CN101705467A - Method for preparing rotary ceramic target - Google Patents
Method for preparing rotary ceramic target Download PDFInfo
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- CN101705467A CN101705467A CN200910051156A CN200910051156A CN101705467A CN 101705467 A CN101705467 A CN 101705467A CN 200910051156 A CN200910051156 A CN 200910051156A CN 200910051156 A CN200910051156 A CN 200910051156A CN 101705467 A CN101705467 A CN 101705467A
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Abstract
The invention relates to the technical field of films, in particular to a method for preparing a rotary ceramic target, which comprises the following steps: (1) preparing a precursor of the target, namely weighting metal oxide powder of which the purity is not less than 99 weight percent, putting the powders into a mould for cold isostatic pressing to prepare the precursor of the target, wherein the reaction pressure is between 130 and 230 MPa, and the reaction time is between 20 and 70 minutes; and (2) sintering, namely putting the precursor of the target obtained in the step (1) into a sintering furnace for sintering densification, wherein the sintering temperature is between 1,000 and 1,600 DEG C, and the sintering time is between 40 and 85 hours. The wall thickness of rotary ceramic target prepared by the method is multiple times that of a plane target, so that the time of using the target continuously by customers is prolonged, the continuous productive power is improved and the total production cost is reduced.
Description
Technical field
The present invention relates to the thin film technique field, relate in particular to a kind of preparation method of rotary ceramic target.
Background technology
Existing technology of producing rotary ceramic target adopts the mode of spraying usually, comprise modes such as thermospray and plasma spraying, but be subjected to the limitation of spraying coating process, very difficult employing spraying method production at present has the rotary ceramic target thick than heavy wall, and the thickest that adopts the rotary ceramic sputtering target material of spraying method production at present is in 9 millimeter.This will cause the user can not long-time continuous production, need frequent shutdown to come more exchange device and then influence production efficiency to improve total cost of production.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing rotary ceramic target, this method technology is simple, and the target wall thickness that makes is thicker, obtain very big prolongation duration of service.
The object of the present invention is achieved like this:
A kind of preparation method of rotary ceramic target, this preparation method is as follows:
(1) preparation target precursor
Take by weighing purity and be not less than the metal-oxide powder of 99wt%, the mould of packing into carries out isostatic cool pressing, makes the target precursor, wherein:
Reaction pressure is 130～230Mpa;
Reaction times is 20～70min.
(2) sintering
Gained target precursor in the step (1) is put into sintering oven, densified sintering product, wherein:
Sintering temperature is 1000～1600 ℃;
Sintering time is 40～85 hours.
Further, can in step (1), add the metal-powder that purity is not less than 99wt%, behind metal-powder and metal-oxide powder thorough mixing, the mould of packing into, carry out isostatic cool pressing, make the target precursor, wherein, the content of metal oxide powder is 90～99wt%, and the content of metal-powder is 1～10wt%.
Wherein, described metal-powder can be metal niobium powder, metal tantalum powder, metal titanium powder, tungsten powder, metallic nickel powder or vanadium metal powder, preferable alloy niobium powder or metal titanium powder.
Also can take by weighing two or more metal-oxide powders in step (1), behind the thorough mixing, the mould of packing into carries out isostatic cool pressing, makes the target precursor.
Wherein, described metal-oxide powder is Zinc oxide powder, alumina powder jointed, niobium pentaoxide powder, tantalum pentoxide powder, titanium dioxide powder, nickel oxide powder, tin indium oxide powder or vanadium oxide powder.
The present invention is owing to adopted technique scheme, make it compared with prior art, has following beneficial effect: can have the thicker ceramic rotary target material of wall thickness according to customer demand production by the present invention, wall thickness can reach the several times of planar targets, thereby prolong the time that the client uses target continuously, improve the continuous production ability and lower total cost of production.
Embodiment
Further describe the present invention by the following examples, but be not limited thereto.
