CN104973864A - Niobium oxide plane target preparation method and niobium oxide plane target - Google Patents
Niobium oxide plane target preparation method and niobium oxide plane target Download PDFInfo
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- CN104973864A CN104973864A CN201510398196.9A CN201510398196A CN104973864A CN 104973864 A CN104973864 A CN 104973864A CN 201510398196 A CN201510398196 A CN 201510398196A CN 104973864 A CN104973864 A CN 104973864A
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- niobium oxides
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Abstract
The present invention discloses a niobium oxide plane target preparation method, which comprises: 1) powder preparation: uniformly mixing niobium oxide powder and metal niobium powder, and grinding the powder mixture to achieve the particle size of 50-200 nm; 2) powder calcining: carrying out vacuum calcining on the grinded powder mixture obtained in the step 1); 3) granulation: carrying out a granulation treatment on the calcined powder mixture in the step 2 and carrying out a drying treatment; 4) molding: pre-molding the dried powder in the step 3) under 20-70 MPa, and carrying out cold isostatic pressing molding on the pre-molded billet under 200-300 MPa; 5) atmosphere sintering: carrying out an atmosphere sintering treatment on the billet obtained in the step 4) in an atmosphere sintering furnace; and 6) target billet fine processing: cooling the sintered target billet obtained in the step 5) to a room temperature, and carrying out fine processing on the target billet according to the desired size so as to obtain the niobium oxide plane target. The preparation method of the present invention has characteristics of simple preparation process and high production efficiency.
Description
Technical field
The present invention relates to a kind of preparation method of magnetron sputtering target, be specifically related to a kind of atmosphere sintering legal system that utilizes for the method for niobium oxides planar targets, in addition, the invention still further relates to a kind of niobium oxides planar targets prepared by this preparation method, belong to target manufacturing technology field.
Background technology
Niobium Pentxoxide is widely used in many fields of modern technologies due to the physics and chemistry character of its uniqueness.Such as, utilize the ultraviolet absorption ability that it is stronger, can used as the protective membrane of ultraviolet sensitivity material; Utilize the characteristic that its film refractive index is higher, can with SiO
2the film with different refractivity can be prepared Deng cooperation.Due to these significant advantages, Niobium Pentxoxide target is widely used in the various fields such as solar cell, liquid-crystal display, ion display, collection touch screen, opticglass, gas sensor.Along with the development of science and technology and the continuous extension of Application Areas, the demand of niobium oxide target also constantly increases.
At present, market uses maximum be niobium oxides planar targets, mostly adopt vacuum hot-pressing to prepare.But employing the method, niobium oxides target base thickness is comparatively large, needs to cut open blade technolgy processing by machining and reach required thickness requirement in the course of processing.The current blade technolgy that cuts open mainly adopts diamond wire saw and Wire EDM.Because niobium oxide target belongs to ceramic product, hardness is comparatively large, causes the efficiency of diamond wire saw lower; And although niobium oxide target has certain electroconductibility, compared with metal targets, resistivity is still too high, causes Wire EDM efficiency lower.Therefore, when adopting pressure sintering to prepare niobium oxides target base, the operation cuing open sheet significantly reduces overall production efficiency.Therefore, a kind of production efficiency high oxidation niobium planar targets complete processing of exploitation is needed badly.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, the preparation method of the niobium oxides planar targets providing a kind of production efficiency high.In addition, another object of the present invention is to provide a kind of and processed the niobium oxides planar targets obtained by this preparation method.
For achieving the above object, the present invention is by the following technical solutions:
A preparation method for niobium oxides planar targets, its preparation process comprises:
1) powder preparation: niobium oxides powder and metal niobium powder are mixed and the particle diameter of powder mixture is ground to 50-200nm;
2) powder calcination: to step 1) in powder mixture after fine grinding carry out vacuum calcining;
3) granulation: to step 2) in calcining after powder mixture carry out granulation process and drying treatment;
4) shaping: by step 3) in the premolding under 20-70MPa of dried powder, subsequently by preformed base substrate cold isostatic compaction under 200-300MPa;
5) atmosphere sintering: by step 4) in the biscuit that obtains of cold isostatic compaction in atmosphere sintering furnace, carry out atmosphere sintering process;
6) target base precision work: by step 5) in after target base after sintering processes is cooled to room temperature, by desired size, precision work is carried out to target base, obtains described niobium oxides planar targets.
