CN104961463B - 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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- CN104961463B CN104961463B CN201510397195.2A CN201510397195A CN104961463B CN 104961463 B CN104961463 B CN 104961463B CN 201510397195 A CN201510397195 A CN 201510397195A CN 104961463 B CN104961463 B CN 104961463B
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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, and in particular to a kind of Rotary niobium oxide target material, additionally, the present invention is also
It is related to a kind of method that utilization atmosphere sintering method prepares the Rotary niobium oxide target material, belongs to target manufacturing technology field.
Background technology
Niobium pentaoxide is widely used in many necks of modern technologies due to its unique physics and chemical property
Domain.For example, using its stronger ultraviolet absorption ability, the protecting film of ultraviolet sensitivity material can be used as；Using its thin film
The higher characteristic of refractive index, can be with SiO2The thin film with different refractivity can be prepared Deng coordinating.Due to these significant advantages,
Niobium pentaoxide target is widely used in solaode, liquid crystal display, ion display, collection touch screen, optics glass
The various fields such as glass, gas sensor.With the continuous development and the continuous extension of application of science and technology, niobium oxide target
Demand also constantly increases.
At present, use on market it is most be niobium oxide planar targets, although the technology of preparing of planar targets increasingly becomes
In maturation, but planar targets are in use, and its utilization rate only has 20-30%, that is, most target is wasted
Fall, so as to virtually increased production cost.In order to improve the utilization rate of target and reduce enterprise's production capacity, people start to grind
Study carefully new target type body, and find that the utilization rate of rotary target is very high, can reach 70-80%, high usage can reduce downstream product
The cost of product, while more environmentally friendly and saving material.
The production of Rotary niobium oxide target material is presently mainly to adopt spraying coating process, using the target of this technique productions, density
It is relatively low, generally less than 80%, easily cause sparking, scaling-off in use, so affect downstream product quality and into
Product rate；And, limited by hot pressing furnace size and graphite jig size, the height of the Rotary niobium oxide target material prepared using pressure sintering
Less, generally less than 100mm is spent, and for length easily is up to the rotary target of 1500mm, it usually needs by 15 height be 100mm
Pipe target splicing after just can use, cause piece more, affect coated product quality.Because above-mentioned deficiency is limited, one on market
A little all to adopt external rotary target material to sputtering the high producer of prescription, high cost is usually under one's control.It would therefore be highly desirable to open
Send out to prepare the rotary target material technique of high compactness a kind of, to meet the market demand of current expanding day.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, there is provided a kind of density is high, the rotation of the niobium oxide of good conductivity
Turn target.Additionally, another object of the present invention is to providing a kind of preparation method of the rotary target material.
As an object of the present invention, the invention provides a kind of density is high, the Rotary niobium oxide target material of good conductivity,
Its density >=4.5g/cm3, resistivity≤2.0 × 10-3Ω·cm。
Further, the height of Rotary niobium oxide target material of the invention can reach >=300mm.
Another object of the present invention is to, there is provided a kind of preparation side of the Rotary niobium oxide target material with character described above
Method, its preparation process includes：
1) prepared by powder body：By niobium oxide powder body and metal niobium powder body mix homogeneously, and under the rotating speed of 2000-6000rpm
Fine grinding 3-10 hours；
2) powder calcination：To step 1) in powder mixture after fine grinding carry out vacuum calcining；
3) pelletize：To step 2) in calcining after powder mixture carry out pelletize process and dried；
4) cold isostatic compaction：By step 3) in dried powder body cold isostatic compaction under 200-300MPa；
5) atmosphere sintering：By step 4) in the biscuit that obtains of cold isostatic compaction atmosphere sintering is carried out in atmosphere sintering furnace
Process；
6) target blankss polish：By step 5) in target blankss after sintered process be cooled to after room temperature, by required size to target
Base carries out polish, obtains final product described Rotary niobium oxide target material.
Preferably：The step 1) in, it is 0.1%-10% to mix niobium amount, i.e.,：In the powder mixture, metal niobium powder
The amount of body is 0.1-10% (wt%)；
Preferably：The particle diameter of the niobium oxide powder body is 0.5-10 μm；The particle diameter of the metal niobium powder body is 1-50 μm.
Preferably：Step 1) in it is finely ground after mixed powder particle diameter be 30-150nm；
Preferably：Step 2) described in vacuum calcining, vacuum is 1-1000Pa, and calcining heat is 300-600 DEG C, is forged
The burning time is 2-5 hours.
