CN102699325A - Preparing method for Ti-Si alloy target materials - Google Patents
Preparing method for Ti-Si alloy target materials Download PDFInfo
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- CN102699325A CN102699325A CN2012102037478A CN201210203747A CN102699325A CN 102699325 A CN102699325 A CN 102699325A CN 2012102037478 A CN2012102037478 A CN 2012102037478A CN 201210203747 A CN201210203747 A CN 201210203747A CN 102699325 A CN102699325 A CN 102699325A
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Abstract
The invention discloses a preparing method for Ti-Si alloy target materials. According to the method, silica powder and titanium powder are taken as raw materials, are mixed mechanically according to a certain proportion, filled into a graphitic mould, and are treated with vacuum induction hot pressing sintering to prepare the Ti-Si alloy target materials with different ingredients and sizes. The Ti-Si alloy target materials prepared according to the method has the advantages that the grains are fine; the ingredients are uniform; segregation is avoided; the cost is low; the density is high; and mass production is realized.
Description
Technical field
The present invention relates to field of metallurgy, specifically a kind of manufacturing approach of titanium silicon target.
Background technology
The physical vapor deposition (PVD) technology is under vacuum condition, solid material is gasificated into gaseous atom, molecule or partial ionization becomes ion, through low-pressure gas (or plasma) process, has the technology of the film of certain specific function in the matrix surface deposition.The main method of physical vapour deposition (PVD) has vapor deposition, sputter plating, ion plating.Chemical vapor deposition (CVD) also has vast application as one type of coating process; But relatively to have a technological temperature low, with short production cycle, pollution-free for PVD and CVD on the whole; And plurality of advantages such as PVD coatings surface has, and better metallic luster, thicknesses of layers are thin, hardness is high, stable chemical performance, coefficient of friction are little, it is universal in fields such as machinery, electronics, semiconductor, optics, aviation, traffic gradually.
Development along with the hard Coating Materials; (HV 2300 from initial TiN, TiC; 500 ~ 600 ℃ of application of temperature) develop into TiCN, TiAlN (HV3000,800 ℃ of application of temperature), the anti-wear performance and the application of temperature that how to improve rete become main direction of studying.When the TiSi target as sputter, feed the TiSiN hard coating that nitrogen forms; Its microhardness reaches HV3673; Serviceability temperature is 1100 ℃; The anti-mechanical wear of rete, the relative TiCN with application of temperature of wear-resistant grinding abrasion performance and TiAlN etc. improve a lot, for industries such as automobile, Aeronautics and Astronautics, heavy-duty machine provide the wear-resisting oxidation-resistant film material of excellent high-temperature more.
Magnetron sputtering prepares one of key technology of TiSiN hard film layer, provides high-quality titanium silicon target material.Titanium silicon belongs to intermetallic compound; The titanium silicon target material of existing method of smelting preparation exists shortcomings such as alloy fragility and component segregation; The silicon addition generally is no more than 15% of weight, is easy to generate cracking greater than 15% silicon addition ingot casting, is easy to generate component segregation and brittle crack less than 15% silicon addition; Alloy ductility difference also causes being difficult for cold and hot working simultaneously, so the titanium silicon target is difficult to adopt the casting method preparation.The high temperature insostatic pressing (HIP) method is because shortcomings such as high manufacturing cost and jacket selection difficulty thereof also limit its application aspect preparation titanium silicon target material.
Summary of the invention
The objective of the invention is deficiency to the prior art existence; Provide a kind of and be equipped with the method for silicotitanium target through the vacuum heating-press sintering legal system, the target that this method produces have wide composition proportion, composition evenly, tiny, the high finished product rate of segregation-free, crystal grain and characteristics cheaply.
For realizing the foregoing invention purpose, the technical scheme that the present invention adopts is a kind of manufacturing approach of titanium silicon target, may further comprise the steps:
1) place mixed powder jar to carry out mechanical mixture silica flour, titanium valve, obtain mixed-powder, mixing time is 1-16 hour;
2) take by weighing resulting mixed-powder in the step 1), in the graphite jig of packing into, then graphite jig is put into hot pressing furnace, close fire door, carry out precompressed at room temperature condition earlier, preload pressure is at 5-20MPa;
3) then vacuum system to vacuumizing in the stove; When vacuum reached 1x10-2Pa in the stove, copper induction coil energising heating mould, mixed-powder and pressure head to 465 ℃-765 ℃ were incubated 1-5 hour; Get rid of the gas of itself bringing in the powder, reduce the gas hole defect in the moulding stock; Then utilize the dual-heated of vacuum induction and resistance to make temperature be warming up to 800-1300 ℃ rapidly, heating rate 50-100 ℃/min, when reaching sintering temperature, go up push-down head and begin pressurization; Pressure is controlled at 10-80MPa; Be incubated 2-6 hour, stop heating then, shed pressure;
4) after the demoulding to be cooled, the titanium silicon target base of moulding is carried out machinery and electric machining, clean after the completion of processing, oven dry, packaging process, obtain final required titanium silicon target material.