In powder mixture preferably: step 1), the amount of metal niobium powder is 0.1-10% (wt%), that is: mixing niobium amount is 0.1%-10%;
Process of lapping preferably: step 1) is: described powder mixture is fine grinding 3-10 hour under the rotating speed at 2000-6000rpm;
Preferably: the particle diameter of described niobium oxides powder is 0.5-10 μm; The particle diameter of described metal niobium powder is 1-50 μm.
Vacuum calcining preferably: step 2), vacuum tightness is 100-1000Pa, and calcining temperature is 300-600 DEG C, and calcination time is 2-5 hour.
In granulation process preferably: step 3), add binding agent.
Preferably: described binding agent is polyvinyl alcohol or polyvinyl butyral acetal, and its add-on is the 1-5% of mixed powder weight.
Atmosphere sintering treating processes preferably: step 5) is: under 0.01Pa, 800 DEG C are warming up to the temperature rise rate of 50-200 DEG C/h, and be incubated 3-5 hour, pass into argon gas subsequently or nitrogen makes pressure reach 200-1000Kpa, and continue to be warming up to 1250-1450 DEG C with the temperature rise rate of 150 DEG C/h, and be incubated 3-7 hour.
Another object of the present invention is to provide a kind of and processed the niobium oxides planar targets obtained by above-mentioned preparation method, its density>=4.5g/cm
3, resistivity≤2.0 × 10
-3Ω cm.
Beneficial effect of the present invention is, the present invention, by material powder is carried out nanometer process, significantly reduces the granularity of metal niobium powder, and make metal niobium powder niobium oxides powder distribute more even, and then make the electroconductibility of target higher.Moreover atmosphere sintering treatment step of the present invention, adopts the mode that sectional type heats up, and improves the density of target further.In addition, target base thickness of the present invention can free setting according to demand, and the target base without the need to preparing as pressure sintering again needs to cut open sheet operation, thus can greatly enhance productivity.
Embodiment
Below in conjunction with specific embodiment, the specific embodiment of the present invention is described further.
The present invention adopts atmosphere sintering legal system for niobium oxides planar targets, and its preparation process comprises:
1) powder preparation: niobium oxides powder and metal niobium powder are mixed, and press material ball ratio 2:1 in nano-level grinder under the rotating speed of 2000-6000rpm fine grinding 3-10 hour;
2) powder calcination: by step 1) in mixed powder after fine grinding in vacuum calcining stove, calcine that solid state reaction is carried out to powder;
3) granulation: use spray-drier to carry out granulation process and drying treatment to the powder after calcining;
4) shaping: by step 3) in dried powder be placed in moulding press premolding under 20-70MPa, then preformed base substrate is put into cold isostatic press and is carried out at cold isostatic compaction under 200-300MPa;
5) atmosphere sintering: by step 4) in the biscuit that obtains of cold isostatic compaction in atmosphere sintering furnace, carry out atmosphere sintering process;
6) target base precision work: by step 5) in after target base after sintering processes cools to room temperature with the furnace, by desired size, precision work is carried out to target base, obtains niobium oxides planar targets of the present invention.
