CN104961463A - Niobium oxide rotating target and preparing method of niobium oxide rotating target - Google Patents
Niobium oxide rotating target and preparing method of niobium oxide rotating target Download PDFInfo
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- CN104961463A CN104961463A CN201510397195.2A CN201510397195A CN104961463A CN 104961463 A CN104961463 A CN 104961463A CN 201510397195 A CN201510397195 A CN 201510397195A CN 104961463 A CN104961463 A CN 104961463A
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Abstract
The invention discloses a niobium oxide rotating target with the density being greater than or equal to 4.5g/cm<3> and with the resistivity being smaller than or equal to 2.0*10<-3> ohm*cm. A preparing method of the niobium oxide rotating target comprises the steps of (1) powder preparation: uniformly mixing niobium oxide powder and metal niobium powder, and finely grinding the powder at the rotating speed being 2000 to 6000rpm for 3 to 10 hours; (2) powder roasting: performing vacuum roasting on the mixed powder finely ground in the first step; (3) granulation: carrying out granulation processing and drying processing on powder sintered in the second step; (4) cold isopressing forming: performing cold isopressing forming on powder dried in the third step at 200 to 300MPa; (5) atmosphere sintering: carrying out atmosphere sintering processing on biscuits obtained through cold isopressing forming in the fourth step in an atmosphere sintering furnace; (6) target blank fine processing: cooling a target blank subjected to sintering processing in the fifth step to the room temperature, processing fine processing on the target blank according to the required dimension, and obtaining the niobium oxide rotating target. The preparing method has the characteristics that the processing process is simple, and the production efficiency is high.
Description
Technical field
The present invention relates to a kind of magnetron sputtering target, be specifically related to a kind of Rotary niobium oxide target material, in addition, the invention still further relates to a kind of atmosphere sintering legal system that utilizes for the method for this Rotary niobium oxide target material, 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, although the technology of preparing of planar targets is tending towards ripe day by day, but planar targets is in use, its utilization ratio only has 20-30%, that is, most target is wasted, thus virtually adds production cost.In order to improve the utilization ratio of target and reduce enterprise's production cost, the target type body that people begin one's study new, and find that the utilization ratio of rotary target is very high, can reach 70-80%, high utilization rate can reduce the cost of derived product, simultaneously more environmental protection and save material.
The production of Rotary niobium oxide target material mainly adopts spraying coating process at present, and utilize the target of this explained hereafter, density is lower, is generally all less than 80%, in use easily causes sparking, falls slag, and then affects quality and the yield rate of derived product; And, by the restriction of hot pressing furnace size and graphite jig size, the height of the Rotary niobium oxide target material adopting pressure sintering to prepare is less, be generally less than 100mm, and the rotary target of 1500mm is reached for length easily, usually need by 15 height be 100mm pipe target splicing after just can use, cause piece more, affect coated product quality.Because above-mentioned deficiency limit, on market, some producers high to sputtering specification of quality all adopt external rotary target material, and cost is high, usually under one's control.Therefore, a kind of rotary target material technique preparing high compactness is urgently developed, to meet the market requirement of current expanding day.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide that a kind of density is high, the Rotary niobium oxide target material of good conductivity.In addition, another object of the present invention is to the preparation method that this rotary target material a kind of is provided.
As an object of the present invention, the invention provides that a kind of density is high, the Rotary niobium oxide target material of good conductivity, its density>=4.5g/cm
3, resistivity≤2.0 × 10
-3Ω cm.
Further, the height of Rotary niobium oxide target material of the present invention can reach >=300mm.
Another object of the present invention is to, provide a kind of preparation method with the Rotary niobium oxide target material of characteristic described above, its preparation process comprises:
1) powder preparation: niobium oxides powder and metal niobium powder are mixed, and under the rotating speed of 2000-6000rpm fine grinding 3-10 hour;
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) cold isostatic compaction: by step 3) in dried powder 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 Rotary niobium oxide target material.
Preferably: described step 1), mixing niobium amount is 0.1%-10%, that is:, in described powder mixture, the amount of metal niobium powder is 0.1-10% (wt%);
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.
The particle diameter of the mixed powder preferably: step 1) after fine grinding is 30-150nm;
Vacuum calcining preferably: step 2), vacuum tightness is 1-1000Pa, 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
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; And, the defect that restriction that Rotary niobium oxide target material is vulnerable to equipment size causes the height < 100mm of target is prepared relative to adopting pressure sintering, method of the present invention is not by the impact of equipment size, utilize different moulds can obtain the target of different size, the height of target can reach more than 300mm.
Embodiment
Below in conjunction with specific embodiment and specific embodiment, the specific embodiment of the present invention is described further.
The present invention adopts atmosphere sintering legal system for Rotary niobium oxide target material, 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) cold isostatic compaction: by step 3) in dried powder 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 Rotary niobium oxide target material of the present invention.
