CN103121838A - WO3-TiO2 composite target material and preparation method of same - Google Patents
WO3-TiO2 composite target material and preparation method of same Download PDFInfo
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- CN103121838A CN103121838A CN2011103728498A CN201110372849A CN103121838A CN 103121838 A CN103121838 A CN 103121838A CN 2011103728498 A CN2011103728498 A CN 2011103728498A CN 201110372849 A CN201110372849 A CN 201110372849A CN 103121838 A CN103121838 A CN 103121838A
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Abstract
The invention discloses preparation method for a WO3-TiO2 composite target material, which is characterized in that the WO3-TiO2 composite target material having a purity of greater than 99.9%, a relative density of greater than 95% and a bending strength of greater than 60Mpa is prepared by adopting a low-cost normal-pressure sintering process and in the condition of no any sintering aids. The target material is especially suitable for preparing a WO3-TiO2 composite film, and has wide applications in the fields of photocatalytic purification, gas sensing, photovoltaic conversion, and the like.
Description
Technical field
The invention belongs to inorganic non-metallic element and compound thereof.
Background technology
Tungsten oxide 99.999/titanium oxide composite film is a kind of functional materials be widely studied.Molar ratio by titanium oxide and Tungsten oxide 99.999 in the adjusting laminated film can be to its photocatalysis performance, air-sensitive performance, and electrochromic properties etc. carry out Effective Regulation.Materials is having wide practical use in fields such as opticglass, flat pannel display, opto-electronic conversion, electrochromism, photochromic, light catalytic purifying sewage, photo-catalyst, gas sensors.
Tungsten oxide 99.999/titanium oxide composite film preparation method mainly contains: the whole bag of tricks such as sol-gel, strike, chemical vapour deposition, spray pyrolysis, anodic oxidation, physical vapor deposition.The film wherein prepared due to physical vapor deposition and the bonding strength of matrix is high, sedimentation effect is high, technical maturity is stable is widely used.Need to use fine and close Tungsten oxide 99.999/titanium oxide composite target material and prepare Tungsten oxide 99.999/titanium oxide composite film with physical vapor deposition, by energy-beam, the target bombardment be gasified, then deposit to matrix surface.Because the self-diffusion coefficient of Tungsten oxide 99.999/titanium oxide composite material is low, and therefore the Tungsten oxide 99.999 in target is difficult to densified sintering product about 1470 ℃ fusings.If the interpolation sintering aid, Tungsten oxide 99.999/the titanium oxide composite film of vapour deposition is because impurity affects its photoelectric characteristic.
Summary of the invention
The invention discloses the preparation of a kind of Tungsten oxide 99.999 of novel densification/titanium oxide composite target material.It is characterized in that not adding any sintering aid and make Tungsten oxide 99.999/titanium oxide composite target material sintering densification, thus the purity that makes this composite target material higher than 99.9%, relative density is greater than 95%, bending strength is greater than 60Mpa.Due to its high purity and high-density, the Tungsten oxide 99.999/titanium oxide composite material of this densification, suitable especially conduct prepares with physical vaporous deposition the target that Tungsten oxide 99.999/titanium oxide composite film is used.
The present invention has studied and has grasped ball milling, moulding and the sintering process rule that affects on densification, performance and the structure of sintered tungsten oxide/titanium oxide composite target material material in great detail, thereby can effectively control its densification, structure and performance, prepare high purity, high-density and high-intensity Tungsten oxide 99.999/titanium oxide composite target material.
The invention has the advantages that and both be applicable to common Tungsten oxide 99.999 and titanium oxide powder powder stock (powder size 5-30 micron) also for ultra-fine nanometer tungsten oxide and titanium oxide powder powder stock, and do not add any sintering aid, just can prepare high purity, high-density and high-intensity Tungsten oxide 99.999/titanium oxide composite target material.This target, can as required, make various complicated shapes expediently.