The percentage by weight of silica flour and titanium valve is silica flour: titanium valve=1%-50%:50%-99% in the said step 1).
The titanium valve granularity is 40-83 μ m in the said step 1), and the silicon powder particle degree is 30-100 μ m.
In the said step 1) titanium valve purity more than 99.9%, silica flour purity is more than 99.9%.
It is titanium silicon target material between the 1%-50% that said method can process silicone content, and packing reaches more than 99%, the even segregation-free phenomenon of composition.
Beneficial effect: the manufacturing approach of titanium silicon target provided by the invention; Have wide composition proportion, composition evenly, tiny, the high finished product rate of segregation-free, crystal grain and advantage cheaply; Having remedied the deficiency that founding and high temperature insostatic pressing (HIP) method prepare titanium silicon target material, is optimum titanium silicon target material manufacturing approach.
Description of drawings
Fig. 1 is a vacuum hot-pressing chamber sketch map of the present invention.
The specific embodiment
Below in conjunction with specific embodiment, further illustrate the present invention, present embodiment is being to implement under the prerequisite with technical scheme of the present invention, should understand these embodiment only be used to the present invention is described and be not used in the restriction scope of the present invention.
Embodiment one: selecting purity for use is 99.9% titanium valve, and purity is 99.99% silica flour, titanium valve average particle size 42 μ m, silica flour average particle size 32 μ m, join powder by the part by weight of silicon: titanium=10:90 after, in the batch mixer of packing into, mixing time 9 hours.The powder that mixes is packed in the graphite jig, graphite jig size Ф 300x300, wall thickness 20mm puts into vacuum hotpressing stove then; Last push-down head applies 5MPa pressure and carries out precompressed, and vacuum system begins to vacuumize then, when vacuum reaches 1*10-2Pa, is warming up to 650 ℃; Be incubated 2 hours, be warming up to 1000 ℃ subsequently rapidly, 70 ℃/min of heating rate, and be forced into 10MPa; Be incubated 4 hours, stop heating, with coming out of the stove after the stove cooling, machined obtains final 90/10 titanium silicon circle target.
Embodiment two: selecting purity for use is 99.95% titanium valve, and purity is 99.99% silica flour, titanium valve average particle size 62 μ m, silica flour average particle size 40 μ m, join powder by the part by weight of silicon: titanium=30:70 after, in the batch mixer of packing into, mixing time 1 hour.The powder that mixes is packed in the graphite jig, graphite jig size Ф 350x350, wall thickness 20mm puts into vacuum hotpressing stove then; Last push-down head applies 10MPa pressure and carries out precompressed, and vacuum system begins to vacuumize then, when vacuum reaches 1*10-2Pa, is warming up to 700 ℃; Be incubated 3 hours, be warming up to 1100 ℃ subsequently rapidly, 80 ℃/min of heating rate, and be forced into 40MPa; Be incubated 2 hours, stop heating, with coming out of the stove after the stove cooling, machined obtains final 70/30 titanium silicon circle target.
Embodiment three: selecting purity for use is 99.99% titanium valve, and purity is 99.91% silica flour, titanium valve average particle size 80 μ m, silica flour average particle size 100 μ m, join powder by the part by weight of silicon: titanium=50:50 after, in the batch mixer of packing into, mixing time 7 hours.The powder that mixes is packed in the graphite jig, graphite jig size Ф 400x400, wall thickness 20mm puts into vacuum hotpressing stove then, and last push-down head applies 15MPa pressure and carries out precompressed; Vacuum system begins to vacuumize then, when vacuum reaches 1*10-2Pa, is warming up to 750 ℃, is incubated 4 hours; Be warming up to 1300 ℃ subsequently rapidly, 100 ℃/min of heating rate,, and be forced into 80MPa; Be incubated 6 hours, stop heating, with coming out of the stove after the stove cooling, machined obtains final 50/50 titanium silicon circle target.
Embodiment four: selecting purity for use is 99.95% titanium valve, and purity is 99.95% silica flour, titanium valve average particle size 70 μ m, silica flour average particle size 90 μ m, join powder by the part by weight of silicon: titanium=40:60 after, in the batch mixer of packing into, mixing time 16 hours.The powder that mixes is packed in the graphite jig, graphite jig size Ф 400x400, wall thickness 20mm puts into vacuum hotpressing stove then, and last push-down head applies 20MPa pressure and carries out precompressed; Vacuum system begins to vacuumize then, when vacuum reaches 1*10-2Pa, is warming up to 470 ℃, is incubated 5 hours; Be warming up to 800 ℃ subsequently rapidly, 90 ℃/min of heating rate,, and be forced into 30MPa; Be incubated 3 hours, stop heating, with coming out of the stove after the stove cooling, machined obtains final 60/40 titanium silicon circle target.