Further, step 1) described in powder preparation process in, mixing niobium amount is 0.1%-10%, that is:, in described mixed powder, the amount of metal niobium powder is 0.1-10% (wt%); And purity >=99.99% of described niobium oxides powder, particle diameter is 0.5-10 μm; Purity >=99.95% of described metal niobium powder, particle diameter is 1-50 μm; Further, step 1) in the particle diameter of mixed powder after fine grinding be 30-150nm: step 2) described in powder calcination step in, vacuum tightness is 1-1000Pa, 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, pass into argon gas subsequently or nitrogen 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 Rotary niobium oxide target material, 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 0.8 μm and 1kg purity are 99.99%, particle diameter is 30 μm mixes, and by the material ball ratio of 2:1 in nano-level grinder under the rotating speed of 5000rpm fine grinding 5h be 80nm 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 500 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) cold isostatic compaction: by step 3) in dried powder put into cold isostatic press and be carried out at cold isostatic compaction under 260MPa;
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 500Kpa, 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 4.53g/cm
3, resistivity is 1.7 × 10
-3Ω cm, carries out precision work according to desired size to rotary target base, must meet the Rotary niobium oxide target material that dimensions requires.
Embodiment 2
A preparation method for Rotary niobium oxide target material, 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 6 μm and 0.06kg 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 3500rpm fine grinding 8h be 50nm 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 220 DEG C;
4) cold isostatic compaction: by step 3) in dried powder load in cold isostatic press and be carried out at cold isostatic compaction under 210MPa;
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 800Kpa, and continue to be warming up to 1300 DEG C with the temperature rise rate of 150 DEG C/h, and be incubated 4 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 4.62g/cm
3, resistivity is 1.9 × 10
-3Ω cm, carries out precision work according to desired size to rotary target base, must meet the Rotary niobium oxide target material that dimensions requires.
Embodiment 3
A preparation method for Rotary niobium oxide target material, 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 3 μm and 2kg purity are 99.99%, particle diameter is 45 μm mixes, and by the material ball ratio of 2:1 in nano-level grinder under the rotating speed of 5500rpm fine grinding 4h be 120nm 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 500Pa, calcining temperature 600 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) cold isostatic compaction: by step 3) in dried powder load in cold isostatic press and be 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 4.70g/cm
3, resistivity is 1.2 × 10
-3Ω cm, carries out precision work according to desired size to rotary target base, must meet the Rotary niobium oxide target material 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.Being intended that all these changes and increasing of applicant has 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 Rotary niobium oxide target material, is characterized in that: the density>=4.5g/cm of described Rotary niobium oxide target material
3, resistivity≤2.0 × 10
-3Ω cm.
2. Rotary niobium oxide target material according to claim 1, is characterized in that: the height >=300mm of described Rotary niobium oxide target material.
3. a preparation method for Rotary niobium oxide target material as claimed in claim 1 or 2, is characterized in that: comprise the following steps:
1) powder preparation: niobium oxides powder and metal niobium powder are mixed, and under the rotating speed of 2000-6000rpm fine grinding 3-10 hour;
2) powder calcination: to step 1) in mixed powder after fine grinding carry out vacuum calcining;
3) granulation: to step 2) in calcining after powder carry out granulation process and drying treatment;
4) cold isostatic compaction: by step 3) in dried powder 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 Rotary niobium oxide target material.
4. preparation method according to claim 3, is characterized in that: described step 1) in, the weight of metal niobium powder is the 0.1%-10% of total powder mixture weight.
5. the preparation method according to claim 3 or 4, 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.
6. preparation method according to claim 3, is characterized in that: step 1) in the particle diameter of powder mixture after fine grinding be 30-150nm.
7. preparation method according to claim 3, is characterized in that: step 2) described in vacuum calcining, vacuum tightness is 1-1000Pa, and calcining temperature is 300-600 DEG C, and calcination time is 2-5 hour.
8. preparation method according to claim 3, is characterized in that: step 3) described in granulation process in, add binding agent.
9. preparation method according to claim 8, 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.
10. preparation method according to claim 3, 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.
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Cited By (6)
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| CN105734506A (en) * | 2016-03-28 | 2016-07-06 | 航天材料及工艺研究所 | Method for preparing hot isostatic pressing niobium oxide target material |
| 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 |
| CN110218090A (en) * | 2019-06-25 | 2019-09-10 | 宋伟杰 | The preparation method of Rotary niobium oxide target material |
| 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 |
| 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 |
| CN114956823A (en) * | 2022-05-27 | 2022-08-30 | 先导薄膜材料（广东）有限公司 | Preparation method of conductive cadmium telluride target |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105734506A (en) * | 2016-03-28 | 2016-07-06 | 航天材料及工艺研究所 | Method for preparing hot isostatic pressing niobium oxide target material |
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| CN110218090B (en) * | 2019-06-25 | 2021-12-24 | 宋伟杰 | Preparation method of niobium oxide rotary target material |
| 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 |
| 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 |
| CN114956823A (en) * | 2022-05-27 | 2022-08-30 | 先导薄膜材料（广东）有限公司 | Preparation method of conductive cadmium telluride target |
| CN114956823B (en) * | 2022-05-27 | 2024-02-27 | 先导薄膜材料（广东）有限公司 | Preparation method of conductive cadmium telluride target |
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Effective date of registration: 20200812 Address after: 1 Hengda street, Yangzhen District, Shunyi District, Beijing Patentee after: BEIJING YEKE MAGNETIC MATERIAL Co.,Ltd. Address before: 101100, Beijing, Tongzhou District Economic Development Zone, five beautiful East Street 06 Patentee before: BEIJING YEKE NANO TECH Co.,Ltd. |
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