CN104973864B - A kind of preparation method and niobium oxide planar targets of niobium oxide planar targets - Google Patents
A kind of preparation method and niobium oxide planar targets of niobium oxide planar targets Download PDFInfo
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- CN104973864B CN104973864B CN201510398196.9A CN201510398196A CN104973864B CN 104973864 B CN104973864 B CN 104973864B CN 201510398196 A CN201510398196 A CN 201510398196A CN 104973864 B CN104973864 B CN 104973864B
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Abstract
The invention discloses a kind of preparation method of niobium oxide planar targets, its step includes：1) prepared by powder body：50 200nm are ground to by niobium oxide powder body and metal niobium powder body mix homogeneously and by the particle diameter of powder mixture；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) molding：By step 3) in the preforming under 20 70MPa of dried powder body, subsequently by the base substrate of preforming under 200 300MPa cold isostatic compaction；5) atmosphere sintering：By step 4) in the biscuit that obtains of cold isostatic compaction atmosphere sintering process is carried out in atmosphere sintering furnace；6) target blankss polish：By step 5) in target blankss after sintered process be cooled to after room temperature, polish is carried out to target blankss by required size, the niobium oxide planar targets are obtained final product.The preparation method of the present invention has preparation process is simple, the characteristics of production efficiency is high.
Description
Technical field
The present invention relates to a kind of preparation method of magnetron sputtering target, and in particular to a kind of to be prepared using atmosphere sintering method
A kind of method of niobium oxide planar targets, moreover, it relates to niobium oxide flat target prepared by the preparation method
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, prepare mostly using vacuum hot-pressing.But
Using the method, niobium oxide target blankss thickness is larger, needs to cut open needed for blade technolgy processing reaches by machining in the course of processing
Thickness requirement.Current cuts open blade technolgy mainly using diamond wire saw and Wire EDM.As niobium oxide target belongs to
Ceramic product, hardness is bigger cause the less efficient of diamond wire saw；And, although niobium oxide target has certain leading
Electrically, but compared with metal targets, resistivity is still too high, causes Wire EDM less efficient.Therefore, using pressure sintering
When preparing niobium oxide target blankss, the operation for cuing open piece significantly reduces overall production efficiency.Therefore, need a kind of production effect of exploitation badly
Rate high oxidation niobium planar targets processing technique.
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 high niobium oxide planar targets of production efficiency
Preparation method.Additionally, another object of the present invention is to providing a kind of niobium oxide plane obtained by the preparation method processing
Target.
For achieving the above object, the present invention is employed the following technical solutions：
A kind of preparation method of niobium oxide planar targets, its preparation process include：
1) prepared by powder body：It is ground to by niobium oxide powder body and metal niobium powder body mix homogeneously and by the particle diameter of powder mixture
50-200nm；
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) molding：By step 3) in the preforming under 20-70MPa of dried powder body, subsequently by the base substrate of preforming in
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 niobium oxide planar targets.
Preferably：Step 1) described in powder mixture in, the amount of metal niobium powder body is 0.1-10% (wt%), i.e.,：
Niobium amount is mixed for 0.1%-10%；
Preferably：Step 1) in process of lapping be：The powder mixture is under the rotating speed of 2000-6000rpm
Fine grinding 3-10 hours；
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 2) described in vacuum calcining, vacuum is 100-1000Pa, and calcining heat is 300-600 DEG C,
Calcination 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 to 800 DEG C, and is incubated 3-5 hours, is 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.
Another object of the present invention is to a kind of niobium oxide planar targets obtained by the processing of above-mentioned preparation method are provided, its
Density >=4.5g/cm3, resistivity≤2.0 × 10-3Ω·cm。
The beneficial effects of the present invention is, the present invention significantly reduces gold by material powder is carried out 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 freely can be 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.
Specific embodiment
The specific embodiment of the present invention is described further with reference to specific embodiment.
The present invention prepares niobium oxide planar targets 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 press 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 and solutionizing are processed；
3) pelletize：Pelletize process and dried are carried out to the powder body after calcining using spray dryer；
4) molding：By step 3) in dried powder body be placed in moulding press the preforming under 20-70MPa, then will be pre-
The base substrate of molding is carried out at cold isostatic compaction under 200-300MPa in being put into cold isostatic press；
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, niobium oxide planar targets of the present invention are obtained final product.
Further, the step 1) in, in mixed powder, the amount of metal niobium powder body is 0.1-10% (wt%)；It is described
Purity >=99.99% of niobium oxide powder body, its particle diameter are 0.5-10 μm；Purity >=99.95% of the metal niobium powder body, its grain
Footpath is 1-50 μm；Further, step 1) in it is finely ground after mixed powder particle diameter be 50-200nm：Step 2) described in
In powder calcination step, vacuum is 100-1000Pa, and calcining heat is 300-600 DEG C, and calcination time is 2-5 hours；Step
3), during the pelletize described in is processed, binding agent, the binding agent preferably polyethylene alcohol or polyvinyl butyral resin are also added into, and are pressed
The percentage by weight meter of powder body, addition 1-5% of the binding agent；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 3-5 hours are incubated, being subsequently passed argon makes furnace pressure reach 200-1000Kpa, and is continued with the heating rate of 150 DEG C/h
1250-1450 DEG C is warming up to, and is incubated 3-7 hours.