Embodiment five: selecting purity for use is 99.9% titanium valve, and purity is 99.9% silica flour, titanium valve average particle size 50 μ m, silica flour average particle size 50 μ m, join powder by the part by weight of silicon: titanium=45:55 after, in the batch mixer of packing into, mixing time 3 hours.The powder that mixes is packed in the graphite jig, graphite jig size Ф 400x400, wall thickness 20mm puts into vacuum hotpressing stove then, and last push-down head applies 18MPa pressure and carries out precompressed; Vacuum system begins to vacuumize then, when vacuum reaches 1*10-2Pa, is warming up to 500 ℃, is incubated 1 hour; Be warming up to 900 ℃ subsequently rapidly, 50 ℃/min of heating rate,, and be forced into 60MPa; Be incubated 5 hours, stop heating, with coming out of the stove after the stove cooling, machined obtains final 55/45 titanium silicon circle target.
Claims (4)
1. the manufacturing approach of a titanium silicon target is characterized in that may further comprise the steps:
1) place mixed powder jar to carry out mechanical mixture silica flour, titanium valve, obtain mixed-powder, mixing time is 1-16 hour;
2) take by weighing resulting mixed-powder in the step 1), in the graphite jig of packing into, then graphite jig is put into hot pressing furnace, close fire door, carry out precompressed at room temperature condition earlier, preload pressure is at 5-20MPa;
3) then vacuum system to vacuumizing in the stove, when vacuum reaches 1x10-2Pa in the stove, copper induction coil energising heating mould, mixed-powder and pressure head to 465 ℃-765 ℃; Be incubated 1-5 hour, then utilize the dual-heated of vacuum induction and resistance to make temperature be warming up to 800-1300 ℃ rapidly, heating rate 50-100 ℃/min; When reaching sintering temperature, go up push-down head and begin pressurization, pressure is controlled at 10-80MPa, is incubated 2-6 hour; Stop heating then, shed pressure;
4) after the demoulding to be cooled, the titanium silicon target base of moulding is carried out machinery and electric machining, clean after the completion of processing, oven dry, packaging process, obtain final required titanium silicon target material.
2. according to the manufacturing approach of the said a kind of titanium silicon target of claim 1, it is characterized in that: the percentage by weight of silica flour and titanium valve is silica flour: titanium valve=1%-50%:50%-99% in the said step 1).
3. according to the manufacturing approach of claim 1 or 2 said a kind of titanium silicon targets, it is characterized in that: the titanium valve granularity is 40-83 μ m in the said step 1), and the silicon powder particle degree is 30-100 μ m.
4. according to the manufacturing approach of the said a kind of titanium silicon target of claim 3, it is characterized in that: in the said step 1) titanium valve purity more than 99.9%, silica flour purity is more than 99.9%.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104148643A (en) * | 2014-08-12 | 2014-11-19 | 成都银河磁体股份有限公司 | Hot-press device for machining magnet |
| CN105331939A (en) * | 2014-08-15 | 2016-02-17 | 安泰科技股份有限公司 | Silicon-alloy-containing target material and preparation method thereof |
| TWI551704B (en) * | 2015-05-21 | 2016-10-01 | China Steel Corp | Copper gallium alloy composite sodium element target manufacturing method |
| CN106367625A (en) * | 2016-08-23 | 2017-02-01 | 大连理工大学 | Preparation method of silicon-zirconium alloy used for sputtering target material |
| CN106467960A (en) * | 2016-09-30 | 2017-03-01 | 东北大学 | A kind of high-intensity magnetic field hot pressing is for the device and method of metal targets |
| CN106835033A (en) * | 2016-12-21 | 2017-06-13 | 包头稀土研究院 | The manufacture method of high Mn content alumal target |
| CN108103460A (en) * | 2017-11-24 | 2018-06-01 | 北京安泰六九新材料科技有限公司 | A kind of titanium carbide target and preparation method thereof |
| CN110257783A (en) * | 2019-06-27 | 2019-09-20 | 上海交通大学 | A kind of low cost preparation method of titanium silicon target |
| CN111947460A (en) * | 2020-08-03 | 2020-11-17 | 宝钢化工湛江有限公司 | Control method of heating furnace for blast furnace gas and coke oven gas mixed combustion |