Further, described step 1) in, in mixed powder, the amount of metal niobium powder is 0.1-10% (wt%); Purity >=99.99% of described niobium oxides powder, its particle diameter is 0.5-10 μm; Purity >=99.95% of described metal niobium powder, its particle diameter is 1-50 μm; Further, step 1) in the particle diameter of mixed powder after fine grinding be 50-200nm: step 2) described in powder calcination step in, vacuum tightness is 100-1000Pa, and calcining temperature is 300-600 DEG C, and calcination time is 2-5 hour; Step 3) described in granulation process in, also add binding agent, described binding agent preferably polyethylene alcohol or polyvinyl butyral acetal, and press the weight percent meter of powder, the add-on 1-5% of described binding agent; Step 3) in drying treatment temperature be 200-270 DEG C; Step 5) described in atmosphere sintering treating processes be: under 0.01Pa, 800 DEG C are warming up to the temperature rise rate of 50-200 DEG C/h, and be incubated 3-5 hour, passing into argon gas subsequently makes furnace pressure reach 200-1000Kpa, and continue to be warming up to 1250-1450 DEG C with the temperature rise rate of 150 DEG C/h, and be incubated 3-7 hour.
Embodiment 1
A preparation method for niobium oxides planar targets, it comprises following preparation process:
1) powder preparation: be 99.99% by 20kg purity, particle diameter is that the metal niobium powder that the niobium oxides powder of 5 μm and 1kg purity are 99.99%, particle diameter is 5 μm mixes, and by the material ball ratio of 2:1 in nano-level grinder under the rotating speed of 4500rpm fine grinding 4h be 100nm to the particle diameter of powder mixture;
2) powder calcination: by step 1) in mixed powder after fine grinding be placed in vacuum calcining stove, at vacuum tightness 100Pa, calcining temperature 450 DEG C, calcine 3h to carry out solid state reaction to powder;
3) granulation: use spray-drier to carry out granulation process to the powder after calcining, add polyvinyl alcohol as binding agent in described granulation process, and its add-on is 3% of powder amount, subsequently the powder after granulation is carried out drying treatment at 240 DEG C;
4) shaping: by step 3) in dried powder load premolding under 30MPa in moulding press, subsequently preformed base substrate is put into cold isostatic press and is carried out at cold isostatic compaction under 220MPa;
5) atmosphere sintering: by step 4) in the biscuit that obtains of cold isostatic compaction be placed in atmosphere sintering furnace, under 0.01Pa, 800 DEG C are warming up to the temperature rise rate of 100 DEG C/h, and be incubated 3 hours, slowly passing into argon gas subsequently makes furnace pressure reach 800Kpa, and continue to be warming up to 1350 DEG C with the temperature rise rate of 150 DEG C/h, and be incubated 5 hours;
6) target base precision work: by step 5) in after target base after sintering processes cools to room temperature with the furnace, after tested the density of niobium oxide target is 4.55g/cm
3, resistivity is 1.68 × 10
-3Ω cm, carries out precision work according to desired size to rotary target base, must meet the niobium oxides planar targets that dimensions requires.
Embodiment 2
A preparation method for niobium oxides planar targets, it comprises following preparation process:
1) powder preparation: be 99.99% by 20kg purity, particle diameter is that the metal niobium powder that the niobium oxides powder of 1.5 μm and 0.05kg purity are 99.99%, particle diameter is 35 μm mixes, and by the material ball ratio of 2:1 in nano-level grinder under the rotating speed of 3500rpm fine grinding 8h be 150nm to the particle diameter of powder mixture;
2) powder calcination: by step 1) in mixed powder after fine grinding be placed in vacuum calcining stove, at vacuum tightness 800Pa, calcining temperature 400 DEG C, calcine 4h to carry out solid state reaction to powder;
3) granulation: use spray-drier to carry out granulation process to the powder after calcining, polyvinyl butyral acetal is added as binding agent in described granulation process, and its add-on is 1% of powder amount, subsequently the powder after granulation is carried out drying treatment at 260 DEG C;
4) shaping: by step 3) in dried powder load premolding under 60MPa in moulding press, subsequently preformed base substrate is put into cold isostatic press and is carried out at cold isostatic compaction under 250MPa;
5) atmosphere sintering: by step 4) in the biscuit that obtains of cold isostatic compaction be placed in atmosphere sintering furnace, under 0.01Pa, 800 DEG C are warming up to the temperature rise rate of 60 DEG C/h, and be incubated 4 hours, slowly passing into argon gas subsequently makes furnace pressure reach 600Kpa, and continue to be warming up to 1300 DEG C with the temperature rise rate of 150 DEG C/h, and be incubated 6 hours;
6) target base precision work: by step 5) in after target base after sintering processes cools to room temperature with the furnace, after tested the density of niobium oxide target is 4.52g/cm
3, resistivity is 1.87 × 10
-3Ω cm, carries out precision work according to desired size to rotary target base, must meet the niobium oxides planar targets that dimensions requires.
