CN101956159A - Method for preparing high-purity molybdenum titanium sputtering target - Google Patents
Method for preparing high-purity molybdenum titanium sputtering target Download PDFInfo
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Abstract
The invention discloses a method for preparing high-purity molybdenum titanium sputtering targets, and relates to a method for preparing molybdenum titanium sputtering targets used in the electronic and photovoltaic field, which is characterized in that the preparation process comprises the following steps: taking ammonium dodecamolybdate as a raw material, preparing high-purity molybdenum powder through two sections of a hydrogen reductive method; carrying out cold isostatic pressing on the high-purity molybdenum powder to press into a molybdenum plate green body; presintering in vacuum; sintering into a molybdenum plate at high temperature at the atmosphere of hydrogen; processing the sintered molybdenum plate into a molybdenum target body by adopting a pressure processing manner of firstly forging and then rolling; vacuum annealing to process into the finished product of molybdenum titanium sputtering target according to a specific specification machine. The preparation method of the invention has low cost, simple operation and low equipment requirements; the prepared molybdenum titanium sputtering target has high purity, low impurity content, high density, uniform particle size and specific crystallization orientation.
Description
Technical field
A kind of preparation method of high-purity molybdenum sputtering targets material relates to a kind of electronics, the photovoltaic field preparation method with the molybdenum sputtering targets material.
Background technology
In electronics and photovoltaic field, the molybdenum sputtering targets material is mainly used in the electrode and the wiring material of flat-panel monitor and thin-film solar cells.Its requirement to the molybdenum sputtering targets material be high purity (＞99.95wt%), high-density (relative density＞98%), tiny and uniform grain structure and certain crystalline orientation, and require content low more good more to elemental gas such as C, O, K and alkali metal.
In order to improve the purity of molybdenum sputtering targets material, some enterprises adopt the method for electron beam melting both at home and abroad.This method cost height, complicated operation, the molybdenum base metal grain after the melting is thick, the following process difficulty, be difficult to guarantee that the finished product target requires tiny and uniform grain structure.Another method for preparing the molybdenum sputtering targets material is to adopt hot isostatic pressing method.The shortcoming of this method is the equipment cost height, technology and operation relative complex, and the density that obtains target is wayward, and because the restriction of specification of equipment, is difficult to prepare the molybdenum sputtering targets material of big specification.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art, provide a kind of and can effectively reduce production costs, simple to operate, have the preparation method of high-purity molybdenum sputtering targets material of high purity, low impurity, tiny and uniform grain structure and certain crystal orientations.
The objective of the invention is to be achieved through the following technical solutions.
A kind of preparation method of high-purity molybdenum sputtering targets material, it is characterized in that its preparation process is raw material with the ammomium dodecamolybdate, method by two sections hydrogen reducings is prepared high pure molybdenum powder, then high pure molybdenum powder is pressed into the molybdenum plate green compact through isostatic cool pressing, again through vacuum presintering, high temperature sintering is made high-purity molybdenum plate base under hydrogen atmosphere then; Rolling press working mode was processed into the molybdenum target base after high-purity molybdenum plate base that will sinter at last adopted and forges earlier, and after vacuum annealing, specification is machined to finished product molybdenum sputtering targets material according to the rules again.
The preparation method of a kind of high-purity molybdenum sputtering targets material of the present invention is characterized in that K content is 2～5ppm in the described ammomium dodecamolybdate raw material, and Fe content is 3-7ppm, and Ni content is smaller or equal to 2ppm, and crystal is the hexa-prism of rule, and size does not evenly have and reunites.
The preparation method of a kind of high-purity molybdenum sputtering targets material of the present invention is characterized in that described hydrogen reducing method prepares in the process of molybdenum powder, and boat adopts molybdenum boat, and the reduction furnace tube internal surface is inlayed the molybdenum lining; The purity of the molybdenum powder that restores is more than or equal to 99.99wt%.