Embodiment 1: rotation zinc oxide aluminum ZnO/Al
2O
3Sputtering target material
With purity is 99.95% Zinc oxide powder (accounting for total mass 95%) and purity is that 99.99% alumina powder (accounting for total mass 2.0%) mixes mutually by ball milling method, well-mixed zinc oxide aluminum mixed powder is formed the rotation AZO target material presoma of 160 millimeters of external diameters, 125 millimeters of internal diameters, 300 millimeters of height, density 60% through isostatic cool pressing; The density that will form through 155Mpa pressure and 50 minute press time by isostatic cool pressing be that 60% rotation AZO target material presoma is put into sintering oven, through 70 hours, and 1200 ℃ of densified sintering products.
Analytical results:
By measure the density of densified sintering product zinc oxide aluminum rotary target material with Archimedes's method, its relative density is 95%;
Gained rotation zinc oxide aluminum ZnO/Al
2O
3Sputtering target material thickness is 17 millimeters.
Embodiment 2: rotation NbOx sputtering target material
With purity is 99.95% Niobium Pentxoxide powder (accounting for total mass 99%) and purity is that 99.99% metal niobium powder (accounting for total mass 1%) mixes mutually by ball milling method, and the mixed powder of well-mixed Niobium Pentxoxide and metal niobium is put into mould forms 160 millimeters of external diameters, 125 millimeters of internal diameters, 300 millimeters of height, density 65% through 150Mpa pressure and 20 minute press time by isostatic cool pressing rotation NbOx target presoma; The density that will form through isostatic cool pressing be that 65% rotation Niobium Pentxoxide target presoma is put into sintering oven, through 60 hours, and 1100 ℃ of densified sintering products.
Analytical results:
By measuring the closely density of densified sintering product target with Archimedes's method, its relative density is 92%;
By adopting XRD that the near target of densified sintering product is analyzed target is NbO
4.98, i.e. X=0.02;
Gained rotation NbOx sputtering target material thickness is 17.3 millimeters.
Embodiment 3: rotation TiOx sputtering target material
With purity is 99.5% titania powder (accounting for total mass 98%) and purity is that 99.5% metal titanium powder (accounting for total mass 2.0%) mixes mutually by ball milling method, and the mixed powder of well-mixed titanium dioxide and metal titanium is put into mould, and to form external diameter 160 millimeter, internal diameter 125 millimeter, height 300 millimeter, density through 160Mpa pressure and 45 minute press time through isostatic cool pressing by isostatic cool pressing be 70% rotation TiOx target presoma; The density that will form through isostatic cool pressing be that 70% rotation TiOx target presoma is put into sintering oven, through 65 hours, and 1150 ℃ of densified sintering products.
Analytical results:
By measuring the closely density of densified sintering product target with Archimedes's method, its relative density is 97%;
By adopting XRD that the near target of densified sintering product is analyzed target is TiO
1.75, i.e. x=0.25;
Gained rotation TiOx sputtering target material thickness is 17 millimeters.
Embodiment 4: rotation ZnO sputtering target material
The pure zinc oxide powder of purity 99.95% is put into mould forms 160 millimeters of external diameters, 125 millimeters of internal diameters, 300 millimeters of height, density 65% by isostatic cool pressing process 170Mpa pressure and 30 minute press time rotation ZnO target presoma, the density that will form through isostatic cool pressing be that 65% rotation ZnO target presoma is put into sintering oven, through 70 hours, 1350 ℃ of densified sintering products.
Analytical results:
By measure the density of densified sintering product zinc oxide aluminum rotary target material with Archimedes's method, its relative density is 95%;
Gained rotation ZnO sputtering target material thickness is 17 millimeters.
Embodiment 5: rotation ITO sputtering target material
With purity be 99.99% tin indium oxide (ITO) powder through the mould of packing into after the Ball milling, the mould that tin indium oxide (ITO) powder will be housed is put into isostatic cool pressing, and to form 160 millimeters of external diameters, 125 millimeters of internal diameters, 300 millimeters of height, density through the pressure of 190Mpa and 50 minute press time be 68% rotation ITO target presoma; The density that will form through isostatic cool pressing be that 68% rotation ITO target presoma is put into sintering oven, through 80 hours, and 1500 ℃ of densified sintering products.
Analytical results:
By measure the density of densified sintering product ITO rotary target material with Archimedes's method, its relative density is 99.0%;
Gained rotation ITO sputtering target material thickness is 17.2 millimeters.
