CN103060760A - Preparation method for molybdenum-titanium alloy target - Google Patents
Preparation method for molybdenum-titanium alloy target Download PDFInfo
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- CN103060760A CN103060760A CN2012104971674A CN201210497167A CN103060760A CN 103060760 A CN103060760 A CN 103060760A CN 2012104971674 A CN2012104971674 A CN 2012104971674A CN 201210497167 A CN201210497167 A CN 201210497167A CN 103060760 A CN103060760 A CN 103060760A
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Abstract
The invention discloses a preparation method for a molybdenum-titanium alloy target. The preparation method for the molybdenum-titanium alloy target disclosed by the invention comprises the following steps of: (1) adequately mixing molybdenum powder, titanium powder and a forming agent, so as to obtain molybdenum-titanium alloy powder; (2) cold-pressing the molybdenum-titanium alloy powder obtained in the step (1) to obtain a pre-formed blank; and (3) performing vacuum hot-pressing forming on the pre-formed blank obtained in the step (2), cooling and cutting to obtain the molybdenum-titanium alloy target. With the adoption of a powder metallurgy method, the preparation method for the molybdenum-titanium alloy target disclosed by the invention is low in cost, high in the rate of finished products, and capable of effectively reducing the cost of the molybdenum-titanium alloy target; and the method disclosed by the invention is pollution-free and free from generating any pollutant such as waste material and waste acid.
Description
Technical field
The invention belongs to the alloy material processing technique field, be specifically related to a kind of preparation method of molybdenum titanium alloy target.
Background technology
The packaged material that sun power of the prior art and semicon industry are used, and the used material of diffusion impervious layer after the wiring of semiconductor copper, aluminium is generally pure tungsten target or tungsten titanium target material, but because the weight of tungsten itself is larger, can't carry out further lightweight to the said products improves, therefore the trend of tungsten-titanium alloy target and pure tungsten target appear replacing with molybdenum titanium alloy now, but the difficulty of processing of molybdenum titanium alloy is larger, and yield rate is low, causes its cost higher.
Summary of the invention
The object of the invention is to overcome the prior art defective, a kind of preparation method who can be applicable to high purity (99.99%) the molybdenum titanium alloy target in sun power and the semicon industry is provided.
Technical scheme of the present invention is as follows:
A kind of preparation method of molybdenum titanium alloy target comprises the steps:
(1) molybdenum powder, titanium valve and binder are fully mixed, obtain the molybdenum titanium alloy powder;
(2) step (1) gained molybdenum titanium alloy powder is colded pressing to get preform;
(3) step (2) gained preform is carried out vacuum hotpressing and be shaped, get the sintering blank after the cooling;
(4) namely get the molybdenum titanium alloy target after the sintering blank cutting with step (3).
In a preferred embodiment of the invention, the Fei Shi mean particle size of described molybdenum powder is 1.0 μ m ~ 10.0 μ m, and purity is 99.99%; The Fei Shi mean particle size of described titanium valve is 20 μ m ~ 100 μ m, and purity is 99.99%.
In a preferred embodiment of the invention, described step (1) is: the weight ratio by 5 ~ 9:4.5 ~ 1 takes by weighing molybdenum powder and titanium valve, behind the adding binder, sends in the V-arrangement blender, and the speed with 10r/min ~ 20r/min under argon gas atmosphere was mixed 10 ~ 20 hours.
In a preferred embodiment of the invention, described binder is Refined Paraffin Wax, and its add-on is 1% ~ 5% of molybdenum powder and titanium valve total mass.
In a preferred embodiment of the invention, described binder is Refined Paraffin Wax, and its add-on is 2.5 ~ 3.5% of molybdenum powder and titanium valve total mass.
In a preferred embodiment of the invention, described step (3) is for to be heated to first the binder volatilization temperature with step (2) gained preform, and be incubated to binder volatilization, reheat to melt temperature and the pressurization of titanium and make product shaping, behind the furnace cooling the sintering blank.
In a preferred embodiment of the invention, described binder is Refined Paraffin Wax, and its volatilization temperature is 500 ~ 550 ℃.
In a preferred embodiment of the invention, the melt temperature of described titanium is 1650 ~ 1700 ℃.
In a preferred embodiment of the invention, described being pressurised into is forced into 30 ~ 50MPa.
The invention has the beneficial effects as follows:
1, method of the present invention with purity be 99.99% molybdenum powder and purity be 99.99% titanium valve with binder fully mix first cold-press moulding again vacuum heating-press sintering prepare the molybdenum titanium alloy target, the cost of the method is low, yield rate is high, effectively reduces the cost of molybdenum titanium alloy target;
2, the present invention adopts the method for powder metallurgy, and preparation process is pollution-free, do not produce the pollutents such as any waste material, spent acid.