Embodiment 1
A kind of preparation method of niobium oxide planar targets, which includes following preparation process：
1) prepared by powder body：20kg purity is niobium oxide powder body that 99.99%, particle diameter is 5 μm and 1kg purity is
99.99%th, particle diameter is 5 μm of metal niobium powder body mix homogeneously, and presses 2：1 material ball ratio is in nano-level grinder in 4500rpm
Rotating speed under fine grinding 4h to powder mixture particle diameter be 100nm；
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 450 DEG C of calcining heat and is processed so that solid state reaction and solutionizing are carried out 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, and subsequently the powder body after pelletize is done at 240 DEG C
Dry process；
4) molding：By step 3) in dried powder body load the preforming under 30MPa in moulding press, subsequently by preforming
Base substrate be put into cold isostatic press in be 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, in 0.01Pa
Under, 800 DEG C are warming up to the heating rate of 100 DEG C/h, and be incubated 3 hours, being subsequently slowly introducing argon reaches furnace pressure
800Kpa, 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 4.55g/cm3, resistivity is 1.68 × 10-3Ω cm, are carried out to rotating target blankss according to required size
Polish, obtains final product the niobium oxide planar targets for meeting dimensions requirement.
Embodiment 2
A kind of preparation method of niobium oxide planar targets, which includes following preparation process：
1) prepared by powder body：20kg purity is niobium oxide powder body that 99.99%, particle diameter is 1.5 μm and 0.05kg purity is
99.99%th, particle diameter is 35 μm of metal niobium powder body mix homogeneously, and presses 2：1 material ball ratio is in nano-level grinder in 3500rpm
Rotating speed under fine grinding 8h to powder mixture particle diameter be 150nm；
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 and is processed so that solid state reaction and solutionizing are carried out 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 butyral resin is used as binding agent, and its addition is the 1% of powder body amount, subsequently by the powder body after pelletize at 260 DEG C
It is dried process；
4) molding：By step 3) in dried powder body load the preforming under 60MPa in moulding press, subsequently by preforming
Base substrate be put into cold isostatic press in be 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, in 0.01Pa
Under, 800 DEG C are warming up to the heating rate of 60 DEG C/h, and be incubated 4 hours, being subsequently slowly introducing argon reaches furnace pressure
600Kpa, and 1300 DEG C are continuously heating to the heating rate of 150 DEG C/h, and it is incubated 6 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 4.54g/cm3, resistivity is 1.70 × 10-3Ω cm, are carried out to rotating target blankss according to required size
Polish, obtains final product the niobium oxide planar targets for meeting dimensions requirement.
Embodiment 3
A kind of preparation method of niobium oxide planar targets, which includes following preparation process：
1) prepared by powder body：20kg purity is niobium oxide powder body that 99.99%, particle diameter is 8.5 μm and 2kg purity is
99.99%th, particle diameter is 50 μm of metal niobium powder body mix homogeneously, and presses 2：1 material ball ratio is in nano-level grinder in 6000rpm
Rotating speed under fine grinding 4h to powder mixture particle diameter be 190nm；
2) powder calcination：By step 1) in mixed powder after fine grinding be placed in vacuum calcining stove, in vacuum 900Pa,
2h is calcined at 550 DEG C of calcining heat and is processed so that solid state reaction and solutionizing are carried out 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, and subsequently the powder body after pelletize is carried out at 260 DEG C
Dried；
4) molding：By step 3) in dried powder body load the preforming under 50MPa in moulding press, subsequently by preforming
Base substrate be put into cold isostatic press in 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, in 0.01Pa
Under, 800 DEG C are warming up to the heating rate of 180 DEG C/h, and be incubated 5 hours, 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 4.51g/cm3, resistivity is 1.92 × 10-3Ω cm, installing required size is carried out to rotating target blankss
Polish, obtains final product the niobium oxide planar targets 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 which is not intended to limit invention.Unless otherwise defined, all terms used herein (include 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 (8)
1. a kind of preparation method of niobium oxide planar targets, it is characterised in that：Comprise the following steps：
1) prepared by powder body：50- is ground to by niobium oxide powder body and metal niobium powder body mix homogeneously and by the particle diameter of powder mixture
200nm；
2) powder calcination：To step 1) in powder mixture after fine grinding carrying out vacuum calcining；
3) pelletize：To step 2) in calcining after powder mixture carry out pelletize process and dried；
4) molding：By step 3) in the preforming under 20-70MPa of dried powder body, subsequently by the base substrate of preforming in 200-
Cold isostatic compaction under 300MPa；
5) atmosphere sintering：By step 4) in the biscuit that obtains of cold isostatic compaction carry 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 niobium oxide planar targets；Wherein：
Step 2) described in vacuum calcining, vacuum is 100-1000Pa, and calcining heat is 300-600 DEG C, and calcination time is 2-5
Hour；
Step 3) described in dried temperature be 200-270 DEG C；
Step 5) described in atmosphere sintering processing procedure be：Under 0.01Pa, 800 are warming up to the heating rate of 50-200 DEG C/h
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.
2. preparation method according to claim 1, it is characterised in that：Step 1) described in powder mixture in, metal niobium
The amount of powder body is 0.1-10wt%.
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 1) in process of lapping be：Powder mixture
In the fine grinding 3-10 hours under the rotating speed of 2000-6000rpm.
5. preparation method according to claim 1, it is characterised in that：Step 3) described in pelletize process in, add viscous
Knot agent.
6. preparation method according to claim 5, 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.
7. a kind of niobium oxide planar targets, it is characterised in that：The niobium oxide planar targets are by the preparation side described in claim 1
Method processing is obtained.
8. niobium oxide planar targets according to claim 7, it is characterised in that：The density of the niobium oxide planar targets >=
4.5g/cm3, resistivity≤2.0 × 10-3Ω·cm。
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| 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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| 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 |
| DE102013016529A1 (en) * | 2013-10-07 | 2015-04-09 | Heraeus Deutschland GmbH & Co. KG | Metal oxide target and process for its preparation |
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