CN102211188A - Reparation method of tungsten titanium alloy target material used in semiconductor and solar sputtering target material industries - Google Patents
Reparation method of tungsten titanium alloy target material used in semiconductor and solar sputtering target material industries Download PDFInfo
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- CN102211188A CN102211188A CN 201110149666 CN201110149666A CN102211188A CN 102211188 A CN102211188 A CN 102211188A CN 201110149666 CN201110149666 CN 201110149666 CN 201110149666 A CN201110149666 A CN 201110149666A CN 102211188 A CN102211188 A CN 102211188A
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 94
- MAKDTFFYCIMFQP-UHFFFAOYSA-N titanium tungsten Chemical compound [Ti].[W] MAKDTFFYCIMFQP-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 239000013077 target material Substances 0.000 title claims abstract description 33
- 239000004065 semiconductor Substances 0.000 title claims abstract description 26
- 238000005477 sputtering target Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000005245 sintering Methods 0.000 claims abstract description 61
- 239000000843 powder Substances 0.000 claims abstract description 55
- 238000002360 preparation method Methods 0.000 claims abstract description 38
- 238000000137 annealing Methods 0.000 claims abstract description 24
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000010936 titanium Substances 0.000 claims abstract description 21
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 21
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000005406 washing Methods 0.000 claims abstract description 6
- 150000004678 hydrides Chemical class 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 15
- 238000010792 warming Methods 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- 229910002804 graphite Inorganic materials 0.000 claims description 13
- 239000010439 graphite Substances 0.000 claims description 13
- 238000005520 cutting process Methods 0.000 claims description 11
- 238000003825 pressing Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000007731 hot pressing Methods 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 230000007797 corrosion Effects 0.000 claims description 5
- 238000005260 corrosion Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 abstract description 8
- 238000007254 oxidation reaction Methods 0.000 abstract description 8
- 239000012535 impurity Substances 0.000 abstract description 4
- -1 titanium hydride Chemical compound 0.000 abstract 2
- 229910000048 titanium hydride Inorganic materials 0.000 abstract 2
- 239000000470 constituent Substances 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 239000010937 tungsten Substances 0.000 abstract 1
- 229910052721 tungsten Inorganic materials 0.000 abstract 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910001080 W alloy Inorganic materials 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910011208 Ti—N Inorganic materials 0.000 description 1
- 229910003077 Ti−O Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000003026 anti-oxygenic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000003913 materials processing Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention discloses a preparation method of a tungsten titanium alloy target material used in semiconductor and solar sputtering target material industries. The method comprises the following steps of: using titanium hydride to replace part of traditional pure titanium; placing tungsten powders, titanium powders and titanium hydride powders into a three-dimensional mixer according to a certain mass ratio; mixing the powders at a certain rotation speed to obtain tungsten titanium alloy powders; placing and sintering a mould filled with the tungsten titanium alloy powders into a vacuum hot-press sintering furnace to obtain a vacuum hot-press sintering blank; after the vacuum hot-press sintering blank is cut according to sizes, placing the vacuum hot-press sintering blank in a vacuum annealing furnace for annealing process; finally washing the surface of the target material by using an ultrasonic cleaner, so as to obtain the tungsten titanium alloy target, wherein the constituents and density of the tungsten titanium alloy target are fully conform to the requirements. The preparation method has the characteristics that the powers are mixed evenly, oxidation is has the possibility of occurring during the preparation procedure, the content of impurity is low, and the density of the prepared tungsten titanium alloy target is high.
Description
Technical field
The present invention relates to the materials processing technology field, particularly relate to a kind of semiconductor and solar energy sputtering target material industry preparation method with the tungsten-titanium alloy target.