Description of drawings
Fig. 1 is the metallograph of the prepared molybdenum titanium alloy target of the embodiment of the invention 1;
Fig. 2 is the metallograph of the prepared molybdenum titanium alloy target of the embodiment of the invention 2;
Fig. 3 is the metallograph of the prepared molybdenum titanium alloy target of the embodiment of the invention 3;
Embodiment
Below by embodiment in connection with accompanying drawing, technical scheme of the present invention is further detailed and describes.
Embodiment 1
(1) weight ratio by 6:4 takes by weighing molybdenum powder and titanium valve, behind the adding Refined Paraffin Wax, sends in the V-arrangement blender, and the speed with 10r/min under argon gas atmosphere was mixed 20 hours, obtained the molybdenum titanium alloy powder; The Fei Shi mean particle size of above-mentioned molybdenum powder is 5 μ m, and purity is 99.99%; The Fei Shi mean particle size of above-mentioned titanium valve is 20 μ m, and purity is 99.99%; The add-on of above-mentioned Refined Paraffin Wax is 2.5% of above-mentioned molybdenum powder and titanium valve total mass;
(2) step (1) gained molybdenum titanium alloy powder is placed the vacuum heating-press sintering mould, with the oil press preform of colding pressing to get;
(3) step (2) gained preform is placed be heated to first 500 ℃ in the valve tube hot pressing furnace, and be incubated to the Refined Paraffin Wax volatilization, reheat to 1700 ℃, allow titanium be in molten state, and be forced into 50MPa and make product shaping, the sintering blank of coming out of the stove behind the furnace cooling to get;
(4) step (3) gained sintering blank is cut to final dimension with the slow wire feeding cutting facility, namely gets structure molybdenum titanium alloy target as shown in Figure 1.
Embodiment 2
(1) weight ratio by 6:4 takes by weighing molybdenum powder and titanium valve, behind the adding Refined Paraffin Wax, sends in the V-arrangement blender, and the speed with 10r/min under argon gas atmosphere was mixed 20 hours, obtained the molybdenum titanium alloy powder; The Fei Shi mean particle size of above-mentioned molybdenum powder is 10 μ m, and purity is 99.99%; The Fei Shi mean particle size of above-mentioned titanium valve is 80 μ m, and purity is 99.99%; The add-on of above-mentioned Refined Paraffin Wax is 3.5% of above-mentioned molybdenum powder and titanium valve total mass;
(2) step (1) gained molybdenum titanium alloy powder is placed the vacuum heating-press sintering mould, with the oil press preform of colding pressing to get;
(3) step (2) gained preform is placed be heated to first 500 ℃ in the valve tube hot pressing furnace, and be incubated to the Refined Paraffin Wax volatilization, reheat to 1700 ℃, allow titanium be in molten state, and be forced into 45MPa and make product shaping, the sintering blank of coming out of the stove behind the furnace cooling to get;
(4) step (3) gained sintering blank is cut to final dimension with the slow wire feeding cutting facility, namely gets structure molybdenum titanium alloy target as shown in Figure 2.
Embodiment 3
(1) weight ratio by 6:4 takes by weighing molybdenum powder and titanium valve, behind the adding Refined Paraffin Wax, sends in the V-arrangement blender, and the speed with 20r/min under argon gas atmosphere was mixed 15 hours, obtained the molybdenum titanium alloy powder; The Fei Shi mean particle size of above-mentioned molybdenum powder is 10 μ m, and purity is 99.99%; The Fei Shi mean particle size of above-mentioned titanium valve is 80 μ m, and purity is 99.99%; The add-on of above-mentioned Refined Paraffin Wax is 3% of above-mentioned molybdenum powder and titanium valve total mass;
(2) step (1) gained molybdenum titanium alloy powder is placed the vacuum heating-press sintering mould, with the oil press preform of colding pressing to get;
(3) step (2) gained preform is placed be heated to first 550 ℃ in the valve tube hot pressing furnace, and be incubated to the Refined Paraffin Wax volatilization, reheat to 1650 ℃, allow titanium be in molten state, and be forced into 50MPa and make product shaping, the sintering blank of coming out of the stove behind the furnace cooling to get;
(4) step (3) gained sintering blank is cut to final dimension with the slow wire feeding cutting facility, namely gets structure molybdenum titanium alloy target as shown in Figure 3.
Adopting the Fei Shi mean particle size is that the purity of 1.0 μ m ~ 10.0 μ m is that purity that 99.99% molybdenum powder and Fei Shi mean particle size are 20 μ m ~ 100 μ m is that 99.99% titanium valve substitutes molybdenum powder and the titanium valve in above-described embodiment, weight ratio with 5 ~ 9:4.5 ~ 1 is mixed, and take the identical working condition of above-described embodiment, also can reach identical technique effect.