Preferably：Step 3) described in pelletize process in, add binding agent.
Preferably：The binding agent is polyvinyl alcohol or polyvinyl butyral resin, and its addition is mixed powder body weight
The 1-5% of amount.
Preferably：Step 5) described in atmosphere sintering processing procedure be：Under 0.01Pa, with the intensification of 50-200 DEG C/h
Ramp is incubated 3-5 hours to 800 DEG C, and being subsequently passed argon or nitrogen makes pressure reach 200-1000Kpa, and with 150
DEG C/heating rate of h is continuously heating to 1250-1450 DEG C, and is incubated 3-7 hours
The beneficial effects of the present invention is, the present invention significantly reduces gold by the way that material powder is carried out into nanorize process
The granularity of category niobium powder body, and cause more uniform, and then the so that conduction of target that metal niobium powder body be distributed in niobium oxide powder body
Property is higher.Furthermore, the atmosphere sintering process step of the present invention by the way of stagewise heats up, further improves the close of target
Degree.Additionally, the target blankss thickness of the present invention can freely set according to demand, and without the need for again as target blankss prepared by pressure sintering need to cut open
Piece operation, so as to production efficiency can be greatly enhanced；And, it is vulnerable to relative to Rotary niobium oxide target material is prepared using pressure sintering
The restriction of equipment size causes the defect of the height ＜ 100mm of target, the method for the present invention not to be affected by equipment size, utilizes
Different moulds can obtain various sizes of target, and the height of target is up to more than 300mm.
Specific embodiment
With reference to specific embodiment the specific embodiment of the present invention is described further with specific embodiment.
The present invention prepares Rotary niobium oxide target material using atmosphere sintering method, and its preparation process includes：
1) prepared by powder body：By niobium oxide powder body and metal niobium powder body mix homogeneously, and by material ball ratio 2：1 in nano-level grinder
In under the rotating speed of 2000-6000rpm fine grinding 3-10 hours；
2) powder calcination：By step 1) in mixed powder after fine grinding calcine in vacuum calcining stove it is solid to carry out to powder body
Phase reaction；
3) pelletize：Pelletize process and dried are carried out to the powder body after calcining using spray dryer；
4) cold isostatic compaction：By step 3) in dried powder body cold isostatic compaction under 200-300MPa；
5) atmosphere sintering：By step 4) in the biscuit that obtains of cold isostatic compaction atmosphere sintering is carried out in atmosphere sintering furnace
Process；
6) target blankss polish：By step 5) in target blankss after sintered process cool to the furnace after room temperature, by required size
Polish is carried out to target blankss, Rotary niobium oxide target material of the present invention is obtained final product.
Further, step 1) described in powder body preparation process in, mix niobium amount for 0.1%-10%, i.e.,：The mixed powder
In body, the amount of metal niobium powder body is 0.1-10% (wt%)；And purity >=99.99% of the niobium oxide powder body, particle diameter is
0.5-10μm；Purity >=99.95% of the metal niobium powder body, particle diameter is 1-50 μm；Further, step 1) in it is finely ground
The particle diameter of mixed powder afterwards is 30-150nm：Step 2) described in powder calcination step in, vacuum is 1-1000Pa, calcining
Temperature is 300-600 DEG C, and calcination time is 2-5 hours；Step 3) described in pelletize process in, be also added into binding agent, it is described
Binding agent preferably polyethylene alcohol or polyvinyl butyral resin, and based on the percentage by weight of powder body, the addition of the binding agent
1-5%；Step 3) in dried temperature be 200-270 DEG C；Step 5) described in atmosphere sintering processing procedure be：
Under 0.01Pa, 800 DEG C are warming up to the heating rate of 50-200 DEG C/h, and are incubated 3-5 hours, being subsequently passed argon or nitrogen makes
Furnace pressure reaches 200-1000Kpa, and is continuously heating to 1250-1450 DEG C with the heating rate of 150 DEG C/h, and is incubated 3-7
Hour.