Background technology
Tungsten titanium W/Ti alloy target material is owing to have low resistance coefficient, good thermal stability and antioxygenic property, successfully be applied to the diffusion impervious layer of Al, Cu and Ag wiring, and also obtained extensive studies and application aspect semicon industry and the solar energy industry sputter coating by various films such as WOx-TOx, W-Ti-C, W-Ti-O and the W-Ti-N etc. of tungsten titanium W/Ti alloy target material preparation.Therefore tungsten titanium W/Ti alloy target material becomes one of focus of target preparation research.But still there are many defectives in the made tungsten-titanium alloy target of the preparation method of prior art, and is not high as easily oxidation in tungsten-titanium alloy powder inequality, the preparation process, impurity content height, the tungsten-titanium alloy target density prepared.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of semiconductor and the solar energy sputtering target material industry preparation method with the tungsten-titanium alloy target is provided, and it is even to have powder, is difficult for oxidation in the preparation process, impurity content is low, the high characteristics of preparing of tungsten-titanium alloy target density.
The technical solution adopted for the present invention to solve the technical problems is: a kind of semiconductor and solar energy sputtering target material industry comprise the steps: with the preparation method of tungsten-titanium alloy target
A. tungsten powder, the Fei Shi particle mean size that with the Fei Shi particle mean size is 1.0 μ m~2.8 μ m is that titanium valve and the Fei Shi particle mean size of 40 μ m~60 μ m is the hydride powder of 20 μ m~60 μ m, by tungsten powder: titanium valve: hydride powder is (7.0~9.0): (0.5~1.5): the mass ratio of (0.5~1.5) places the three-dimensional blender device, at rotating speed is to mix 1.0h~1.5h under 40r/min~70r/min condition, obtains the tungsten-titanium alloy powder;
B. above-mentioned tungsten-titanium alloy powder is placed in the vacuum heating-press sintering mould, use the corrosion resistant plate compacted powder, allow it fully fill mould;
C. the mould of populated tungsten-titanium alloy powder is put into the vacuum heating-press sintering stove, and in time vacuumize;
D. then, be warming up to 500~1000 ℃ and be forced into 280 tons, treat to be warming up to 1400 ℃~1430 ℃ again after pressurization is finished, be incubated 0.5~1.5 hour;
E. then, regulating vacuum hotpressing stove power is " 0 ", can come out of the stove after cooling to room temperature with the furnace, obtains the vacuum heating-press sintering blank of tungsten-titanium alloy target;
F. use linear cutting equipment that above-mentioned vacuum heating-press sintering blank is cut to finished size;
G. will place in the vacuum annealing furnace through the vacuum heating-press sintering blank after the cutting, be warming up to 800 ℃~1000 ℃, annealing 0.5h~1.5h, the vacuum heating-press sintering tungsten-titanium alloy target after obtaining annealing;
H. the vacuum heating-press sintering tungsten-titanium alloy target after will annealing is put into ultrasonic cleaner, add an amount of washing agent and pure water, vacuum heating-press sintering tungsten-titanium alloy target is fully immersed in the liquid to be cleaned 1~2 hour, change clear water subsequently and cleaned once more 1~2 hour, obtain satisfactory tungsten-titanium alloy target at last.
Among the described step a, described tungsten powder purity 〉=99.995%, described titanium valve purity 〉=99.00%., described hydride powder purity 〉=99.00%.
Among the described step b, described vacuum heating-press sintering mould is a graphite jig.
Among the described step c, described in time vacuumizing to being evacuated to below the 800Pa.
Described being forced in 280 tons of processes, pressing speed is controlled at 3~15 tons of per minutes.
A kind of semiconductor of the present invention and solar energy sputtering target material industry are to adopt titantium hydride to replace traditional pure titanium of part with the preparation method of tungsten-titanium alloy target, and the titantium hydride release hydrogen can play reduction, prevent the effect of sample oxidation in the hot pressed sintering process.
A kind of semiconductor of the present invention and solar energy sputtering target material industry have adopted the three-dimensional hybrid device with the preparation method of tungsten-titanium alloy target in material powder mixed process, improved in the past that additive method mixes uneven problem, and hybrid parameter is controlled.