Technical scheme of the present invention is: adopt powder size at common Tungsten oxide 99.999 and the titanium oxide powder powder stock of 5-30 micron or adopt nano level Tungsten oxide 99.999 and the titanium oxide powder powder stock, its purity all requires higher than 99.99%.At first by raw material ball milling mixing 12-48 hour in ball mill, the abrading-ball adopted during ball milling is the column abrading-ball that purity is made higher than 99.9% tungsten, in ball milling, add 3%-8% (with respect to adopted Tungsten oxide 99.999 and the total mass ratio of titanium oxide) PEG20000 as forming agent, by the raw material after ball milling at 60 ℃ of-100 ℃ of lower forced air drying 4-12 hour, after the 40-80 mesh sieve sieves, compression moulding under 60-150Mpa pressure, by the sample of this compression moulding under electric furnace Air atmosphere, be raised to 300-500 ℃ from room temperature, heat-up rate is 0.5 ℃/minute, and under 300-500 ℃ the insulation 2-4 hour de-forming agent, encourage again afterwards sample with the speed of 2 ℃/minute, continue to be warmed up to 1200 ℃-1400 ℃, and under 1200-1400 ℃ the insulation 60-240 minute, furnace cooling afterwards, the Tungsten oxide 99.999 made like this/titanium oxide composite target material, purity is higher than 99.9%, relative density is greater than 95.3%, bending strength is greater than 65Mpa.
The accompanying drawing explanation
Fig. 1 is the correlated performance parameter list of target prepared in the specific embodiment of the invention 1, example 2 and example 3
Embodiment
Embodiment 1
Take the titanium dioxide powder (mean particle size 100 nanometers) of 80g purity 99.99%, the tungsten trioxide powder that 23g purity is 99.99% (mean particle size 80 nanometers), with the 5g purity PEG20000 that is 99.9% as forming agent, above-mentioned raw materials is added to deionized water wet-milling 24 hours in ball mill, again by the raw material after ball milling 60 ℃ of lower forced air dryings 12 hours, after 60 mesh sieves sieve, compression moulding under 100Mpa pressure, after the sample of this compression moulding being incubated under 500 ℃ to 4 hours de-forming agents, under continuous heating to 1250 ℃ in air normal pressure-sintered 120 minutes, furnace cooling, make high fine and close WO
3-TiO
2composite target material, its correlated performance parameter is shown in Fig. 1.
Embodiment 2
The titanium dioxide powder (10 microns of mean particle sizes) that to take 90g purity be 99.99%, the tungsten trioxide powder that 23g purity is 99.99% (17 microns of mean particle sizes), with the 6g purity PEG20000 that is 99.9% as forming agent, above-mentioned raw materials is added to deionized water wet-milling 36 hours in ball mill, again by the raw material after ball milling 80 ℃ of lower forced air dryings 8 hours, after 40 mesh sieves sieve, compression moulding under 150Mpa pressure, after the sample of this compression moulding being incubated under 350 ℃ to 3 hours de-forming agents, under continuous heating to 1400 ℃ in air normal pressure-sintered 200 minutes, furnace cooling, make high fine and close WO
3-TiO
2composite target material, its correlated performance parameter is shown in Fig. 1.
Embodiment 3
The titanium dioxide powder (mean particle size 80 nanometers) that to take 65g purity be 99.99%, the tungsten trioxide powder that 35g purity is 99.99% (5 microns of mean particle sizes), with the 4g purity PEG20000 that is 99.9% as forming agent, above-mentioned raw materials is added to deionized water wet-milling 18 hours in ball mill, again by the raw material after ball milling 100 ℃ of lower forced air dryings 6 hours, after 50 mesh sieves sieve, compression moulding under 120Mpa pressure, after the sample of this compression moulding being incubated under 450 ℃ to 4 hours de-forming agents, under continuous heating to 1350 ℃ in air normal pressure-sintered 60-180 minute, furnace cooling, make high fine and close WO
3-TiO
2composite target material, its correlated performance parameter is shown in Fig. 1.
Claims (6)
1. the WO of a densification
3-TiO
2the composite ceramics target, its feature is not added any sintering aid and is made this target sintering densification, and relative density is more than 95%.
2. WO according to claim 1
3-TiO
2the composite ceramics target, after sintering, the purity of target is higher than 99.9%, and bending strength is greater than 60Mpa.
3. WO according to claim 1
3-TiO
2the composite ceramics target, mainly make by ball milling-drying-sieve-operations such as moulding-sintering.
4. WO according to claim 1
3-TiO
2the composite ceramics target, concrete normal pressure-sintered technique, hot-pressing sintering technique or the gas pressure sintering technique of adopting of its sintering process.
