CN102277558A - Process for manufacturing tungsten spin-coated sputtering tube target - Google Patents
Process for manufacturing tungsten spin-coated sputtering tube target Download PDFInfo
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- CN102277558A CN102277558A CN 201110242640 CN201110242640A CN102277558A CN 102277558 A CN102277558 A CN 102277558A CN 201110242640 CN201110242640 CN 201110242640 CN 201110242640 A CN201110242640 A CN 201110242640A CN 102277558 A CN102277558 A CN 102277558A
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Abstract
The invention discloses a process for manufacturing a tungsten spin-coated sputtering tube target. The process uses tungsten as a raw material, and comprises the following steps: filling a raw material into a rubber mold sleeve and preparing a hollow powder tungsten tube blank; forming in a cold isostatic press, placing a formed solid tube blank into a medium-frequency sintering furnace and keeping the formed blank body for later use; heating the formed blank to 1,300 to 1,700 DEG C for 1 to 3 hours, taking the blank out, and forging the blank with an air hammer till a tungsten rod is formed; boring, lathing an external circle and regulating the roughness of the surface to Ra1.6 to Ra3.2mu M; and thus, manufacturing the sputtering target tube. In the method, the simple manufacturing process with low equipment requirement ensures low cost, the prepared target is desirable in compactness and the relative density of the prepare target reaches over 99 percent.
Description
Technical field
The present invention relates to a kind of manufacture craft of sputter pipe target, a kind of specifically manufacture craft of sputter pipe target of tungsten rotary plating.
Background technology
Tungsten rotary plating sputter pipe target is mainly used in the plated film of photovoltaic element substrate, the physicals of this series products itself directly affects the use properties of plated film, for example: one, tungsten rotary plating sputter pipe target is in the process of sputter coating, when the less sputtering target of compactness is bombarded, because the gas that exists in the target internal void discharges suddenly, cause large-sized target particle or particulate to splash, or the film material is subjected to the particulate that secondary electron bombardment causes and splashes after the film forming, the appearance of these particulates all can reduce film quality, in order to reduce the pore in the target solid, improve film performance, the general requirement sputtering target material has higher density; Target atom is come out along the tightst orientation preferential sputtering of atom six sides easily during two, owing to sputter, therefore, for reaching the highest sputter rate, often increase sputter rate by the method that changes target crystalline texture, the crystallization direction of target is also bigger to the thickness evenness influence of sputtered layer, therefore, it is most important to the sputter procedure of film to obtain the target material structure of certain crystalline orientation.
At present, the external main preparation method of tungsten rotary plating sputter pipe target adopts the moulding process of extruding or drawing to carry out machine-shaping, after thermal treatment, machining and backboard are in conjunction with the tungsten sputter pipe target that forms, these class methods are to the equipment requirements height, complex process, cost is higher, and the target compactness difference and the grain fineness number of preparation are also bigger, use this product when plated film, the homogeneity of film and cloth line mass reduce greatly, therefore can't satisfy the photovoltaic product to the specific impedance of material and the new demand of membrane stress.
Summary of the invention
The objective of the invention is the deficiency for solving the problems of the technologies described above, a kind of manufacture craft of sputter pipe target of tungsten rotary plating is provided, its technology is simple, and is low for equipment requirements, and cost is low, and the relative density of the product of preparation reaches more than 99%.
The present invention is the deficiency that solves the problems of the technologies described above, and the technical scheme that is adopted is: a kind of manufacture craft of sputter pipe target of tungsten rotary plating, and the employing tungsten powder is a raw material, the purity of tungsten powder 〉=99.95%, granularity is at 2.6-3.3 μ m, and making step is as follows:
Step 1, raw material is packed in the rubber die sleeve, be prepared into hollow opaque tungsten pipe, adopt the cold isostatic press moulding then, pressure is 50-400Mpa, solid tube blank molding after 10-20 minutes;
Step 2, the solid pipe after the moulding is put into the intermediate frequency sintering oven, feed hydrogen in the stove, Heating temperature is 1900 °, and be 30 hours heat-up time, and cooling water circulation is adopted in the back, and postcooling to room temperature was finished in 8-16 hours, and molding blank is standby:
Step 3, the one-tenth parison after step 2 handled are heated to 1300 °-1700 °, be 1-3 hours heat-up time, taking out the back is that 750 kilograms air hammer forges 10-20 times with surging force, forge into and put into electrothermal oven tempering half hour behind the tungsten bar, tempering temperature is 450 °-500 °, and the back is standby:
Step 4, the tungsten bar after step 3 handled carry out mechanical workout, bore hole, turning, make surfaceness reach Ra1.6 ~ Ra3.2 μ m after, sputter pipe target completes.
