CN106544632A - A kind of tungsten niobium alloy target processing method - Google Patents
A kind of tungsten niobium alloy target processing method Download PDFInfo
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- CN106544632A CN106544632A CN201610656527.9A CN201610656527A CN106544632A CN 106544632 A CN106544632 A CN 106544632A CN 201610656527 A CN201610656527 A CN 201610656527A CN 106544632 A CN106544632 A CN 106544632A
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- Prior art keywords
- target
- protective layer
- sand blasted
- blasted area
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
Abstract
The invention discloses a kind of tungsten niobium alloy target processing method, processing technology is simple, quality of finished product good, high comprehensive performance, preferably to carry out blasting treatment to the part surface of target, while not interfering with other of target does not need the part of sandblasting.
Description
Technical field
The present invention relates to alloy material manufacture field, and in particular to a kind of tungsten niobium alloy target processing method.
Background technology
In recent years, growing with sputtering target material and sputtering technology, sputtering target material is served more in sputtering technology
Carry out more important effect, the quality of sputtering target material has directly influenced the quality of forming film after sputtering.Sputtering target material is broadly divided into flat
Face target and target, the target are generally made up of sputtering target material and penstock, compared with flat target, the utilization rate of target it is higher and
After sputtering, quality of forming film more preferably, has huge development potentiality in target market.Tungsten niobium hard alloy has high intensity, height hard
The features such as degree, excellent wearability, thermostability and good corrosion resistance, therefore it is widely used in high pressure, high rotating speed, height
The working environments such as temperature, Korrosionsmedium.
For now, tungsten niobium target not only to compactness, hardness and can processing type have very high requirement, while to material
Interior tissue uniformity also have very high requirement.
As the particulate matter that sputtering is produced in sputter procedure, can be left on the edge of target, these particulate matters are gradually
Accumulation becomes deposit.Deposit is assembled on target, peeling it is heavy
Product thing can not only affect to sputter environment, be also easy to drop on product surface, cause product defective or even scrap.For this purpose, existing
There is technology that blasting treatment can be carried out to the part non-sputtered region of target, so part surface through sandblasting becomes coarse, enters
And become easily to adsorb deposit, reduce peeling phenomenon odds.
The content of the invention
The present invention provides a kind of tungsten niobium alloy target processing method, and processing technology is simple, and quality of finished product good, combination property are excellent
It is good, preferably to carry out blasting treatment to the part surface of target, while do not interfere with target other do not need sandblasting portion
Point.
To achieve these goals, the invention provides a kind of tungsten niobium alloy target processing method, the method includes as follows
Step:
(1)Prepare target
Adopt tungsten powder with niobium powder to make raw material, its each component mass percent is tungsten powder:85%-95%, niobium powder:5%-15%;
Tungsten powder purity >=99.99%, granularity are 2-3 μm, and niobium powder purity >=99.99%, granularity are 3-8 μm;
The raw material for choosing aforementioned proportion loads batch mixer, and batch mixer adjustment of rotational speed to 1000-1500 is turned/min, and start is rotated forward
After 6-8h, invert 10-15h, shut down afterwards powder is standby;
Gained powder is loaded in tubular rubber die sleeve, is pressed with cold isostatic press, pressure is 250-300MPa, pressure
Target material blank body is obtained after 20-40 minutes processed standby;
Gained target material blank body is put in sintering furnace heated up stage by stage, heat preservation sintering, the first stage:700 are risen to by room temperature
DEG C, the heating-up time is 5h, and furnace temperature is incubated 7h after rising to 700 DEG C;Second stage:1000 DEG C are risen to by 700 DEG C, the heating-up time is
4h, furnace temperature are incubated 2h after rising to 1000 DEG C;Phase III:1250 DEG C are risen to by 1000 DEG C, the heating-up time is 2h, furnace temperature rises to
1h is incubated after 1250 DEG C;Fourth stage:1600 DEG C are risen to by 1250 DEG C, the heating-up time is 5h, furnace temperature is incubated after rising to 1600 DEG C
2h;5th stage:1850 DEG C are risen to by 1600 DEG C, the heating-up time is 2h, furnace temperature is incubated 4h after rising to 2000 DEG C;So far it is sintered
After the completion of journey, gained metal body is taken out, using recirculated water cooling down to standby after room temperature;
Metal body after gained is cooled down is heated to 1350 DEG C -1600 DEG C, and keeps in this temperature range entering which
Row hot rolling treatment, its thickness is rolled to after 5-100mm, room temperature is naturally cooled to, and obtains target blank;
The surfaces externally and internally of gained target blank is carried out into rough turn, fine grinding, target is obtained;
(2)Blasting treatment
The tungsten niobium alloy target is provided, the target includes treating sand blasted area and do not need the reservation region of sandblasting;
At least in the reservation region near the part for treating sand blasted area, and part treats that protective layer is pasted in sand blasted area;
Remove positioned at treating the protective layer of sand blasted area, sand blasted area is treated be completely exposed target;
Sand blasted area carries out blasting treatment is treated to target;
After the step of blasting treatment, remaining protective layer on target is removed.