Embodiment 6: rotation nickel oxide vanadium sputtering target material
With purity is 99.9% nickel oxide powder (accounting for total mass 92%) and purity is that 99.9% vanadium oxide powder (accounting for total mass 8.0%) mixes mutually by ball milling method, and the mixed powder of well-mixed nickel oxide powder and vanadium oxide powder is put into mould forms 160 millimeters of external diameters, 125 millimeters of internal diameters, 300 millimeters of height, density 60% through isostatic cool pressing through 150Mpa pressure and 60 minute press time by isostatic cool pressing nickel oxide vanadium rotary target material presoma; The density that will form through isostatic cool pressing be that 60% rotation nickel oxide vanadium target presoma is put into sintering oven, through 52 hours, and 1350 ℃ of densified sintering products.
Analytical results:
By measuring the closely density of densified sintering product target with Archimedes's method, its relative density is 99%;
Gained rotation nickel oxide vanadium sputtering target material thickness is 16.8 millimeters.
Embodiment 7: rotation tantalum pentoxide (Ta
2O
5) sputtering target material
With purity 99.99% tantalum pentoxide (Ta
2O
5) powder crosses ball milling method and mix in the mould of packing into, the mould that is equipped with through well-mixed tantalum pentoxide powder is put into isostatic cool pressing, and process isostatic cool pressing 150Mpa pressure and 45 minute press time form the tantalum pentoxide (Ta of 160 millimeters of external diameters, 125 millimeters of internal diameters, 300 millimeters of height, density 68% through isostatic cool pressing
2O
5) the rotary target material presoma; The density that will form through isostatic cool pressing is 68% rotation tantalum pentoxide (Ta
2O
5) the target presoma puts into sintering oven, through 48 hours, 1320 ℃ of densified sintering products.
Analytical results:
By measuring closely densified sintering product tantalum pentoxide (Ta with Archimedes's method
2O
5) density of target, its relative density is 99%;
Gained rotation tantalum pentoxide (Ta
2O
5) sputtering target material thickness is 17.2 millimeters.
Claims (5)
1. the preparation method of a rotary ceramic target is characterized in that this preparation method is as follows:
(1) preparation target precursor
Take by weighing purity and be not less than the metal-oxide powder of 99wt%, the mould of packing into carries out isostatic cool pressing, makes the target precursor, wherein:
Reaction pressure is 130～230Mpa,
Reaction times is 20～70min;
(2) sintering
Gained target precursor in the step (1) is put into sintering oven, densified sintering product, wherein:
Sintering temperature is 1000～1600 ℃,
Sintering time is 40～85 hours.
2. the method for claim 1, it is characterized in that: in step (1), add the metal-powder that purity is not less than 99wt%, behind metal-powder and metal-oxide powder thorough mixing, the mould of packing into, carry out isostatic cool pressing, make the target precursor, wherein: the content of metal oxide powder is 90～99wt%, and the content of metal-powder is 1～10wt%.
3. as claims 2 described methods, it is characterized in that: described metal-powder is metal niobium or metal titanium powder.
4. the method for claim 1, it is characterized in that: step takes by weighing two or more metal-oxide powders in (1), and behind the thorough mixing, the mould of packing into carries out isostatic cool pressing, makes the target precursor.
5. as claim 1 or 4 described methods, it is characterized in that: described metal-oxide powder is zinc oxide, aluminum oxide, Niobium Pentxoxide, tantalum pentoxide, titanium dioxide, nickel oxide, tin indium oxide or vanadium oxide powder.