Oxygen in the described raw material≤0.005%, sulphur≤0.003%, aluminium≤0.002%, iron≤0.005%, molybdenum≤0.01%, magnesium≤0.002%, nickel≤0.003%.
Tungsten rotary plating sputter pipe target is in the process of sputter coating; when the less sputtering target of compactness is bombarded; because the gas that exists in the target internal void discharges suddenly; cause large-sized target particle or particulate to splash; or the film material is subjected to the particulate that secondary electron bombardment causes and splashes after the film forming; the appearance of these particulates all can reduce film quality; in order to reduce the pore in the target solid; improve film performance; the general requirement sputtering target material has higher density, and the target relative density of present method preparation reaches more than 99%.
Because target atom is come out along the tightst orientation preferential sputtering of atom six sides easily during sputter, therefore, for reaching the highest sputter rate, often increase sputter rate by the method that changes target crystalline texture, the crystallization direction of target is also bigger to the thickness evenness influence of sputtered layer, therefore, the target material structure that obtains certain crystalline orientation is most important to the sputter procedure of film, present method adopts the target of high purity tungsten by the series of process preparation, not only satisfied the photovoltaic product to the specific impedance of material and the new demand of membrane stress, but also it is energy-saving and cost-reducing to be not busy, improved production efficiency, reduce cost, add simultaneously and make man-hour the crystal grain of tungsten realize secondary crystal in forging, refinement grain fineness number, changed the structure of crystal grain, the uniformity of film of LED industry glass substrate and cloth line mass have been had significantly improve, prolonged the work-ing life of LCD element.
Present method can keep the characteristics of mould shapes based on tungsten powder, and tungsten powder is prepared into hollow opaque tungsten pipe, has broken through with extruding abroad, and the moulding process of drawing has reduced the requirement to equipment, has reduced production cost.
Present method, behind the base material sintering of moulding, it is carried out secondary heating and forging, improved the bad profile of tungsten pipe behind the sintering, make it to have circularity and linearity preferably, the length of tungsten pipe is extended, make crystal grain produce secondary crystal, refinement grain fineness number, changed crystalline-granular texture, make tungsten pipe target possess higher intensity and density, use this product when the LED plated film, the homogeneity of film and cloth line mass improve greatly.
The invention has the beneficial effects as follows:
1, present method manufacture craft is simple, and is not high to equipment requirements, so input cost is lower, and the target compactness of preparing is better, and relative density reaches more than 99%; Present method has changed external production technique based on extruding, drawing simultaneously, make tungsten pipe recrystallize in the secondary hot environment simultaneously, grain refining, grain fineness number is reduced to micron order by the millimeter level, optimized crystalline-granular texture, use this product when the LED plated film, the homogeneity of film and cloth line mass improve greatly.Not only improved simultaneously the compactness of pipe target in present method forging process, and less demanding to equipment, technology is reasonable, and yield rate is higher, has realized low cost, and high benefit has satisfied the photovoltaic product to the specific impedance of material and the new demand of membrane stress.
2, present method, in the sintering stage of step 2, by control optimum temps and optimum handling time, and the progressive cooling of recirculated water cooling guarantees that the one-tenth parison behind the sintering has higher density, has circularity and linearity preferably simultaneously; In the forging stage of step 3, make the crystallization once more of tungsten pipe by the secondary hot environment, crystalline-granular texture has been optimized in grain refining, has improved the use properties of sputter pipe target.