Preferably, in the step(2)In, there is provided include the step of the tungsten niobium alloy target:Remove to be located at and treat sandblasting
The step of protective layer in region, includes:The protective layer for treating sand blasted area is removed by the way of milling;
Wherein, removal is located at the step for the treatment of the protective layer of sand blasted area and includes:In lathe tool and the target material surface for pasting matcoveredn
Between the gap for being not more than protective layer thickness is set, make the gap in the range of 0.02mm~0.04mm;
Remove after the step for the treatment of the protective layer of sand blasted area, the step of carry out blasting treatment before, the target processing
Method also includes:Using blade for target treats that sandblasting region surface carries out process of removing photoresist;
After the step of pasting protective layer, the step of carry out blasting treatment before, the target processing method also includes:Using lid
Plate is not pasted the part of protective layer and is blocked to reservation region.
It is an advantage of the current invention that processing technology is simple, and quality of finished product good, high comprehensive performance, with the portion preferably to target
Point surface carries out blasting treatment, while not interfering with other of target does not need the part of sandblasting.
Specific embodiment
Embodiment one
Prepare target
Tungsten powder and niobium powder are adopted to make raw material, its each component mass percent is tungsten powder 95%, niobium powder:5%;The tungsten powder is pure
Degree >=99.99%, granularity is 2-3 μm, and niobium powder purity >=99.99%, granularity are 3-8 μm;Choose the raw material of aforementioned proportion
Load batch mixer, by batch mixer adjustment of rotational speed to 1000 turns/min, after start rotates forward 6h, invert 10h, shut down afterwards powder is standby
With.
Gained powder is loaded in tubular rubber die sleeve, is pressed with cold isostatic press, pressure is 250MPa, pressure
System obtains target material blank body after 20 minutes standby.
Gained target material blank body is put in sintering furnace heated up stage by stage, heat preservation sintering, the first stage:Risen to by room temperature
700 DEG C, the heating-up time is 5h, and furnace temperature is incubated 7h after rising to 700 DEG C;Second stage:1000 DEG C are risen to by 700 DEG C, the heating-up time
For 4h, furnace temperature is incubated 2h after rising to 1000 DEG C;Phase III:1250 DEG C are risen to by 1000 DEG C, the heating-up time is 2h, furnace temperature rises to
1h is incubated after 1250 DEG C;Fourth stage:1600 DEG C are risen to by 1250 DEG C, the heating-up time is 5h, furnace temperature is incubated after rising to 1600 DEG C
2h;5th stage:1850 DEG C are risen to by 1600 DEG C, the heating-up time is 2h, furnace temperature is incubated 4h after rising to 2000 DEG C;So far it is sintered
After the completion of journey, gained metal body is taken out, using recirculated water cooling down to standby after room temperature.
Metal body after gained is cooled down is heated to 1350 DEG C, and keeps carrying out heat to which in this temperature range
Process is rolled, its thickness is rolled to after 5-100mm, room temperature is naturally cooled to, obtain target blank;By the interior appearance of gained target blank
Face carries out rough turn, fine grinding, obtains target.
Blasting treatment
The tungsten niobium alloy target is provided, the target includes treating sand blasted area and do not need the reservation region of sandblasting;At least
In the reservation region near the part for treating sand blasted area, and part treats that protective layer is pasted in sand blasted area;Remove positioned to be painted
The protective layer in sand region, treats sand blasted area be completely exposed target;Sand blasted area carries out blasting treatment is treated to target;In spray
After the step of sand is processed, remaining protective layer on target is removed.
Preferably, there is provided include the step of the tungsten niobium alloy target:Remove the step positioned at the protective layer for treating sand blasted area
Suddenly include:The protective layer for treating sand blasted area is removed by the way of milling.
Wherein, removal is located at the step for the treatment of the protective layer of sand blasted area and includes:In lathe tool and the target for pasting matcoveredn
The gap for being not more than protective layer thickness is set between surface, the gap is made in the range of 0.02mm~0.04mm.
Remove after the step for the treatment of the protective layer of sand blasted area, the step of carry out blasting treatment before, the target
Processing method also includes:Using blade for target treats that sandblasting region surface carries out process of removing photoresist.