A kind of semiconductor of the present invention and the solar energy sputtering target material industry preparation method of tungsten-titanium alloy target, in the material powder pressing process, adopted graphite jig, compare with other mould, not only improved high temperature compression strength, and, the graphite atmosphere that graphite jig produces in sintering process helps keeping the purity of raw material, reduces oxygen content.
A kind of semiconductor of the present invention and the solar energy sputtering target material industry preparation method of tungsten-titanium alloy target, control vacuum-sintering atmospheric pressure is to 800pa, according to analysis, existing tungsten-titanium alloy target oxygen content is higher, partly cause is because when air pressure residual in the stove 〉=800Pa, and interior graphite jig and the tungsten-titanium alloy powder of stove will oxidation in temperature-rise period.
A kind of semiconductor of the present invention and the solar energy sputtering target material industry preparation method of tungsten-titanium alloy target, in being forced into 280 tons of processes, adopted the mode of pressing speed, pressing speed is set to 3~15 tons of per minutes, can guarantee that the tungsten-titanium alloy powder shrinks at once under HTHP, reach more than 99% of solid density, thereby satisfy customer requirement.
The invention has the beneficial effects as follows, owing to adopted titantium hydride to replace traditional pure titanium of part, and with tungsten powder, titanium valve and hydride powder, place the three-dimensional blender device by certain mass ratio, under certain speed conditions, mix and obtain the tungsten-titanium alloy powder, then the mould of populated tungsten-titanium alloy powder being put into the vacuum heating-press sintering stove carries out sintering processes and obtains the vacuum heating-press sintering blank, after the vacuum heating-press sintering blank being carried out the size cutting, again the vacuum heating-press sintering blank is placed and carry out annealing in process in the vacuum annealing furnace, at last, use supersonic wave cleaning machine to clean target material surface, obtain the complete satisfactory tungsten-titanium alloy target of composition and density thus.It is even that this preparation method has powder, is difficult for oxidation in the preparation process, and impurity content is low, the high characteristics of preparing of tungsten-titanium alloy target density.
Capital equipment of the present invention is a vacuum hotpressing stove, and scale of mass production is vacuum hotpressing industry common equipment at home, so buy, install, use all simple.
The present invention is pollution-free, can not produce pollutants such as any waste material, spent acid in the preparation process.
Below in conjunction with drawings and Examples the present invention is described in further detail; But a kind of semiconductor of the present invention and solar energy sputtering target material industry are not limited to embodiment with the preparation method of tungsten-titanium alloy target.
Description of drawings
Fig. 1 is the micro-organization chart of the tungsten-titanium alloy target of embodiment one the present invention preparation;
Fig. 2 is the micro-organization chart of the tungsten-titanium alloy target of embodiment two the present invention preparation;
Fig. 3 is the micro-organization chart of the tungsten-titanium alloy target of embodiment three the present invention preparation.
The specific embodiment
Embodiment one, and a kind of semiconductor of the present invention and solar energy sputtering target material industry comprise the steps: with the preparation method of tungsten-titanium alloy target
A. be that the tungsten powder of 2.8 μ m, titanium valve and the Fei Shi particle mean size that the Fei Shi particle mean size is 60 μ m are the hydride powder of 60 μ m with the Fei Shi particle mean size, by tungsten powder: titanium valve: hydride powder is that 7.0: 1.5: 1.5 mass ratio places the three-dimensional blender device, at rotating speed is to mix 1.5h under the 70r/min condition, obtains the tungsten-titanium alloy powder;
Wherein, described tungsten powder purity 〉=99.995%, described titanium valve purity 〉=99.00%., described hydride powder purity 〉=99.00%;
B. above-mentioned tungsten-titanium alloy powder is placed in the vacuum heating-press sintering mould, use the corrosion resistant plate compacted powder, allow it fully fill mould; Wherein, this vacuum heating-press sintering mould is a graphite jig;
C. the mould of populated tungsten-titanium alloy powder is put into the vacuum heating-press sintering stove, and in time vacuumize; Wherein, described in time vacuumizing to being evacuated to below the 800Pa;
D. then, be warming up to 500 ℃ and be forced into 280 tons, treat to be warming up to 1430 ℃ again after pressurization is finished, be incubated 1.5 hours; Wherein, be forced in 280 tons of processes, pressing speed is controlled at 15 tons of per minutes;
E. then, regulating vacuum hotpressing stove power is " 0 ", can come out of the stove after cooling to room temperature with the furnace, obtains the vacuum heating-press sintering blank of tungsten-titanium alloy target;
F. use linear cutting equipment that above-mentioned vacuum heating-press sintering blank is cut to finished size;
G. will place in the vacuum annealing furnace through the vacuum heating-press sintering blank after the cutting, be warming up to 1000 ℃, annealing 1.5h, the vacuum heating-press sintering tungsten-titanium alloy target after obtaining annealing;
H. the vacuum heating-press sintering tungsten-titanium alloy target after will annealing is put into ultrasonic cleaner, add an amount of washing agent and pure water, vacuum heating-press sintering tungsten-titanium alloy target is fully immersed in the liquid to be cleaned 2 hours, change clear water subsequently and cleaned once more 2 hours, obtain satisfactory tungsten-titanium alloy target at last.