Embodiment
A kind of manufacture craft of sputter pipe target of tungsten rotary plating, the employing tungsten powder is a raw material, tungsten powder
Purity 〉=99.95%, granularity is at 2.6-3.3 μ m, hardness HV200-235, making step is as follows:
Step 1, raw material is packed in the rubber die sleeve, be prepared into hollow opaque tungsten pipe, adopt the cold isostatic press moulding then, pressure is 50-400Mpa, solid tube blank molding after 10-20 minutes;
Step 2, the solid pipe after the moulding is put into the intermediate frequency sintering oven, feed hydrogen in the stove, Heating temperature is 1900 °, and be 30 hours heat-up time, and cooling water circulation is adopted in the back, and postcooling to room temperature was finished in 8-16 hours, and molding blank is standby:
Step 3, the one-tenth parison after step 2 handled are heated to 1300 °-1700 °, be 1-3 hours heat-up time, taking out the back is that 750 kilograms air hammer forges 10-20 times with surging force, forge into and put into electrothermal oven tempering half hour behind the tungsten bar, tempering temperature is 450 °-500 °, and the back is standby:
Step 4, the tungsten bar after step 3 handled carry out mechanical workout, bore hole, turning, make surfaceness reach Ra1.6 ~ Ra3.2 μ m after, sputter pipe target completes.
Oxygen in the described raw material≤0.005%, sulphur≤0.003%, aluminium≤0.002%, iron≤0.005%, molybdenum≤0.01%, magnesium≤0.002%, nickel≤0.003%, determine in the raw material harmful element and limit the quantity of through overtesting, guaranteed that the chemical property of tungsten rotary plating sputter pipe target is more stable.
Embodiment one:
A kind of manufacture craft of sputter pipe target of tungsten rotary plating, the employing tungsten powder is a raw material, tungsten powder
Purity 〉=99.95%, granularity is at 2.6 μ m, hardness HV200, making step is as follows:
Step 1, raw material is packed in the rubber die sleeve, be prepared into hollow opaque tungsten pipe, adopt the cold isostatic press moulding then, pressure is 50Mpa, solid tube blank molding after 20 minutes;
Step 2, the solid pipe after the moulding is put into the intermediate frequency sintering oven, feeds hydrogen in the stove,
Guarantee that pipe heats in the atmosphere of hydrogen, Heating temperature is 1900 °, and be 30 hours heat-up time, and cooling water circulation is adopted in the back, and postcooling to room temperature was finished in 8 hours, and molding blank is standby:
Step 3, the one-tenth parison after step 2 handled are heated to 1300 °, be 3 hours heat-up time, and taking out the back is that 750 kilograms air hammer forges 10 times with surging force, forges into to put into electrothermal oven tempering half hour behind the tungsten bar, tempering temperature is 450 °, and the back is standby:
Step 4, the tungsten bar after step 3 handled carry out mechanical workout, right boring endoporus and finish turning cylindrical, caliber behind aperture and the finish turning is set according to customer demand and pipe target model, and the processing back guarantees that sputter pipe target all surface roughness reaches Ra1.6 ~ Ra3.2 μ m, completes.
Oxygen in the described raw material≤0.005%, sulphur≤0.003%, aluminium≤0.002%, iron≤0.005%, molybdenum≤0.01%, magnesium≤0.002%, nickel≤0.003%.
Embodiment two:
A kind of manufacture craft of sputter pipe target of tungsten rotary plating, the employing tungsten powder is a raw material, tungsten powder
Purity 〉=99.95%, granularity is at 3 μ m, hardness HV215, making step is as follows:
Step 1, raw material is packed in the rubber die sleeve, be prepared into hollow opaque tungsten pipe, adopt the cold isostatic press moulding then, pressure is 200Mpa, solid tube blank molding after 15 minutes;
Step 2, the solid pipe after the moulding is put into the intermediate frequency sintering oven, feeds hydrogen in the stove,
Guarantee that pipe heats in the atmosphere of hydrogen, Heating temperature is 1900 °, and be 30 hours heat-up time, and cooling water circulation is adopted in the back, and postcooling to room temperature was finished in 10 hours, and molding blank is standby:
Step 3, the one-tenth parison after step 2 handled are heated to 1500 °, be 2 hours heat-up time, and taking out the back is that 750 kilograms air hammer forges 15 times with surging force, forges into to put into electrothermal oven tempering half hour behind the tungsten bar, tempering temperature is 475 °, and the back is standby:
Step 4, the tungsten bar after step 3 handled carry out mechanical workout, right boring endoporus and finish turning cylindrical, caliber behind aperture and the finish turning is set according to customer demand and pipe target model, and the processing back guarantees that sputter pipe target all surface roughness reaches Ra1.6 ~ Ra3.2 μ m, completes.
