CN111304607A - Method for manufacturing molybdenum-titanium alloy target - Google Patents
Method for manufacturing molybdenum-titanium alloy target Download PDFInfo
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- CN111304607A CN111304607A CN202010257787.5A CN202010257787A CN111304607A CN 111304607 A CN111304607 A CN 111304607A CN 202010257787 A CN202010257787 A CN 202010257787A CN 111304607 A CN111304607 A CN 111304607A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
- C22C1/0458—Alloys based on titanium, zirconium or hafnium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
Abstract
The invention discloses a method for manufacturing a molybdenum-titanium alloy target, which solves the problems that the existing large-size MoTi alloy target manufacturing method is high in process and equipment cost and is difficult to achieve a proper processing rate. The method comprises the following steps: selecting molybdenum powder and titanium powder, wherein the average grain size of the molybdenum powder is less than 20 microns, and the average grain size of the titanium powder is 10-300 microns; mixing molybdenum powder and titanium powder under the protection of inert gas; carrying out cold isostatic pressing on the mixed powder; performing pressure sintering on the formed molybdenum-titanium mixed powder to obtain a molybdenum-titanium pressing ingot; the pressure in the pressure sintering process is 75-300MPa, the temperature is 650-1000 ℃, and the time is 2-12 hours; rolling the molybdenum-titanium pressed ingot to reach the required size; and carrying out heat treatment on the rolled molybdenum-titanium plate to form a recrystallization structure required by target sputtering, thus obtaining the target plate. Compared with the existing production mode, the invention has lower cost and is not limited by the size of equipment.
Description
Technical Field
The invention relates to a method for manufacturing a MoTi alloy target, in particular to a method for manufacturing a high-generation and large-size MoTi alloy target which can be applied to a flat display panel.
Background
In thin film electrodes of flat display TFT-LCDs, low-resistance Al, Cu, Ag, or the like is used as a wiring material. However, in order to prevent the interdiffusion between the wiring material and the substrate glass and semiconductor from affecting the efficacy of the TFT, a barrier layer material needs to be added between the wiring layer metal and the substrate semiconductor.
The conventional barrier material Ti has high cost due to its etching process, and in recent years, an alloy has been used instead of Ti as a barrier layer, including a MoTi thin film as a substrate or a coating film of a wiring layer material such as Al, Cu, and the like.
With the enlargement of the size of the flat display panel and the requirement of the flat display panel for high efficiency in production, the size of the MoTi target gradually moves to the advanced generation and the large size. The traditional production process of the large-size MoTi alloy target material is twice hot isostatic pressing, a small-size MoTi blank is prepared through the first hot isostatic pressing, and then a plurality of blanks are bonded together to form the final large-size MoTi alloy target material, and the method can be found in patent document CN 10130576A. However, the MoTi alloy targets produced by this process are limited by the size of the equipment used for the second step of hot isostatic pressing, and on the one hand, the equipment cost of the large-size hot isostatic pressing equipment is high, for example, the hot isostatic pressing equipment with the length of 4 meters is needed for the molybdenum titanium targets of 10.5 generations. Even worldwide, the number of devices of corresponding size is small; on the other hand, the hot isostatic pressing process is high in cost, so that the production cost of the molybdenum-titanium target material is high.
When the size of the target material cannot meet the requirement, the traditional method for changing the size of the molybdenum or molybdenum alloy target material is to thermally deform a sintered or hot-isostatic-pressed target material blank in a rolling mode so as to change the length and the thickness of the target material and achieve the required size, for example, in patent CN103146974A, the sintered molybdenum niobium alloy target material is rolled, but for the molybdenum titanium target material, a β -MoTi mixed phase can be formed due to mutual diffusion of molybdenum and titanium at high temperature, β -MoTi is very brittle and is very easy to break in the rolling process, so that the proper processing rate cannot be achieved to change the size.
Disclosure of Invention
The invention provides a method for manufacturing a molybdenum-titanium alloy target, which solves the problems that the conventional method for manufacturing a large-size MoTi alloy target is high in process and equipment cost and is difficult to achieve a proper processing rate.
The technical scheme of the invention is as follows:
a method for manufacturing a molybdenum-titanium alloy target material comprises the following steps:
1) selecting molybdenum powder and titanium powder, wherein the content of the selected titanium powder is 10-90 at%, and the balance is molybdenum powder; the average grain diameter of the molybdenum powder is less than 20 mu m, and the average grain diameter of the titanium powder is 10-300 mu m;
2) mixing molybdenum powder and titanium powder under the protection of inert gas to form mixed powder;
3) carrying out cold isostatic pressing on the mixed powder to ensure that the density of a pressed blank reaches 60-80% of the theoretical density;
4) performing pressure sintering on the formed molybdenum-titanium mixed powder to obtain a molybdenum-titanium pressing ingot; the pressure in the pressure sintering process is 75-300MPa, the temperature is 650-1000 ℃, and the time is 2-12 hours;
5) rolling the molybdenum-titanium pressed ingot to reach the required size;
6) and carrying out heat treatment on the rolled molybdenum-titanium plate to form a recrystallization structure required by target sputtering, thus obtaining the target plate.