The above only is preferred embodiment of the present invention, therefore can not limit according to this scope of the invention process, the equivalence of namely doing according to claim of the present invention and description changes and modifies, and all should still belong in the scope that the present invention contains.
Claims (9)
1. the preparation method of a molybdenum titanium alloy target is characterized in that: comprise the steps:
(1) molybdenum powder, titanium valve and binder are fully mixed, obtain the molybdenum titanium alloy powder;
(2) step (1) gained molybdenum titanium alloy powder is colded pressing to get preform;
(3) step (2) gained preform is carried out vacuum hotpressing and be shaped, get the sintering blank after the cooling;
(4) namely get the molybdenum titanium alloy target after the sintering blank cutting with step (3).
2. the preparation method of a kind of molybdenum titanium alloy target as claimed in claim 1, it is characterized in that: the Fei Shi mean particle size of described molybdenum powder is 1.0 μ m ~ 10.0 μ m, and purity is 99.99%; The Fei Shi mean particle size of described titanium valve is 20 μ m ~ 100 μ m, and purity is 99.99%.
3. the preparation method of a kind of molybdenum titanium alloy target as claimed in claim 2, it is characterized in that: described step (1) is: the weight ratio by 5 ~ 9:4.5 ~ 1 takes by weighing molybdenum powder and titanium valve, after adding binder, send in the V-arrangement blender, the speed with 10r/min ~ 20r/min under argon gas atmosphere was mixed 10 ~ 20 hours.
4. the preparation method of a kind of molybdenum titanium alloy target as claimed in claim 3, it is characterized in that: described binder is Refined Paraffin Wax, its add-on is 1% ~ 5% of molybdenum powder and titanium valve total mass.
5. the preparation method of a kind of molybdenum titanium alloy target as claimed in claim 4, it is characterized in that: described binder is Refined Paraffin Wax, its add-on is 2.5 ~ 3.5% of molybdenum powder and titanium valve total mass.
6. the preparation method of a kind of molybdenum titanium alloy target as claimed in claim 1, it is characterized in that: described step (3) is for to be heated to first the binder volatilization temperature with step (2) gained preform, and be incubated to binder and volatilize, reheat to the melt temperature of titanium and pressurization and make product shaping, behind the furnace cooling the sintering blank.
7. the preparation method of a kind of molybdenum titanium alloy target as claimed in claim 6, it is characterized in that: described binder is Refined Paraffin Wax, its volatilization temperature is 500 ~ 550 ℃.
8. the preparation method of a kind of molybdenum titanium alloy target as claimed in claim 6, it is characterized in that: the melt temperature of described titanium is 1650 ~ 1700 ℃.
9. the preparation method of a kind of molybdenum titanium alloy target as claimed in claim 6, it is characterized in that: described being pressurised into is forced into 30 ~ 50MPa.
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Cited By (5)
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| CN104416156A (en) * | 2013-09-11 | 2015-03-18 | 安泰科技股份有限公司 | Chromium-aluminum alloy target and preparation method thereof |
| CN104480446A (en) * | 2014-12-30 | 2015-04-01 | 山东昊轩电子陶瓷材料有限公司 | Molybdenum-titanium alloy target material and production method thereof |
| CN104532201A (en) * | 2014-12-29 | 2015-04-22 | 金堆城钼业股份有限公司 | Method for preparing molybdenum-titanium alloy sputtering target board |
| CN104550979A (en) * | 2014-12-29 | 2015-04-29 | 金堆城钼业股份有限公司 | Method for manufacturing molybdenum-niobium alloy target plates |
| CN106148903A (en) * | 2015-04-22 | 2016-11-23 | 宁波江丰电子材料股份有限公司 | The manufacture method of molybdenum titanium target |
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| CN104416156A (en) * | 2013-09-11 | 2015-03-18 | 安泰科技股份有限公司 | Chromium-aluminum alloy target and preparation method thereof |
| CN104532201A (en) * | 2014-12-29 | 2015-04-22 | 金堆城钼业股份有限公司 | Method for preparing molybdenum-titanium alloy sputtering target board |
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| CN104550979B (en) * | 2014-12-29 | 2016-12-07 | 金堆城钼业股份有限公司 | A kind of preparation method of molybdenum niobium alloy target plate |
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| CN106148903A (en) * | 2015-04-22 | 2016-11-23 | 宁波江丰电子材料股份有限公司 | The manufacture method of molybdenum titanium target |
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Application publication date: 20130424 |