The preparation method of a kind of molybdenum sputtering targets material of the present invention is characterized in that the described high pure molybdenum powder of preparing by the method for two sections hydrogen reducings when isostatic cool pressing is made the molybdenum plate green compact, and pressing pressure is 180～200MPa, 10～20 minutes dwell times.
The preparation method of a kind of high-purity molybdenum sputtering targets material of the present invention, it is characterized in that described molybdenum plate green compact are through vacuum presintering, high temperature sintering is made in the process of high-purity molybdenum plate base under hydrogen atmosphere then, the vacuum calcined temperature is 1200 ℃～1400 ℃, and vacuum tightness is more than or equal to 10
-3Pa, soaking time 1～2 hour; The high temperature sintering temperature is 1820 ℃～1980 ℃ under the hydrogen atmosphere, soaking time 6～8 hours.
The preparation method of a kind of high-purity molybdenum sputtering targets material of the present invention, it is characterized in that it is 70%～90% that the described molybdenum plate base press working that is processed into molybdenum target base process becomes the total deformation of molybdenum target base, the deflection that wherein forges processing is 30%-50%, the deflection of rolling processing is 40%～60%, and rolling mode is a unidirection rolling; The vacuum annealing temperature of the molybdenum target base that is processed into is 1000 ℃～1150 ℃, and vacuum tightness is more than or equal to 10
-3Pa, soaking time 1～1.5 hour.
The preparation method of a kind of high-purity molybdenum sputtering targets material of the present invention, the finished product target of preparing, its relative density is 99%～99.9%, and purity is more than or equal to 99.995wt%, and C content is less than 10ppm, and O content is less than 10ppm, and K content is 3-8ppm.Molybdenum sputtering targets material homogeneous grain size, mean grain size are 50 μ m～100 μ m, crystalline orientation with 100}＜011〉be preferential texture orientation.
The preparation method of a kind of high-purity molybdenum sputtering targets material of the present invention, cost is low, and is simple to operate, and equipment requirements is not high.The molybdenum sputtering targets material purity height of preparing, foreign matter content is low, the density height, homogeneous grain size, and specific crystalline orientation is arranged.
Description of drawings
Fig. 1 embodiment 1 uses ammomium dodecamolybdate;
Fig. 2 embodiment 1 molybdenum sputtering targets material microtexture;
Fig. 3 embodiment 2 uses ammomium dodecamolybdate;
Fig. 4 embodiment 2 molybdenum sputtering targets material microtextures;
Fig. 5 embodiment 3 uses ammomium dodecamolybdate;
Fig. 6 embodiment 3 molybdenum sputtering targets material microtextures
Embodiment
A kind of preparation method of high-purity molybdenum sputtering targets material, its preparation process is raw material with the ammomium dodecamolybdate, method by two sections hydrogen reducings is prepared high pure molybdenum powder, then the high pure molybdenum powder isostatic cool pressing is pressed into the molybdenum plate green compact, again through vacuum presintering, high temperature sintering is made high-purity molybdenum plate base under hydrogen atmosphere then; Rolling press working mode was processed into the molybdenum target base after high-purity molybdenum plate base that will sinter at last adopted and forges earlier, and after vacuum annealing, specification is machined to finished product molybdenum sputtering targets material according to the rules again.
During operation, be regular hexa-prism, size evenly with crystal morphology, not having the ammomium dodecamolybdate of reuniting is raw material, control K content is 2～5ppm, Fe content is 3-7ppm, Ni content carries out two sections hydrogen reductions smaller or equal to 2ppm in hydrogen reducing furnace, reducing process carries out according to the reducing process of conventional molybdenum powder.Boat adopts molybdenum boat in the reduction process, and the reduction furnace tube internal surface is inlayed the molybdenum lining, prepares the molybdenum powder of purity more than or equal to 99.99wt%.