Further, the average grain diameter of the molybdenum powder is 2-10 microns, and the average grain diameter of the titanium powder is 20-200 microns.
Further, the titanium powder is spherical titanium powder, and the average grain diameter is 20-150 mu m.
Furthermore, the purity of the molybdenum powder and the purity of the titanium powder are both more than 99.9 percent.
Furthermore, the content of the selected titanium powder is 40-65 at%, and the rest is molybdenum powder.
Further, the pressure sintering operation in step 4) is hot isostatic pressing, vacuum hot pressing or inert gas hot pressing.
Further, the pressure sintering operation in the step 4) is carried out at the pressure of 150-.
Further, the rolling temperature of the rolling treatment in the step 5) is 600-1000 ℃.
Further, the rolling treatment in the step 5) has the rolling temperature of 700-900 ℃, and the rolled plate is annealed under the vacuum condition after each rolling, the annealing temperature of 400-700 ℃, and the annealing time of 0.5-3 hours.
Further, the heat treatment in step 6) is carried out under the conditions of gas pressure lower than 100Pa and temperature of 800-1400 ℃, and the treatment time is 2-12 hours.
The invention has the following beneficial effects:
according to the invention, the size of the MoTi target material is changed by a rolling mode after primary pressure sintering, and the generation of β -MoTi phase is effectively reduced by finely controlling the sizes of Mo particles and Ti particles and the temperature and pressure of the process, so that the satisfactory large-size MoTi alloy target material and the satisfactory processing rate are obtained.
The method is not limited by the size of equipment, the overall process cost is low, and particularly, a better large-size MoTi alloy target can be finally obtained by adding a sheath rolling process after primary hot isostatic pressing.
Drawings
FIG. 1 is a metallographic phase of a molybdenum titanium ingot after HIP.
Fig. 2 shows the metallographic phase of the molybdenum-titanium target after rolling according to an embodiment of the present invention.
FIG. 3 is a phase diagram of molybdenum-titanium alloy.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The concepts of the present invention are described in detail below and further illustrated by the various examples.
Because the β -MoTi alloy phase is very brittle and difficult to roll, the first step pressure sintering (preferably hot isostatic pressing) process of the present invention desirably produces a MoTi sputtering target with trace or substantially no β -MoTi and a target density of 99% or more of theoretical density.
Fig. 3 refers to a phase diagram of molybdenum-titanium alloy (ASM Handbook, vol.3, ASM International, MaterialsPark, OH (1992)). as shown, to avoid the β -MoTi phase formation, the target processing temperature should be controlled at or below the monotectic reaction temperature of 695 ± 20 ℃.
In order to reduce the sintering temperature of the MoTi target material as much as possible, the invention selects the molybdenum powder with smaller grain diameter to promote sintering and improve the sintering density. The preferred average particle size of the molybdenum powder is less than 20 microns, more preferably less than 10 microns. Meanwhile, in order to reduce diffusion, titanium powder with larger particle size is selected, preferably 10-300 microns, and more preferably 20-200 microns. In addition, the shape of the titanium powder is preferably spherical, so that the contact area with the molybdenum powder is reduced, and the interdiffusion degree is reduced; on the other hand, the molybdenum-titanium mixed powder using the spherical titanium powder has higher pressing density, which is beneficial to improving the final sintering density, and when the spherical titanium powder is selected, the particle size of the titanium powder is preferably 20-150 microns. The purity of the molybdenum powder and the titanium powder is at least 99.9 percent.
The molybdenum and titanium powders are mixed under an inert atmosphere using techniques well known in the art. Then carrying out Cold Isostatic Pressing (CIP) molding on the mixed powder to ensure that the compact density reaches 60-80% of the theoretical density.
After the molding, the green compact needs to be sintered under heat and pressure. Sintering methods include, but are not limited to, hot isostatic pressing, vacuum hot pressing, inert gas hot pressing, and the like. The pressure is 75-300MPa, preferably 150-220MPa, the temperature is 650-1000 ℃, preferably 750-900 ℃, and the time is 2-12 hours, preferably 4-8 hours.