Embodiment 1
A kind of preparation method of Rotary niobium oxide target material, it includes following preparation process：
1) prepared by powder body：20kg purity is niobium oxide powder body that 99.99%, particle diameter is 0.8 μm and 1kg purity is
99.99%th, particle diameter is 30 μm of metal niobium powder body mix homogeneously, and by 2：1 material ball ratio is in nano-level grinder in 5000rpm
Rotating speed under fine grinding 5h to powder mixture particle diameter be 80nm；
2) powder calcination：By step 1) in mixed powder after fine grinding be placed in vacuum calcining stove, in vacuum 100Pa,
3h is calcined at 500 DEG C of calcining heat to carry out solid state reaction to powder body；
3) pelletize：Pelletize process is carried out to the powder body after calcining using spray dryer, the pelletize is added in processing
Polyvinyl alcohol is used as binding agent, and its addition is the 3% of powder body amount, is subsequently done the powder body after pelletize at 240 DEG C
Dry process；
4) cold isostatic compaction：By step 3) in dried powder body be put in cold isostatic press be carried out at it is cold under 260MPa
Isostatic pressing；
5) atmosphere sintering：By step 4) in the biscuit that obtains of cold isostatic compaction be placed in atmosphere sintering furnace, in 0.01Pa
Under, 800 DEG C are warming up to the heating rate of 100 DEG C/h, and 3 hours are incubated, being subsequently slowly introducing argon reaches furnace pressure
500Kpa, and 1350 DEG C are continuously heating to the heating rate of 150 DEG C/h, and it is incubated 5 hours；
6) target blankss polish：By step 5) in target blankss after sintered process cool to the furnace after room temperature, Jing tests to obtain oxygen
The density for changing niobium target is 4.53g/cm3, resistivity is 1.7 × 10-3Ω cm, essence is carried out according to required size to rotating target blankss
Processing, obtains final product the Rotary niobium oxide target material for meeting dimensions requirement.
Embodiment 2
A kind of preparation method of Rotary niobium oxide target material, it includes following preparation process：
1) prepared by powder body：20kg purity is niobium oxide powder body that 99.99%, particle diameter is 6 μm and 0.06kg purity is
99.99%th, particle diameter is 5 μm of metal niobium powder body mix homogeneously, and by 2：1 material ball ratio is in nano-level grinder in 3500rpm
Rotating speed under fine grinding 8h to powder mixture particle diameter be 50nm；
2) powder calcination：By step 1) in mixed powder after fine grinding be placed in vacuum calcining stove, in vacuum 800Pa,
4h is calcined at 400 DEG C of calcining heat to carry out solid state reaction to powder body；
3) pelletize：Pelletize process is carried out to the powder body after calcining using spray dryer, the pelletize adds poly- in processing
Vinyl butyral is used as binding agent, and its addition is the 1% of powder body amount, subsequently enters the powder body after pelletize at 220 DEG C
Row dried；
4) cold isostatic compaction：By step 3) in dried powder body be fitted in cold isostatic press be carried out at it is cold under 210MPa
Isostatic pressing；
5) atmosphere sintering：By step 4) in the biscuit that obtains of cold isostatic compaction be placed in atmosphere sintering furnace, in 0.01Pa
Under, 800 DEG C are warming up to the heating rate of 60 DEG C/h, and 4 hours are incubated, being subsequently slowly introducing argon reaches furnace pressure
800Kpa, and 1300 DEG C are continuously heating to the heating rate of 150 DEG C/h, and it is incubated 4 hours；
6) target blankss polish：By step 5) in target blankss after sintered process cool to the furnace after room temperature, Jing tests to obtain oxygen
The density for changing niobium target is 4.62g/cm3, resistivity is 1.9 × 10-3Ω cm, essence is carried out according to required size to rotating target blankss
Processing, obtains final product the Rotary niobium oxide target material for meeting dimensions requirement.
Embodiment 3
A kind of preparation method of Rotary niobium oxide target material, it includes following preparation process：
1) prepared by powder body：20kg purity is niobium oxide powder body that 99.99%, particle diameter is 3 μm and 2kg purity is
99.99%th, particle diameter is 45 μm of metal niobium powder body mix homogeneously, and by 2：1 material ball ratio is in nano-level grinder in 5500rpm
Rotating speed under fine grinding 4h to powder mixture particle diameter be 120nm；
2) powder calcination：By step 1) in mixed powder after fine grinding be placed in vacuum calcining stove, in vacuum 500Pa,
2h is calcined at 600 DEG C of calcining heat to carry out solid state reaction to powder body；
3) pelletize：Pelletize process is carried out to the powder body after calcining using spray dryer, the pelletize is added in processing
Polyvinyl alcohol is used as binding agent, and its addition is the 4.5% of powder body amount, subsequently carries out the powder body after pelletize at 260 DEG C
Dried；
4) cold isostatic compaction：By step 3) in dried powder body be fitted in cold isostatic press be carried out at it is cold under 280MPa
Isostatic pressing；
5) atmosphere sintering：By step 4) in the biscuit that obtains of cold isostatic compaction be placed in atmosphere sintering furnace, in 0.01Pa
Under, 800 DEG C are warming up to the heating rate of 180 DEG C/h, and 5 hours are incubated, being subsequently slowly introducing nitrogen reaches furnace pressure
200Kpa, and 1450 DEG C are continuously heating to the heating rate of 150 DEG C/h, and it is incubated 7 hours；
6) target blankss polish：By step 5) in target blankss after sintered process cool to the furnace after room temperature, Jing tests to obtain oxygen
The density for changing niobium target is 4.70g/cm3, resistivity is 1.2 × 10-3Ω cm, essence is carried out according to required size to rotating target blankss
Processing, obtains final product the Rotary niobium oxide target material for meeting dimensions requirement.