| CN112919470A (en) * | 2021-01-21 | 2021-06-08 | 辽宁中色新材科技有限公司 | Production process of titanium silicon carbide |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01136969A (en) * | 1987-11-24 | 1989-05-30 | Mitsubishi Metal Corp | Manufacture of target for titanium silicide sputtering |
| JPH03107453A (en) * | 1989-09-21 | 1991-05-07 | Hitachi Metals Ltd | Ti-w target and production thereof |
| JPH04116161A (en) * | 1990-09-05 | 1992-04-16 | Hitachi Metals Ltd | Titanium target material and production thereof |
| JP2002212708A (en) * | 2000-11-16 | 2002-07-31 | Hitachi Metals Ltd | Ti-Si ALLOY BASED TARGET MATERIAL, PRODUCTION METHOD THEREFOR AND FILM COATING METHOD |
| JP3792007B2 (en) * | 1997-06-12 | 2006-06-28 | 株式会社日鉱マテリアルズ | Manufacturing method of sputtering target |
| CN102260802A (en) * | 2011-07-20 | 2011-11-30 | 佛山市钜仕泰粉末冶金有限公司 | Target preparation device and target processing method thereof |
| CN102321833A (en) * | 2011-09-29 | 2012-01-18 | 余鹏 | Al-Ti-Si alloy target material and preparation method thereof |
| CN102366833A (en) * | 2011-11-21 | 2012-03-07 | 宁波江丰电子材料有限公司 | Production method of tungsten-titanium target blank |
-
2012
- 2012-06-20 CN CN2012102037478A patent/CN102699325A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01136969A (en) * | 1987-11-24 | 1989-05-30 | Mitsubishi Metal Corp | Manufacture of target for titanium silicide sputtering |
| JPH03107453A (en) * | 1989-09-21 | 1991-05-07 | Hitachi Metals Ltd | Ti-w target and production thereof |
| JPH04116161A (en) * | 1990-09-05 | 1992-04-16 | Hitachi Metals Ltd | Titanium target material and production thereof |
| JP3792007B2 (en) * | 1997-06-12 | 2006-06-28 | 株式会社日鉱マテリアルズ | Manufacturing method of sputtering target |
| JP2002212708A (en) * | 2000-11-16 | 2002-07-31 | Hitachi Metals Ltd | Ti-Si ALLOY BASED TARGET MATERIAL, PRODUCTION METHOD THEREFOR AND FILM COATING METHOD |
| CN102260802A (en) * | 2011-07-20 | 2011-11-30 | 佛山市钜仕泰粉末冶金有限公司 | Target preparation device and target processing method thereof |
| CN102321833A (en) * | 2011-09-29 | 2012-01-18 | 余鹏 | Al-Ti-Si alloy target material and preparation method thereof |
| CN102366833A (en) * | 2011-11-21 | 2012-03-07 | 宁波江丰电子材料有限公司 | Production method of tungsten-titanium target blank |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104148643A (en) * | 2014-08-12 | 2014-11-19 | 成都银河磁体股份有限公司 | Hot-press device for machining magnet |
| CN105331939A (en) * | 2014-08-15 | 2016-02-17 | 安泰科技股份有限公司 | Silicon-alloy-containing target material and preparation method thereof |
| TWI551704B (en) * | 2015-05-21 | 2016-10-01 | China Steel Corp | Copper gallium alloy composite sodium element target manufacturing method |
| CN106367625A (en) * | 2016-08-23 | 2017-02-01 | 大连理工大学 | Preparation method of silicon-zirconium alloy used for sputtering target material |
| CN106467960B (en) * | 2016-09-30 | 2019-02-01 | 东北大学 | A kind of high-intensity magnetic field hot pressing for metal targets device and method |
| CN106467960A (en) * | 2016-09-30 | 2017-03-01 | 东北大学 | A kind of high-intensity magnetic field hot pressing is for the device and method of metal targets |
| CN106835033A (en) * | 2016-12-21 | 2017-06-13 | 包头稀土研究院 | The manufacture method of high Mn content alumal target |
| CN108103460A (en) * | 2017-11-24 | 2018-06-01 | 北京安泰六九新材料科技有限公司 | A kind of titanium carbide target and preparation method thereof |
| CN108103460B (en) * | 2017-11-24 | 2019-11-29 | 北京安泰六九新材料科技有限公司 | A kind of titanium carbide target and preparation method thereof |
| CN110257783A (en) * | 2019-06-27 | 2019-09-20 | 上海交通大学 | A kind of low cost preparation method of titanium silicon target |
| CN111947460A (en) * | 2020-08-03 | 2020-11-17 | 宝钢化工湛江有限公司 | Control method of heating furnace for blast furnace gas and coke oven gas mixed combustion |
| CN111947460B (en) * | 2020-08-03 | 2022-06-21 | 宝钢化工湛江有限公司 | Control method of heating furnace for blast furnace gas and coke oven gas mixed combustion |
| CN112919470A (en) * | 2021-01-21 | 2021-06-08 | 辽宁中色新材科技有限公司 | Production process of titanium silicon carbide |
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Application publication date: 20121003 |