5. WO according to claim 1
3-TiO
2the composite ceramics target, both being applicable to granularity is common granularity Tungsten oxide 99.999 and the titanium oxide powder powder stock of 5-30 micron, also be applicable to nano level Tungsten oxide 99.999 and titanium oxide powder powder stock, and this target can be made various complicated shapes expediently.
6. the WO of a densification
3-TiO
2the preparation method of composite ceramics target, it comprises the steps: raw material claimed in claim 5 ball milling 12-48 hour at room temperature, and then under 60-100 ℃ dry 4-12 hour, dried raw material is being crossed the 40-80 mesh sieve, under the pressure of 60-150Mpa, be pressed, material after moulding is incubated 2-4 hour under 300-500 ℃, last normal pressure-sintered 2-6 hour in 1200-1400 ℃ of lower air atmosphere again, furnace cooling.
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| CN2011103728498A CN103121838A (en) | 2011-11-21 | 2011-11-21 | WO3-TiO2 composite target material and preparation method of same |
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| CN2011103728498A CN103121838A (en) | 2011-11-21 | 2011-11-21 | WO3-TiO2 composite target material and preparation method of same |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106946292A (en) * | 2017-03-08 | 2017-07-14 | 重庆大学 | A kind of preparation method of titanium dioxide/tungsten trioxide nano-rod composite |
| CN107200580A (en) * | 2017-06-21 | 2017-09-26 | 佛山市钜仕泰粉末冶金有限公司 | A kind of optical nano ceramic insulation glass for strengthening visible light-transmissive and preparation method thereof |
| CN111362304A (en) * | 2020-04-13 | 2020-07-03 | 中国原子能科学研究院 | Method for preparing oxygen isotope target |
| CN112358294A (en) * | 2020-11-13 | 2021-02-12 | 北京航大微纳科技有限公司 | Hot-pressing sintering preparation method of tungsten oxide-based ceramic target material |
| CN112374887A (en) * | 2020-11-13 | 2021-02-19 | 北京航大微纳科技有限公司 | Gel injection molding preparation method of tungsten oxide-based ceramic target material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007290875A (en) * | 2006-04-20 | 2007-11-08 | Sumitomo Metal Mining Co Ltd | Titanium oxide-based sintered compact and its manufacturing method |
| CN101319307A (en) * | 2008-07-14 | 2008-12-10 | 王悦林 | Method of manufacturing tin indium oxide target material |
| CN101851745A (en) * | 2009-04-02 | 2010-10-06 | 宜兴佰伦光电材料科技有限公司 | Indium zinc gallium oxide (IZGO) sputtering target for transparent conductive film and manufacturing method |
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2011
- 2011-11-21 CN CN2011103728498A patent/CN103121838A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007290875A (en) * | 2006-04-20 | 2007-11-08 | Sumitomo Metal Mining Co Ltd | Titanium oxide-based sintered compact and its manufacturing method |
| CN101319307A (en) * | 2008-07-14 | 2008-12-10 | 王悦林 | Method of manufacturing tin indium oxide target material |
| CN101851745A (en) * | 2009-04-02 | 2010-10-06 | 宜兴佰伦光电材料科技有限公司 | Indium zinc gallium oxide (IZGO) sputtering target for transparent conductive film and manufacturing method |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106946292A (en) * | 2017-03-08 | 2017-07-14 | 重庆大学 | A kind of preparation method of titanium dioxide/tungsten trioxide nano-rod composite |
| CN107200580A (en) * | 2017-06-21 | 2017-09-26 | 佛山市钜仕泰粉末冶金有限公司 | A kind of optical nano ceramic insulation glass for strengthening visible light-transmissive and preparation method thereof |
| CN107200580B (en) * | 2017-06-21 | 2019-05-24 | 佛山市钜仕泰粉末冶金有限公司 | A kind of optical nano ceramic insulation glass and preparation method thereof enhancing visible light-transmissive |
| CN111362304A (en) * | 2020-04-13 | 2020-07-03 | 中国原子能科学研究院 | Method for preparing oxygen isotope target |
| CN112358294A (en) * | 2020-11-13 | 2021-02-12 | 北京航大微纳科技有限公司 | Hot-pressing sintering preparation method of tungsten oxide-based ceramic target material |
| CN112374887A (en) * | 2020-11-13 | 2021-02-19 | 北京航大微纳科技有限公司 | Gel injection molding preparation method of tungsten oxide-based ceramic target material |
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Application publication date: 20130529 |