Oxygen in the described raw material≤0.005%, sulphur≤0.003%, aluminium≤0.002%, iron≤0.005%, molybdenum≤0.01%, magnesium≤0.002%, nickel≤0.003%.
Embodiment three:
A kind of manufacture craft of sputter pipe target of tungsten rotary plating, the employing tungsten powder is a raw material, tungsten powder
Purity 〉=99.95%, granularity is at 3.3 μ m, hardness HV235, making step is as follows:
Step 1, raw material is packed in the rubber die sleeve, be prepared into hollow opaque tungsten pipe, adopt the cold isostatic press moulding then, pressure is 400Mpa, solid tube blank molding after 10 minutes;
Step 2, the solid pipe after the moulding is put into the intermediate frequency sintering oven, feeds hydrogen in the stove,
Guarantee that pipe heats in the atmosphere of hydrogen, Heating temperature is 1900 °, and be 30 hours heat-up time, and cooling water circulation is adopted in the back, and postcooling to room temperature was finished in 16 hours, and molding blank is standby:
Step 3, the one-tenth parison after step 2 handled are heated to 1700 °, be 1 hour heat-up time, and taking out the back is that 750 kilograms air hammer forges 20 times with surging force, forges into to put into electrothermal oven tempering half hour behind the tungsten bar, tempering temperature is 500 °, and the back is standby:
Step 4, the tungsten bar after step 3 handled carry out mechanical workout, right boring endoporus and finish turning cylindrical, caliber behind aperture and the finish turning is set according to customer demand and pipe target model, and the processing back guarantees that sputter pipe target all surface roughness reaches Ra1.6 ~ Ra3.2 μ m, completes.
Oxygen in the described raw material≤0.005%, sulphur≤0.003%, aluminium≤0.002%, iron≤0.005%, molybdenum≤0.01%, magnesium≤0.002%, nickel≤0.003%.
Claims (2)
1. the manufacture craft of the sputter pipe target of a tungsten rotary plating, it is characterized in that: the employing tungsten powder is a raw material, the purity of tungsten powder 〉=99.95%, granularity is at 2.6-3.3 μ m, and making step is as follows:
Step 1, raw material is packed in the rubber die sleeve, be prepared into hollow opaque tungsten pipe, adopt the cold isostatic press moulding then, pressure is 50-400Mpa, solid tube blank molding after 10-20 minutes;
Step 2, the solid pipe after the moulding is put into the intermediate frequency sintering oven, feed hydrogen in the stove, Heating temperature is 1900 °, and be 30 hours heat-up time, and cooling water circulation is adopted in the back, and postcooling to room temperature was finished in 8-16 hours, and molding blank is standby;
Step 3, the one-tenth parison after step 2 handled are heated to 1300 °-1700 °, be 1-3 hours heat-up time, taking out the back is that 750 kilograms air hammer forges 10-20 times with surging force, forge into and put into electrothermal oven tempering half hour behind the tungsten bar, tempering temperature is 450 °-500 °, and the back is standby;
Step 4, the tungsten bar after step 3 handled carry out mechanical workout, bore hole, turning, make surfaceness reach Ra1.6 ~ Ra3.2 μ m after, sputter pipe target completes.
2. according to the manufacture craft of the sputter pipe target of a kind of tungsten rotary plating described in the claim 1, it is characterized in that: oxygen in the described raw material≤0.005%, sulphur≤0.003%, aluminium≤0.002%, iron≤0.005%, molybdenum≤0.01%, magnesium≤0.002%, nickel≤0.003%.
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CN110014156A (en) * | 2019-03-19 | 2019-07-16 | 江门富祥电子材料有限公司 | A kind of method that powder metallurgy prepares tantalum pipe |
CN111136264A (en) * | 2020-01-14 | 2020-05-12 | 西安瑞福莱钨钼有限公司 | Method for producing ultra-thick tungsten plate by upsetting tungsten rod |
CN111136264B (en) * | 2020-01-14 | 2022-03-15 | 西安瑞福莱钨钼有限公司 | Method for producing ultra-thick tungsten plate by upsetting tungsten rod |
CN113549881A (en) * | 2021-05-31 | 2021-10-26 | 洛阳科威钨钼有限公司 | Preparation method of tungsten-nickel alloy target material |
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