The present invention is by preferred embodiment having carried out detailed explanation.However, by studying carefully above, to each
The change and increase of embodiment is also apparent to one of ordinary skill in the art.It is intended that it is all this
A little changes and increase fall in the protection domain of the claims in the present invention.Term used herein is only to specific enforcement
Example is illustrated, and it is not intended to limit invention.Unless otherwise defined, all terms used herein are (including skill
Art term and scientific terminology) it is identical with the understanding of those skilled in the art of the art.Known function or structure
For briefly and clearly considering or repeat no more.
Claims (5)
1. a kind of preparation method of Rotary niobium oxide target material, it is characterised in that：Comprise the following steps：
1）It is prepared by powder body：By niobium oxide powder body and metal niobium powder body mix homogeneously, and the fine grinding under the rotating speed of 2000-6000rpm
3-10 hours；
2）Powder calcination：To step 1）Mixed powder after middle fine grinding carries out vacuum calcining；
3）Pelletize：To step 2）Powder body after middle calcining carries out pelletize process and dried；
4）Cold isostatic compaction：By step 3）In dried powder body cold isostatic compaction under 200-300MPa；
5）Atmosphere sintering：By step 4）The biscuit that middle cold isostatic compaction is obtained is carried out at atmosphere sintering in atmosphere sintering furnace
Reason；
6）Target blankss polish：By step 5）In target blankss after sintered process be cooled to after room temperature, target blankss are entered by required size
Row polish, obtains final product described Rotary niobium oxide target material；Wherein：
Step 2）Described vacuum calcining, vacuum is 1-1000Pa, and calcining heat is 300-600 DEG C, and calcination time is that 2-5 is little
When；
Step 3）In baking temperature be 200-270 DEG C；
Step 5）Described atmosphere sintering processing procedure is：Under 0.01Pa, with the heating rate of 50-200 DEG C/h 800 are warming up to
DEG C, and 3-5 hours are incubated, being subsequently passed argon or nitrogen makes pressure reach 200-1000KPa, and with the intensification speed of 150 DEG C/h
Rate is continuously heating to 1250-1450 DEG C, and is incubated 3-7 hours；
Step 1）In it is finely ground after powder mixture particle diameter be 30-150nm；
Density >=the 4.5g/cm of obtained Rotary niobium oxide target material, resistivity≤2.0 × 10-3Ω ﹒ cm.
2. preparation method according to claim 1, it is characterised in that：The step 1）In, the weight of metal niobium powder body is
The 0.1%-10% of total powder mixture weight.
3. preparation method according to claim 1 and 2, it is characterised in that：The particle diameter of the niobium oxide powder body is 0.5-10 μ
m；The particle diameter of the metal niobium powder body is 1-50 μm.
4. preparation method according to claim 1, it is characterised in that：Step 3）During described pelletize is processed, add viscous
Knot agent.
5. preparation method according to claim 4, it is characterised in that：The binding agent is that polyvinyl alcohol or polyvinyl alcohol contract
Butyraldehyde, and its addition is the 1-5% of mixed powder weight.
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| CN105734506B (en) * | 2016-03-28 | 2019-01-15 | 航天材料及工艺研究所 | A kind of preparation method of hot isostatic pressing niobium oxide target |
| 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 |
| 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 |
| 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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| 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 |
| CN101705467A (en) * | 2009-05-14 | 2010-05-12 | 上海高展金属材料有限公司 | Method for preparing rotary ceramic target |
| KR101137913B1 (en) * | 2009-11-12 | 2012-05-03 | 삼성코닝정밀소재 주식회사 | Multi-phase NbOx sputtering target and method of fabricating the same |
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