材料科技（苏州）有限公司 SnO2the preparation method of doping ZnO sputtering target material
CN106380193A (en) * 2016-08-29 2017-02-08 基迈克材料科技（苏州）有限公司 Preparation method of MgO-doped ZnO sputtering target material
CN106588023A (en) * 2016-12-27 2017-04-26 北京有色金属研究总院 Preparation method and application for 10B enriched ZrB2 sputtering target material
CN107746280A (en) * 2017-08-31 2018-03-02 北京安泰六九新材料科技有限公司 A kind of high-compactness TiB2The preparation method of ceramic target
CN108220894A (en) * 2017-12-29 2018-06-29 清远先导材料有限公司 Target Preparation equipment
CN112236541A (en) * 2018-04-20 2021-01-15 普兰西复合材料有限公司 Target and method for producing target
CN113773084A (en) * 2021-09-08 2021-12-10 宁波江丰电子材料股份有限公司 Tungsten carbide target material for decorative coating and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101468918A (en) * 2007-12-28 2009-07-01 北京有色金属研究总院 High purity zirconium boride / hafnium boride and preparation of superhigh temperature ceramic target material
CN102869807A (en) * 2010-05-04 2013-01-09 攀时欧洲公司 Titanium diboride target
CN105018890A (en) * 2015-08-17 2015-11-04 基迈克材料科技（苏州）有限公司 TiB2 direct-current magnetron sputtering coating target prepared through vacuum gas shield pressure sintering

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101468918A (en) * 2007-12-28 2009-07-01 北京有色金属研究总院 High purity zirconium boride / hafnium boride and preparation of superhigh temperature ceramic target material
CN102869807A (en) * 2010-05-04 2013-01-09 攀时欧洲公司 Titanium diboride target
CN105018890A (en) * 2015-08-17 2015-11-04 基迈克材料科技（苏州）有限公司 TiB2 direct-current magnetron sputtering coating target prepared through vacuum gas shield pressure sintering

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106222618A (en) * 2016-08-29 2016-12-14 基迈克材料科技（苏州）有限公司 SnO2the preparation method of doping ZnO sputtering target material
CN106380193A (en) * 2016-08-29 2017-02-08 基迈克材料科技（苏州）有限公司 Preparation method of MgO-doped ZnO sputtering target material
CN106222618B (en) * 2016-08-29 2018-12-18 基迈克材料科技（苏州）有限公司 The preparation method of SnO2 doping ZnO sputtering target material
CN106588023A (en) * 2016-12-27 2017-04-26 北京有色金属研究总院 Preparation method and application for 10B enriched ZrB2 sputtering target material
CN107746280A (en) * 2017-08-31 2018-03-02 北京安泰六九新材料科技有限公司 A kind of high-compactness TiB2The preparation method of ceramic target
CN107746280B (en) * 2017-08-31 2020-07-07 北京安泰六九新材料科技有限公司 High-density TiB2Preparation method of ceramic target material
CN108220894A (en) * 2017-12-29 2018-06-29 清远先导材料有限公司 Target Preparation equipment
CN108220894B (en) * 2017-12-29 2020-03-13 清远先导材料有限公司 Target material preparation equipment
CN112236541A (en) * 2018-04-20 2021-01-15 普兰西复合材料有限公司 Target and method for producing target
CN113773084A (en) * 2021-09-08 2021-12-10 宁波江丰电子材料股份有限公司 Tungsten carbide target material for decorative coating and preparation method thereof

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