Fig. 1 sees in the micro-organization chart of the tungsten-titanium alloy target that makes thus.
Embodiment two, and a kind of semiconductor of the present invention and solar energy sputtering target material industry comprise the steps: with the preparation method of tungsten-titanium alloy target
A. be that the tungsten powder of 2.0 μ m, titanium valve and the Fei Shi particle mean size that the Fei Shi particle mean size is 40 μ m are the hydride powder of 40 μ m with the Fei Shi particle mean size, by tungsten powder: titanium valve: hydride powder is that 8.0: 0.5: 1.0 mass ratio places the three-dimensional blender device, at rotating speed is to mix 1.5h under the 50r/min condition, obtains the tungsten-titanium alloy powder;
Wherein, described tungsten powder purity 〉=99.995%, described titanium valve purity 〉=99.00%., described hydride powder purity 〉=99.00%;
B. above-mentioned tungsten-titanium alloy powder is placed in the vacuum heating-press sintering mould, use the corrosion resistant plate compacted powder, allow it fully fill mould; Wherein, this vacuum heating-press sintering mould is a graphite jig;
C. the mould of populated tungsten-titanium alloy powder is put into the vacuum heating-press sintering stove, and in time vacuumize; Wherein, described in time vacuumizing to being evacuated to below the 800Pa;
D. then, be warming up to 700 ℃ and be forced into 280 tons, treat to be warming up to 1410 ℃ again after pressurization is finished, be incubated 1.0 hours; Wherein, be forced in 280 tons of processes, pressing speed is controlled at 10 tons of per minutes;
E. then, regulating vacuum hotpressing stove power is " 0 ", can come out of the stove after cooling to room temperature with the furnace, obtains the vacuum heating-press sintering blank of tungsten-titanium alloy target;
F. use linear cutting equipment that above-mentioned vacuum heating-press sintering blank is cut to finished size;
G. will place in the vacuum annealing furnace through the vacuum heating-press sintering blank after the cutting, be warming up to 900 ℃, annealing 1.0h, the vacuum heating-press sintering tungsten-titanium alloy target after obtaining annealing;
H. the vacuum heating-press sintering tungsten-titanium alloy target after will annealing is put into ultrasonic cleaner, add an amount of washing agent and pure water, vacuum heating-press sintering tungsten-titanium alloy target is fully immersed in the liquid to be cleaned 1 hour, change clear water subsequently and cleaned once more 1 hour, obtain satisfactory tungsten-titanium alloy target at last.
Fig. 2 sees in the micro-organization chart of the tungsten-titanium alloy target that makes thus.