The high pure molybdenum powder of preparing is pressed into the molybdenum plate green compact through isostatic cool pressing, pressing pressure 180～200MPa, 10～20 minutes dwell times.Then the molybdenum plate green compact are carried out the vacuum pre-burning, calcined temperature is 1200 ℃～1400 ℃, and vacuum tightness is more than or equal to 10
-3Pa, soaking time 1～2 hour; The pre-molybdenum plate base that burns down carries out high temperature sintering, 1820 ℃～1980 ℃ of sintering temperatures, soaking time 6～8 hours again under hydrogen atmosphere.
Adopt elder generation's rolling processing mode in forging back to carry out press working high-purity molybdenum plate base of preparing and make the molybdenum target base, the press working total deformation is 70%-90%, the deflection that wherein forges processing is 30%-50%, and the deflection of rolling processing is 40%～60%, and rolling mode is a unidirection rolling.The technology of forging and rolling processing is carried out according to the heat processing technique of common molybdenum plate.The molybdenum target base that is processed into is annealed in vacuum annealing furnace, 1000 ℃～1150 ℃ of annealing temperatures, and vacuum tightness is more than or equal to 10
-3Pa, soaking time 1～1.5 hour.
Specification is machined to finished product molybdenum sputtering targets material according to the rules at last.The finished product molybdenum sputtering targets material that is processed into, its relative density is 99%～99.9%, and purity is more than or equal to 99.995wt%, and C content is less than 10ppm, and O content is less than 10ppm, and K content is 3-8ppm.Molybdenum sputtering targets material homogeneous grain size, mean grain size are 50 μ m～100 μ m, crystalline orientation with 100}＜011〉be preferential texture orientation.
Embodiment 1
Be regular hexa-prism, size evenly with crystal morphology, not having the ammomium dodecamolybdate of reuniting is raw material (Fig. 1), and control K content is 5ppm, and Fe content is 7ppm, and Ni content is 2ppm.It is carried out two sections hydrogen reductions in hydrogen reducing furnace, reducing process carries out according to the reducing process of conventional molybdenum powder.Boat adopts molybdenum boat in the reduction process, and the reduction furnace tube internal surface is inlayed the molybdenum lining.The purity of the molybdenum powder of preparing is 99.99wt%.
This molybdenum powder is pressed into the molybdenum plate green compact through isostatic cool pressing, pressing pressure 180MPa, 10 minutes dwell times.Then the molybdenum plate green compact are carried out the vacuum pre-burning, calcined temperature is 1400 ℃, and vacuum tightness is 10
-3Pa, soaking time 1 hour; The pre-molybdenum plate base that burns down carries out high temperature sintering, 1820 ℃ of sintering temperatures, soaking time 6 hours again under hydrogen atmosphere.
Adopt elder generation to forge the rolling press working mode in back high-purity molybdenum plate base of preparing and make the molybdenum target base, the processing total deformation is 70%, and wherein forging the deflection of processing is 30%, and the deflection of rolling processing is 40%, and rolling mode is a unidirection rolling.The technology of forging and rolling processing is carried out according to the heat processing technique of common molybdenum plate.The molybdenum target base that is processed into carries out high temperature annealing at 1150 ℃ in vacuum annealing furnace, vacuum tightness is 10
-3Pa, soaking time 1 hour.At last with the molybdenum target base according to the rules specification be machined to finished product molybdenum sputtering targets material.
The finished product molybdenum sputtering targets material that is processed into, its relative density is 99%, and purity is 99.995wt%, and C content is 6ppm, and O content is 9ppm, K content is 8ppm.Molybdenum sputtering targets material homogeneous grain size, mean grain size are 100 μ m, crystalline orientation with 100}＜011〉be preferential texture orientation.Fig. 2 is the microtexture photo of this molybdenum sputtering targets material.