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| CN200910051156A CN101705467A (en) | 2009-05-14 | 2009-05-14 | Method for preparing rotary ceramic target |
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|---|---|---|---|
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603285A (en) * | 2012-02-23 | 2012-07-25 | 西北稀有金属材料研究院 | Preparation method of zinc oxide-based tubular rotary target material |
| CN102699626A (en) * | 2012-01-04 | 2012-10-03 | 洛阳科威钨钼有限公司 | Fabricating technique of tungsten plane targets |
| CN103724008A (en) * | 2013-12-13 | 2014-04-16 | 西北稀有金属材料研究院 | Pure zinc oxide ceramic sputtering target material and preparation method thereof |
| CN103993281A (en) * | 2014-05-30 | 2014-08-20 | 天津大学 | Preparation method of FTO (F-doped SiO2) transparent conducting thin film |
| CN104557021A (en) * | 2015-01-14 | 2015-04-29 | 河北东同光电科技有限公司 | High-compactness titanium oxide target material and preparation method thereof |
| CN104961463A (en) * | 2015-07-08 | 2015-10-07 | 北京冶科纳米科技有限公司 | Niobium oxide rotating target and preparing method of niobium oxide rotating target |
| CN107628811A (en) * | 2017-08-11 | 2018-01-26 | 东台市超品光电材料有限公司 | Large scale binding formula gallium and yttrium codope zinc oxide rotary ceramic pipe target |
| EP3375904A1 (en) * | 2017-03-14 | 2018-09-19 | Materion Advanced Materials Germany GmbH | Cylindrical titanium oxide sputtering target and process for manufacturing the same |
| CN109536909A (en) * | 2019-01-16 | 2019-03-29 | 广州市尤特新材料有限公司 | A kind of rare earth metal rotary target material and its manufacturing method |
| CN110467462A (en) * | 2019-08-09 | 2019-11-19 | 宁夏中色新材料有限公司 | A kind of high-densit low resistance Rotary niobium oxide target material and preparation method thereof |
| CN115925416A (en) * | 2023-01-17 | 2023-04-07 | 丰联科光电(洛阳)股份有限公司 | Preparation method of tantalum oxide target material |
-
2009
- 2009-05-14 CN CN200910051156A patent/CN101705467A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102699626A (en) * | 2012-01-04 | 2012-10-03 | 洛阳科威钨钼有限公司 | Fabricating technique of tungsten plane targets |
| CN102603285A (en) * | 2012-02-23 | 2012-07-25 | 西北稀有金属材料研究院 | Preparation method of zinc oxide-based tubular rotary target material |
| CN102603285B (en) * | 2012-02-23 | 2013-08-28 | 西北稀有金属材料研究院 | Preparation method of zinc oxide-based tubular rotary target material |
| CN103724008A (en) * | 2013-12-13 | 2014-04-16 | 西北稀有金属材料研究院 | Pure zinc oxide ceramic sputtering target material and preparation method thereof |
| CN103993281A (en) * | 2014-05-30 | 2014-08-20 | 天津大学 | Preparation method of FTO (F-doped SiO2) transparent conducting thin film |
| CN104557021A (en) * | 2015-01-14 | 2015-04-29 | 河北东同光电科技有限公司 | High-compactness titanium oxide target material and preparation method thereof |
| CN104961463A (en) * | 2015-07-08 | 2015-10-07 | 北京冶科纳米科技有限公司 | Niobium oxide rotating target and preparing method of niobium oxide rotating target |
| EP3375904A1 (en) * | 2017-03-14 | 2018-09-19 | Materion Advanced Materials Germany GmbH | Cylindrical titanium oxide sputtering target and process for manufacturing the same |
| WO2018166831A1 (en) * | 2017-03-14 | 2018-09-20 | Materion Advanced Materials Germany Gmbh | Cylindrical titanium oxide sputtering target and process for manufacturing the same |
| US20200002235A1 (en) * | 2017-03-14 | 2020-01-02 | Materion Advanced Materials Germany Gmbh | Cylindrical titanium oxide sputtering target and process for manufacturing the same |
| CN107628811A (en) * | 2017-08-11 | 2018-01-26 | 东台市超品光电材料有限公司 | Large scale binding formula gallium and yttrium codope zinc oxide rotary ceramic pipe target |
| CN109536909A (en) * | 2019-01-16 | 2019-03-29 | 广州市尤特新材料有限公司 | A kind of rare earth metal rotary target material and its manufacturing method |
| CN110467462A (en) * | 2019-08-09 | 2019-11-19 | 宁夏中色新材料有限公司 | A kind of high-densit low resistance Rotary niobium oxide target material and preparation method thereof |
| CN115925416A (en) * | 2023-01-17 | 2023-04-07 | 丰联科光电(洛阳)股份有限公司 | Preparation method of tantalum oxide target material |
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Open date: 20100512 |