Embodiment three, and a kind of semiconductor of the present invention and solar energy sputtering target material industry comprise the steps: with the preparation method of tungsten-titanium alloy target
A. be that the tungsten powder of 1.0 μ m, titanium valve and the Fei Shi particle mean size that the Fei Shi particle mean size is 50 μ m are the hydride powder of 20 μ m with the Fei Shi particle mean size, by tungsten powder: titanium valve: hydride powder is that 9.0: 1.0: 0.5 mass ratio places the three-dimensional blender device, at rotating speed is to mix 1.0h under the 40r/min condition, obtains the tungsten-titanium alloy powder;
Wherein, described tungsten powder purity 〉=99.995%, described titanium valve purity 〉=99.00%., described hydride powder purity 〉=99.00%;
B. above-mentioned tungsten-titanium alloy powder is placed in the vacuum heating-press sintering mould, use the corrosion resistant plate compacted powder, allow it fully fill mould; Wherein, this vacuum heating-press sintering mould is a graphite jig;
C. the mould of populated tungsten-titanium alloy powder is put into the vacuum heating-press sintering stove, and in time vacuumize; Wherein, described in time vacuumizing to being evacuated to below the 800Pa;
D. then, be warming up to 1000 ℃ and be forced into 280 tons, treat to be warming up to 1400 ℃ again after pressurization is finished, be incubated 0.5 hour; Wherein, be forced in 280 tons of processes, pressing speed is controlled at 3 tons of per minutes;
E. then, regulating vacuum hotpressing stove power is " 0 ", can come out of the stove after cooling to room temperature with the furnace, obtains the vacuum heating-press sintering blank of tungsten-titanium alloy target;
F. use linear cutting equipment that above-mentioned vacuum heating-press sintering blank is cut to finished size;
G. will place in the vacuum annealing furnace through the vacuum heating-press sintering blank after the cutting, be warming up to 800 ℃, annealing 0.5h, the vacuum heating-press sintering tungsten-titanium alloy target after obtaining annealing;
H. the vacuum heating-press sintering tungsten-titanium alloy target after will annealing is put into ultrasonic cleaner, add an amount of washing agent and pure water, vacuum heating-press sintering tungsten-titanium alloy target is fully immersed in the liquid to be cleaned 1.5 hours, change clear water subsequently and cleaned once more 1.5 hours, obtain satisfactory tungsten-titanium alloy target at last.
Fig. 3 sees in the micro-organization chart of the tungsten-titanium alloy target that makes thus.
A kind of semiconductor of the present invention and solar energy sputtering target material industry are to adopt titantium hydride to replace traditional pure titanium of part with the preparation method of tungsten-titanium alloy target, and the titantium hydride release hydrogen can play reduction, prevent the effect of sample oxidation in the hot pressed sintering process.
A kind of semiconductor of the present invention and solar energy sputtering target material industry have adopted the three-dimensional hybrid device with the preparation method of tungsten-titanium alloy target in material powder mixed process, improved in the past that additive method mixes uneven problem, and hybrid parameter is controlled.
A kind of semiconductor of the present invention and the solar energy sputtering target material industry preparation method of tungsten-titanium alloy target, in the material powder pressing process, adopted graphite jig, compare with other mould, not only improved high temperature compression strength, and, the graphite atmosphere that graphite jig produces in sintering process helps keeping the purity of raw material, reduces oxygen content.
A kind of semiconductor of the present invention and the solar energy sputtering target material industry preparation method of tungsten-titanium alloy target, control vacuum-sintering atmospheric pressure is to 800pa, according to analysis, existing tungsten-titanium alloy target oxygen content is higher, partly cause is because when air pressure residual in the stove 〉=800Pa, and interior graphite jig and the tungsten-titanium alloy powder of stove will oxidation in temperature-rise period.
A kind of semiconductor of the present invention and the solar energy sputtering target material industry preparation method of tungsten-titanium alloy target, in being forced into 280 tons of processes, adopted the mode of pressing speed, pressing speed is set to 3~15 tons of per minutes, can guarantee that the tungsten-titanium alloy powder shrinks at once under HTHP, reach more than 99% of solid density, thereby satisfy customer requirement.