Embodiment 2
Be regular hexa-prism, size evenly with crystal morphology, not having the ammomium dodecamolybdate of reuniting is raw material (Fig. 3), and control K content is 2ppm, and Fe content is 3ppm, and Ni content is less than 1ppm.It is carried out two sections hydrogen reductions in hydrogen reducing furnace, reducing process carries out according to the reducing process of conventional molybdenum powder.Boat adopts molybdenum boat in the reduction process, and the reduction furnace tube internal surface is inlayed the molybdenum lining.The purity of the molybdenum powder of preparing is 99.992wt%.
This molybdenum powder is pressed into the molybdenum plate green compact through isostatic cool pressing, pressing pressure 200MPa, 20 minutes dwell times.Then the molybdenum plate green compact are carried out the vacuum pre-burning, calcined temperature is 1200 ℃, and vacuum tightness is 10
-4Pa, soaking time 2 hours; The pre-molybdenum plate base that burns down carries out high temperature sintering, 1880 ℃ of sintering temperatures, soaking time 6 hours again under hydrogen atmosphere.
Adopt elder generation to forge the rolling press working mode in back high-purity molybdenum plate base of preparing and make the molybdenum target base, the press working total deformation is 90%, and the deflection that wherein forges processing is 40%, and the deflection of rolling processing is 50%, and rolling mode is a unidirection rolling.The technology of forging and rolling processing is carried out according to the heat processing technique of common molybdenum plate.The molybdenum target base that is processed into carries out high temperature annealing at 1050 ℃ in vacuum annealing furnace, vacuum tightness is 10
-4Pa, soaking time 1 hour.At last with the molybdenum target base according to the rules specification be machined to finished product molybdenum sputtering targets material.
The finished product molybdenum sputtering targets material that is processed into, its relative density is 99.9%, and purity is 99.997wt%, and C is 6ppm, and O content is 8ppm, K content is 5ppm.Molybdenum sputtering targets material homogeneous grain size, mean grain size are 50 μ m, crystalline orientation with 100}＜011〉be preferential texture orientation.Fig. 4 is the microtexture photo of this molybdenum sputtering targets material.
Embodiment 3
Be regular hexa-prism, size evenly with crystal morphology, not having the ammomium dodecamolybdate of reuniting is raw material (Fig. 5), and control K content is 4ppm, and Fe content is 5ppm, and Ni content is 1ppm.It is carried out two sections hydrogen reductions in hydrogen reducing furnace, reducing process carries out according to the reducing process of conventional molybdenum powder.Boat adopts molybdenum boat in the reduction process, and the reduction furnace tube internal surface is inlayed the molybdenum lining.The purity of the molybdenum powder of preparing is 99.99wt%.
This molybdenum powder is pressed into the molybdenum plate green compact through isostatic cool pressing, pressing pressure 180MPa, 15 minutes dwell times.Then the molybdenum plate green compact are carried out the vacuum pre-burning, calcined temperature is 1300 ℃, and vacuum tightness is 10
-4Pa, soaking time 2 hours; The pre-molybdenum plate base that burns down carries out high temperature sintering, 1960 ℃ of hydrogen high temperature sintering temperature, soaking time 8 hours again under hydrogen atmosphere.The purity of the molybdenum plate base of preparing is 99.995wt%,
Adopt elder generation to forge the rolling press working mode in back the molybdenum plate base of preparing and make the molybdenum target base, the press working total deformation is 80%, and the deflection that wherein forges processing is 40%, and the deflection of rolling processing is 40%, and rolling mode is a unidirection rolling.The molybdenum target base that is processed into carries out high temperature annealing at 1050 ℃ in vacuum annealing furnace, vacuum tightness is 10
-4Pa, soaking time 1.5 hours.At last with the molybdenum target base according to the rules specification be machined to finished product molybdenum sputtering targets material.