After the step of pasting protective layer, the step of carry out blasting treatment before, the target processing method also includes:Adopt
Block the part that protective layer is not pasted to reservation region with cover plate.
Embodiment two
Prepare target
Adopt tungsten powder with niobium powder to make raw material, its each component mass percent is tungsten powder:85%, niobium powder: 15%;The tungsten
Powder purity >=99.99%, granularity are 2-3 μm, and niobium powder purity >=99.99%, granularity are 3-8 μm;Choose the original of aforementioned proportion
Material loads batch mixer, by batch mixer adjustment of rotational speed to 1500 turns/min, after start rotates forward 8h, inverts 15h, shuts down to obtain powder afterwards
Material is standby.
Gained powder is loaded in tubular rubber die sleeve, is pressed with cold isostatic press, pressure is 300MPa, pressure
System obtains target material blank body after 40 minutes standby.
Gained target material blank body is put in sintering furnace heated up stage by stage, heat preservation sintering, the first stage:Risen to by room temperature
700 DEG C, the heating-up time is 5h, and furnace temperature is incubated 7h after rising to 700 DEG C;Second stage:1000 DEG C are risen to by 700 DEG C, the heating-up time
For 4h, furnace temperature is incubated 2h after rising to 1000 DEG C;Phase III:1250 DEG C are risen to by 1000 DEG C, the heating-up time is 2h, furnace temperature rises to
1h is incubated after 1250 DEG C;Fourth stage:1600 DEG C are risen to by 1250 DEG C, the heating-up time is 5h, furnace temperature is incubated after rising to 1600 DEG C
2h;5th stage:1850 DEG C are risen to by 1600 DEG C, the heating-up time is 2h, furnace temperature is incubated 4h after rising to 2000 DEG C;So far it is sintered
After the completion of journey, gained metal body is taken out, using recirculated water cooling down to standby after room temperature.
Metal body after gained is cooled down is heated to 1350 DEG C -1600 DEG C, and keeps right in this temperature range
Which carries out hot rolling treatment, and its thickness is rolled to after 5-100mm, room temperature is naturally cooled to, and obtains target blank;By gained target blank
Surfaces externally and internally carry out rough turn, fine grinding, obtain target.
Blasting treatment
The tungsten niobium alloy target is provided, the target includes treating sand blasted area and do not need the reservation region of sandblasting;At least
In the reservation region near the part for treating sand blasted area, and part treats that protective layer is pasted in sand blasted area;Remove positioned to be painted
The protective layer in sand region, treats sand blasted area be completely exposed target;Sand blasted area carries out blasting treatment is treated to target;In spray
After the step of sand is processed, remaining protective layer on target is removed.
Preferably, there is provided include the step of the tungsten niobium alloy target:Remove the step positioned at the protective layer for treating sand blasted area
Suddenly include:The protective layer for treating sand blasted area is removed by the way of milling.
Wherein, removal is located at the step for the treatment of the protective layer of sand blasted area and includes:In lathe tool and the target for pasting matcoveredn
The gap for being not more than protective layer thickness is set between surface, the gap is made in the range of 0.02mm~0.04mm.
Remove after the step for the treatment of the protective layer of sand blasted area, the step of carry out blasting treatment before, the target
Processing method also includes:Using blade for target treats that sandblasting region surface carries out process of removing photoresist.
After the step of pasting protective layer, the step of carry out blasting treatment before, the target processing method also includes:Adopt
Block the part that protective layer is not pasted to reservation region with cover plate.