The foregoing description only is used for further specifying the preparation method of a kind of semiconductor of the present invention and solar energy sputtering target material industry usefulness tungsten-titanium alloy target; but the present invention is not limited to embodiment; every foundation technical spirit of the present invention all falls in the protection domain of technical solution of the present invention any simple modification, equivalent variations and modification that above embodiment did.
Claims (5)
1. semiconductor and solar energy sputtering target material industry is characterized in that: comprise the steps: with the preparation method of tungsten-titanium alloy target
A. tungsten powder, the Fei Shi particle mean size that with the Fei Shi particle mean size is 1.0 μ m~2.8 μ m is that titanium valve and the Fei Shi particle mean size of 40 μ m~60 μ m is the hydride powder of 20 μ m~60 μ m, by tungsten powder: titanium valve: hydride powder is (7.0~9.0): (0.5~1.5): the mass ratio of (0.5~1.5) places the three-dimensional blender device, at rotating speed is to mix 1.0h~1.5h under 40r/min~70r/min condition, obtains the tungsten-titanium alloy powder;
B. above-mentioned tungsten-titanium alloy powder is placed in the vacuum heating-press sintering mould, use the corrosion resistant plate compacted powder, allow it fully fill mould;
C. the mould of populated tungsten-titanium alloy powder is put into the vacuum heating-press sintering stove, and in time vacuumize;
D. then, be warming up to 500~1000 ℃ and be forced into 280 tons, treat to be warming up to 1400 ℃~1430 ℃ again after pressurization is finished, be incubated 0.5~1.5 hour;
E. then, regulating vacuum hotpressing stove power is " 0 ", can come out of the stove after cooling to room temperature with the furnace, obtains the vacuum heating-press sintering blank of tungsten-titanium alloy target;
F. use linear cutting equipment that above-mentioned vacuum heating-press sintering blank is cut to finished size;
G. will place in the vacuum annealing furnace through the vacuum heating-press sintering blank after the cutting, be warming up to 800 ℃~1000 ℃, annealing 0.5h~1.5h, the vacuum heating-press sintering tungsten-titanium alloy target after obtaining annealing;
H. the vacuum heating-press sintering tungsten-titanium alloy target after will annealing is put into ultrasonic cleaner, add an amount of washing agent and pure water, vacuum heating-press sintering tungsten-titanium alloy target is fully immersed in the liquid to be cleaned 1~2 hour, change clear water subsequently and cleaned once more 1~2 hour, obtain satisfactory tungsten-titanium alloy target at last.
2. semiconductor according to claim 1 and the solar energy sputtering target material industry preparation method of tungsten-titanium alloy target is characterized in that: among the described step a, and described tungsten powder purity 〉=99.995%, described titanium valve purity 〉=99.00%., described hydride powder purity 〉=99.00%.
3. semiconductor according to claim 1 and the solar energy sputtering target material industry preparation method of tungsten-titanium alloy target, it is characterized in that: among the described step b, described vacuum heating-press sintering mould is a graphite jig.
4. semiconductor according to claim 1 and the solar energy sputtering target material industry preparation method of tungsten-titanium alloy target is characterized in that: among the described step c, and described in time vacuumizing to being evacuated to below the 800Pa.
5. semiconductor according to claim 1 and the solar energy sputtering target material industry preparation method of tungsten-titanium alloy target, it is characterized in that: described being forced in 280 tons of processes, pressing speed is controlled at 3~15 tons of per minutes.