Embodiment 3
A preparation method for niobium oxides planar targets, it comprises following preparation process:
1) powder preparation: be 99.99% by 20kg purity, particle diameter is that the metal niobium powder that the niobium oxides powder of 8.5 μm and 2kg purity are 99.99%, particle diameter is 50 μm mixes, and by the material ball ratio of 2:1 in nano-level grinder under the rotating speed of 6000rpm fine grinding 4h be 190nm to the particle diameter of powder mixture;
2) powder calcination: by step 1) in mixed powder after fine grinding be placed in vacuum calcining stove, at vacuum tightness 900Pa, calcining temperature 550 DEG C, calcine 2h to carry out solid state reaction to powder;
3) granulation: use spray-drier to carry out granulation process to the powder after calcining, add polyvinyl alcohol as binding agent in described granulation process, and its add-on is 4.5% of powder amount, subsequently the powder after granulation is carried out drying treatment at 260 DEG C;
4) shaping: by step 3) in dried powder load premolding under 50MPa in moulding press, subsequently preformed base substrate is put into cold isostatic press and is carried out at cold isostatic compaction under 280MPa;
5) atmosphere sintering: by step 4) in the biscuit that obtains of cold isostatic compaction be placed in atmosphere sintering furnace, under 0.01Pa, 800 DEG C are warming up to the temperature rise rate of 180 DEG C/h, and be incubated 5 hours, slowly passing into nitrogen subsequently makes furnace pressure reach 200Kpa, and continue to be warming up to 1450 DEG C with the temperature rise rate of 150 DEG C/h, and be incubated 7 hours;
6) target base precision work: by step 5) in after target base after sintering processes cools to room temperature with the furnace, after tested the density of niobium oxide target is 4.65g/cm
3, resistivity is 1.27 × 10
-3Ω cm, installs desired size and carries out precision work to rotary target base, must meet the niobium oxides planar targets that dimensions requires.
The present invention is by preferred embodiment having carried out detailed explanation.But, by studying carefully above, to the change of each embodiment with to increase also be that one of ordinary skill in the art institute is apparent.The meaning of applicant
figurethat all these changes and increase have dropped in the protection domain of the claims in the present invention.Term used herein is only and is illustrated specific embodiment, and it is also not intended to limit invention.Unless otherwise defined, all terms used herein (comprising technical term and scientific terminology) are all identical with the understanding of one of ordinary skill in the art of the present invention.Known function or structure are for briefly and clearly consider or repeat no more.
Claims (10)
1. a preparation method for niobium oxides planar targets, is characterized in that: comprise the following steps:
1) powder preparation: niobium oxides powder and metal niobium powder are mixed and the particle diameter of powder mixture is ground to 50-200nm;
2) powder calcination: to step 1) in powder mixture after fine grinding carrying out vacuum calcining;
3) granulation: to step 2) in calcining after powder mixture carry out granulation process and drying treatment;
4) shaping: by step 3) in the premolding under 20-70MPa of dried powder, subsequently by preformed base substrate cold isostatic compaction under 200-300MPa;
5) atmosphere sintering: by step 4) in the biscuit that obtains of cold isostatic compaction in atmosphere sintering furnace, carry out atmosphere sintering process;
6) target base precision work: by step 5) in after target base after sintering processes is cooled to room temperature, by desired size, precision work is carried out to target base, obtains described niobium oxides planar targets.
2. preparation method according to claim 1, is characterized in that: step 1) described in powder mixture in, the amount of metal niobium powder is 0.1-10%.
3. preparation method according to claim 1 and 2, is characterized in that: the particle diameter of described niobium oxides powder is 0.5-10 μm; The particle diameter of described metal niobium powder is 1-50 μm.