Claims (2)
1. a kind of tungsten niobium alloy target processing method, the method comprise the steps:
(1)Prepare target
Adopt tungsten powder with niobium powder to make raw material, its each component mass percent is tungsten powder:85%-95%, niobium powder:5%-15%;
Tungsten powder purity >=99.99%, granularity are 2-3 μm, and niobium powder purity >=99.99%, granularity are 3-8 μm;
The raw material for choosing aforementioned proportion loads batch mixer, and batch mixer adjustment of rotational speed to 1000-1500 is turned/min, and start is rotated forward
After 6-8h, invert 10-15h, shut down afterwards powder is standby;
Gained powder is loaded in tubular rubber die sleeve, is pressed with cold isostatic press, pressure is 250-300MPa, pressure
Target material blank body is obtained after 20-40 minutes processed standby;
Gained target material blank body is put in sintering furnace heated up stage by stage, heat preservation sintering, the first stage:700 are risen to by room temperature
DEG C, the heating-up time is 5h, and furnace temperature is incubated 7h after rising to 700 DEG C;Second stage:1000 DEG C are risen to by 700 DEG C, the heating-up time is
4h, furnace temperature are incubated 2h after rising to 1000 DEG C;Phase III:1250 DEG C are risen to by 1000 DEG C, the heating-up time is 2h, furnace temperature rises to
1h is incubated after 1250 DEG C;Fourth stage:1600 DEG C are risen to by 1250 DEG C, the heating-up time is 5h, furnace temperature is incubated after rising to 1600 DEG C
2h;5th stage:1850 DEG C are risen to by 1600 DEG C, the heating-up time is 2h, furnace temperature is incubated 4h after rising to 2000 DEG C;So far it is sintered
After the completion of journey, gained metal body is taken out, using recirculated water cooling down to standby after room temperature;
Metal body after gained is cooled down is heated to 1350 DEG C -1600 DEG C, and keeps in this temperature range entering which
Row hot rolling treatment, its thickness is rolled to after 5-100mm, room temperature is naturally cooled to, and obtains target blank;
The surfaces externally and internally of gained target blank is carried out into rough turn, fine grinding, target is obtained;
(2)Blasting treatment
The tungsten niobium alloy target is provided, the target includes treating sand blasted area and do not need the reservation region of sandblasting;
At least in the reservation region near the part for treating sand blasted area, and part treats that protective layer is pasted in sand blasted area;
Remove positioned at treating the protective layer of sand blasted area, sand blasted area is treated be completely exposed target;
Sand blasted area carries out blasting treatment is treated to target;
After the step of blasting treatment, remaining protective layer on target is removed.
2. the method for claim 1, it is characterised in that in the step(2)In, there is provided the tungsten niobium alloy target
Step includes:Removal is located at the step for the treatment of the protective layer of sand blasted area to be included:Sandblasting area is treated described in removing by the way of milling
The protective layer in domain;
Wherein, removal is located at the step for the treatment of the protective layer of sand blasted area and includes:In lathe tool and the target material surface for pasting matcoveredn
Between the gap for being not more than protective layer thickness is set, make the gap in the range of 0.02mm~0.04mm;
Remove after the step for the treatment of the protective layer of sand blasted area, the step of carry out blasting treatment before, the target processing
Method also includes:Using blade for target treats that sandblasting region surface carries out process of removing photoresist;
After the step of pasting protective layer, the step of carry out blasting treatment before, the target processing method also includes:Using lid
Plate is not pasted the part of protective layer and is blocked to reservation region.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111378936A (en) * | 2018-12-27 | 2020-07-07 | 合肥江丰电子材料有限公司 | Manufacturing method of target assembly |
CN112593195A (en) * | 2020-11-25 | 2021-04-02 | 宝鸡同盈稀有金属有限公司 | Production method of tantalum and niobium tubular target |
CN114714257A (en) * | 2022-03-21 | 2022-07-08 | 合肥江丰电子材料有限公司 | Sand blasting method for target material |
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CN102699326A (en) * | 2012-01-04 | 2012-10-03 | 洛阳科威钨钼有限公司 | Process for manufacturing large, single and heavy tungsten plate |
CN103255379A (en) * | 2013-04-16 | 2013-08-21 | 洛阳高新四丰电子材料有限公司 | Molybdenum-tungsten alloy sputtering target material for flat panel display and preparation method thereof |
CN104439247A (en) * | 2014-12-30 | 2015-03-25 | 山东昊轩电子陶瓷材料有限公司 | Molybdenum alloy target preparation method |
CN105695943A (en) * | 2014-11-28 | 2016-06-22 | 宁波江丰电子材料股份有限公司 | Target processing method |
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CN102139371A (en) * | 2011-05-04 | 2011-08-03 | 佛山市钜仕泰粉末冶金有限公司 | Tungsten alloy target material and preparation method thereof |
CN102699326A (en) * | 2012-01-04 | 2012-10-03 | 洛阳科威钨钼有限公司 | Process for manufacturing large, single and heavy tungsten plate |
CN103255379A (en) * | 2013-04-16 | 2013-08-21 | 洛阳高新四丰电子材料有限公司 | Molybdenum-tungsten alloy sputtering target material for flat panel display and preparation method thereof |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN111378936A (en) * | 2018-12-27 | 2020-07-07 | 合肥江丰电子材料有限公司 | Manufacturing method of target assembly |
CN112593195A (en) * | 2020-11-25 | 2021-04-02 | 宝鸡同盈稀有金属有限公司 | Production method of tantalum and niobium tubular target |
CN114714257A (en) * | 2022-03-21 | 2022-07-08 | 合肥江丰电子材料有限公司 | Sand blasting method for target material |
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Application publication date: 20170329 |