The finished product molybdenum sputtering targets material that is processed into, its relative density is 99.5%, and purity is 99.996wt%, and C content is 7ppm, and O content is 9ppm, K content is 7ppm.Molybdenum sputtering targets material homogeneous grain size, mean grain size are 70 μ m, crystalline orientation with 100}＜011〉be preferential texture orientation.Fig. 6 is the microtexture photo of this molybdenum sputtering targets material.
Claims (8)
1. the preparation method of a high-purity molybdenum sputtering targets material, it is characterized in that its preparation process is raw material with the ammomium dodecamolybdate, method by two sections hydrogen reducings is prepared high pure molybdenum powder, then high pure molybdenum powder is pressed into the molybdenum plate green compact through isostatic cool pressing, again through vacuum presintering, high temperature sintering is made high-purity molybdenum plate base under hydrogen atmosphere then; Rolling press working mode was processed into the molybdenum target base after high-purity molybdenum plate base that will sinter at last adopted and forges earlier, and after vacuum annealing, specification is machined to finished product molybdenum sputtering targets material according to the rules again.
2. the preparation method of a kind of high-purity molybdenum sputtering targets material according to claim 1 is characterized in that K content is 2～5ppm in the described ammomium dodecamolybdate raw material, and Fe content is 3-7ppm, Ni content is smaller or equal to 2ppm, crystal is the hexa-prism of rule, and size does not evenly have and reunites.
3. the preparation method of a kind of high-purity molybdenum sputtering targets material according to claim 1 is characterized in that described hydrogen reduction method prepares in the process of high pure molybdenum powder, and boat adopts molybdenum boat, and the reduction furnace tube internal surface is inlayed the molybdenum lining; The purity of the molybdenum powder that restores is more than or equal to 99.99wt%.
4. the preparation method of a kind of high-purity molybdenum sputtering targets material according to claim 1, it is characterized in that the described high pure molybdenum powder of preparing by the method for two sections hydrogen reducings is when isostatic cool pressing is made the molybdenum plate green compact, pressing pressure is 180～200MPa, 10～20 minutes dwell times.
5. the preparation method of a kind of high-purity molybdenum sputtering targets material according to claim 1, it is characterized in that described molybdenum plate green compact are through vacuum presintering, high temperature sintering is made in the process of high-purity molybdenum plate base under hydrogen atmosphere then, the vacuum calcined temperature is 1200 ℃～1400 ℃, and vacuum tightness is more than or equal to 10
-3Pa, soaking time 1～2 hour; The high temperature sintering temperature is 1820 ℃～1980 ℃ under the hydrogen atmosphere, soaking time 6～8 hours.
6. the preparation method of a kind of high-purity molybdenum sputtering targets material according to claim 1, it is characterized in that it is 70%～90% that the described high-purity molybdenum plate base press working that is processed into molybdenum target base process becomes the total deformation of molybdenum target base, the deflection that wherein forges processing is 30%-50%, the deflection of rolling processing is 40%～60%, and rolling mode is a unidirection rolling.
7. the preparation method of a kind of high-purity molybdenum sputtering targets material according to claim 1 is characterized in that the annealing temperature of the molybdenum target base vacuum annealing that it is processed into is 1000 ℃～1150 ℃, and vacuum tightness is more than or equal to 10
-3Pa, soaking time 1～1.5 hour.
8. the method for the high-purity molybdenum sputtering targets material of preparation according to claim 1, the relative density that it is characterized in that the finished product molybdenum sputtering targets material prepared is 99%～99.9%, and purity is more than or equal to 99.995wt%, and C content is less than 10ppm, O content is less than 10ppm, and K content is 3-8ppm.Molybdenum sputtering targets material homogeneous grain size, mean grain size are 50 μ m～100 μ m, crystalline orientation with 100}＜011〉be preferential texture orientation.
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| 《中国钼业》 20100630 冯鹏发等 钼及钼合金粉末冶金技术研究现状与发展 39-45 第34卷, 第3期 * |
| 冯鹏发等: "钼及钼合金粉末冶金技术研究现状与发展", 《中国钼业》 * |
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