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| CN115679282A (en) * | 2022-11-02 | 2023-02-03 | 基迈克材料科技(苏州)有限公司 | Preparation method of titanium-silicon target material |
| CN115725944A (en) * | 2022-12-05 | 2023-03-03 | 基迈克材料科技(苏州)有限公司 | A kind of preparation method of tungsten-titanium sputtering target |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04116161A (en) * | 1990-09-05 | 1992-04-16 | Hitachi Metals Ltd | Titanium target material and production thereof |
| CN1270864A (en) * | 2000-04-26 | 2000-10-25 | 刘学晖 | Ultrasonic atomization of low-oxygen titanium with high-purity gas andtitanium alloy powder preparing process and product thereof |
| JP2004346423A (en) * | 2003-04-30 | 2004-12-09 | Hitachi Metals Ltd | Fe-Co-B ALLOY TARGET MATERIAL, ITS MANUFACTURING METHOD, SOFT MAGNETIC FILM, MAGNETIC RECORDING MEDIUM AND TMR ELEMENT |
| US20080038145A1 (en) * | 2006-05-02 | 2008-02-14 | Sanyo Special Steel Co., Ltd. | Fe-Co based target material and method for producing the same |
| CN101348895A (en) * | 2008-06-27 | 2009-01-21 | 贵州振华云科电子有限公司 | Preparation of porous stack metal or alloy sputtering target material |
-
2011
- 2011-06-03 CN CN 201110149666 patent/CN102211188B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04116161A (en) * | 1990-09-05 | 1992-04-16 | Hitachi Metals Ltd | Titanium target material and production thereof |
| CN1270864A (en) * | 2000-04-26 | 2000-10-25 | 刘学晖 | Ultrasonic atomization of low-oxygen titanium with high-purity gas andtitanium alloy powder preparing process and product thereof |
| JP2004346423A (en) * | 2003-04-30 | 2004-12-09 | Hitachi Metals Ltd | Fe-Co-B ALLOY TARGET MATERIAL, ITS MANUFACTURING METHOD, SOFT MAGNETIC FILM, MAGNETIC RECORDING MEDIUM AND TMR ELEMENT |
| US20080038145A1 (en) * | 2006-05-02 | 2008-02-14 | Sanyo Special Steel Co., Ltd. | Fe-Co based target material and method for producing the same |
| CN101348895A (en) * | 2008-06-27 | 2009-01-21 | 贵州振华云科电子有限公司 | Preparation of porous stack metal or alloy sputtering target material |
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| CN102398035B (en) * | 2011-11-25 | 2013-07-31 | 宁波江丰电子材料有限公司 | Nickel target blank and target manufacturing methods |
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| CN103691953B (en) * | 2012-09-27 | 2016-04-06 | 宁波江丰电子材料股份有限公司 | The manufacture method of the manufacture method of tungsten titanium target material and tungsten titanium target material combination |
| CN103834923A (en) * | 2012-11-27 | 2014-06-04 | 宁波江丰电子材料有限公司 | Preparation method of tungsten-titanium target |
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| CN113423859A (en) * | 2019-03-15 | 2021-09-21 | 三菱综合材料株式会社 | Tungsten oxide sputtering target |
| CN112111719A (en) * | 2020-09-11 | 2020-12-22 | 宁波江丰电子材料股份有限公司 | Tungsten titanium silicon alloy sputtering target material and preparation method thereof |
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| CN114619038A (en) * | 2022-01-31 | 2022-06-14 | 北京科技大学 | A kind of preparation method of high-purity tungsten-titanium alloy target |
| CN114535579A (en) * | 2022-03-15 | 2022-05-27 | 崇义章源钨业股份有限公司 | Preparation method of high-purity silicon tungsten powder |
| CN114535579B (en) * | 2022-03-15 | 2023-12-05 | 崇义章源钨业股份有限公司 | Preparation method of high-purity silicon tungsten powder |
| CN114951676A (en) * | 2022-04-20 | 2022-08-30 | 崇义章源钨业股份有限公司 | Preparation method of high-purity tungsten powder with controlled content of non-metallic elements |
| CN114951676B (en) * | 2022-04-20 | 2023-09-22 | 崇义章源钨业股份有限公司 | A method for preparing high-purity tungsten powder that controls the content of non-metallic elements |
| CN115679282A (en) * | 2022-11-02 | 2023-02-03 | 基迈克材料科技(苏州)有限公司 | Preparation method of titanium-silicon target material |
| CN115725944A (en) * | 2022-12-05 | 2023-03-03 | 基迈克材料科技(苏州)有限公司 | A kind of preparation method of tungsten-titanium sputtering target |
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