4. preparation method according to claim 1, is characterized in that: step 1) in process of lapping be: powder mixture is fine grinding 3-10 hour under the rotating speed at 2000-6000rpm.
5. preparation method according to claim 1, is characterized in that: step 2) described in vacuum calcining, vacuum tightness is 100-1000Pa, and calcining temperature is 300-600 DEG C, and calcination time is 2-5 hour.
6. preparation method according to claim 1, is characterized in that: step 3) described in granulation process in, add binding agent.
7. preparation method according to claim 6, is characterized in that: described binding agent is polyvinyl alcohol or polyvinyl butyral acetal, and its add-on is the 1-5% of mixed powder weight.
8. preparation method according to claim 1, it is characterized in that: step 5) described in atmosphere sintering treating processes be: under 0.01Pa, 800 DEG C are warming up to the temperature rise rate of 50-200 DEG C/h, and be incubated 3-5 hour, pass into argon gas subsequently or nitrogen makes pressure reach 200-1000Kpa, and continue to be warming up to 1250-1450 DEG C with the temperature rise rate of 150 DEG C/h, and be incubated 3-7 hour.
9. a niobium oxides planar targets, is characterized in that: described niobium oxides planar targets is processed by preparation method according to claim 1 and obtained.
10. niobium oxides planar targets according to claim 9, is characterized in that: the density>=4.5g/cm of described niobium oxides planar targets
3, resistivity≤2.0 × 10
-3Ω cm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106747439A (en) * | 2016-12-19 | 2017-05-31 | 湖南稀土金属材料研究院 | Niobium oxide target and preparation method thereof |
| CN108530066A (en) * | 2018-04-10 | 2018-09-14 | 九江有色金属冶炼有限公司 | A kind of manufacturing method of high purity niobium oxide ontology crucible |
| CN111606708A (en) * | 2020-06-03 | 2020-09-01 | 福建阿石创新材料股份有限公司 | Low-resistivity niobium pentoxide hot-pressing target material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101851740A (en) * | 2009-04-02 | 2010-10-06 | 宜兴佰伦光电材料科技有限公司 | Conductive Nb2O5-x target material for magnetron sputtering coating and production method thereof |
| WO2015052139A1 (en) * | 2013-10-07 | 2015-04-16 | Heraeus Deutschland GmbH & Co. KG | Metal oxide target and method for producing same |
-
2015
- 2015-07-08 CN CN201510398196.9A patent/CN104973864B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101851740A (en) * | 2009-04-02 | 2010-10-06 | 宜兴佰伦光电材料科技有限公司 | Conductive Nb2O5-x target material for magnetron sputtering coating and production method thereof |
| WO2015052139A1 (en) * | 2013-10-07 | 2015-04-16 | Heraeus Deutschland GmbH & Co. KG | Metal oxide target and method for producing same |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106747439A (en) * | 2016-12-19 | 2017-05-31 | 湖南稀土金属材料研究院 | Niobium oxide target and preparation method thereof |
| CN106747439B (en) * | 2016-12-19 | 2019-08-02 | 湖南稀土金属材料研究院 | Niobium oxide target and preparation method thereof |
| CN108530066A (en) * | 2018-04-10 | 2018-09-14 | 九江有色金属冶炼有限公司 | A kind of manufacturing method of high purity niobium oxide ontology crucible |
| CN111606708A (en) * | 2020-06-03 | 2020-09-01 | 福建阿石创新材料股份有限公司 | Low-resistivity niobium pentoxide hot-pressing target material and preparation method thereof |
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| CN104973864B (en) | 2017-03-29 |
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Effective date of registration: 20180718 Address after: 065200 187 Yan Chang Road, Yanjiao Development Zone, Sanhe, Hebei. Patentee after: Yeke Metal Co.,Ltd. Address before: 101100 Beijing Tongzhou District Economic Development Zone East District five street 06 Patentee before: Beijing Yeke Nano Technology Co.,Ltd. |