Sintering is a hot isostatic pressing process, which requires the green compact to be encapsulated prior to sintering. The packaging material can be selected from low-carbon steel, stainless steel and the like. After encapsulation the compact is degassed under vacuum. The degassing pressure is less than 0.01Pa, and the degassing temperature is 200-400 ℃.
And after hot pressing, obtaining the molybdenum-titanium pressed ingot. And rolling the molybdenum-titanium pressing ingot to enable the size of the molybdenum-titanium pressing ingot to meet the length requirement of the required target. The rolling temperature is 600-1000 ℃, and preferably 700-900 ℃. When the overall deformation ratio is large, it is necessary to anneal the rolled sheet after each rolling. The annealing is preferably carried out under vacuum conditions at an annealing temperature of 400-700 ℃ for an annealing time of 0.5-3 hours.
After the rolling step is completed, the target material needs to be subjected to high-temperature heat treatment to form a recrystallization structure required by target material sputtering. The high-temperature heat treatment is carried out in vacuum, the gas pressure is less than 100Pa, the heat treatment temperature is 800-1400 ℃, and the treatment time is 2-12 hours.
Finally, the target plate is machined and then bonded to a backing plate to form the final sputtering target.
Example one (the best mode)
Mixing molybdenum powder with particle size of 4-5 μm and titanium powder with particle size of 20 μm at atom ratio of 1: 1. A V-shaped mixer is used in the mixing process, and argon is introduced for protection. And (3) performing cold isostatic pressing on the mixed molybdenum-titanium mixed powder to form the molybdenum-titanium mixed powder. The molding pressure is 150MPa, and the dwell time is 300 s. And coating the outside of the formed molybdenum-titanium pressing ingot with a steel plate, and degassing at 200 ℃ at a degassing pressure of 0.01 Pa. Thereafter, the molybdenum titanium compact was subjected to pressure sintering (hot isostatic pressing). The pressure sintering temperature is 850 ℃, the pressure is 180MPa, and the pressure maintaining time is 4 hours. A molybdenum titanium compact with a density of 7.11g/cm3 was obtained. And removing the coated steel plate, and rolling the molybdenum-titanium pressing ingot. The rolling temperature was 800 ℃ and the total deformation was 40%. After alkali cleaning, leveling, annealing and surface mechanical processing, high-temperature heat treatment is carried out before the surface mechanical processing, the treatment is carried out under the conditions of gas pressure lower than 100Pa and 800-1400 ℃, and the treatment time is 2-12 hours, so as to obtain the molybdenum-titanium bare target. FIG. 1 is a side metallographic photograph of a molybdenum titanium compact obtained after HIP; FIG. 2 is a side metallographic photograph of the rolled molybdenum-titanium target material. As can be seen, molybdenum and titanium are distributed in a two-phase manner in the target material; after rolling, the two phases are uniformly extended in the rolling direction, and the final tissue is uniform and fine.
For visual comparison, other embodiments are described below in table 1 with reference to embodiment one; the parameters and specific operations not mentioned in table 1 are equivalent to those of the first embodiment.
Table 1 examples one to eight
As can be seen from table 1, based on the principle of the present invention, the proper adjustment of the main process parameters can achieve better effect than the prior art.
Finally, it should be noted that: the above embodiments are only used for illustrating the technical solutions of the present application, and not for limiting the same; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present application.
Claims (10)
1. A method for manufacturing a molybdenum-titanium alloy target is characterized by comprising the following steps:
1) selecting molybdenum powder and titanium powder, wherein the content of the selected titanium powder is 10-90 at%, and the balance is molybdenum powder; the average grain diameter of the molybdenum powder is less than 20 mu m, and the average grain diameter of the titanium powder is 10-300 mu m;
2) mixing molybdenum powder and titanium powder under the protection of inert gas to form mixed powder;
3) carrying out cold isostatic pressing on the mixed powder to ensure that the density of a pressed blank reaches 60-80% of the theoretical density;
4) performing pressure sintering on the formed molybdenum-titanium mixed powder to obtain a molybdenum-titanium pressing ingot; the pressure in the pressure sintering process is 75-300MPa, the temperature is 650-1000 ℃, and the time is 2-12 hours;
5) rolling the molybdenum-titanium pressed ingot to reach the required size;
6) and carrying out heat treatment on the rolled molybdenum-titanium plate to form a recrystallization structure required by target sputtering, thus obtaining the target plate.
2. The method for manufacturing a molybdenum-titanium alloy target according to claim 1, wherein: the average grain diameter of the molybdenum powder is 2-10 microns, and the average grain diameter of the titanium powder is 20-200 microns.
3. The method for manufacturing a molybdenum-titanium alloy target according to claim 1 or 2, wherein: the titanium powder is spherical titanium powder, and the average grain diameter is 20-150 mu m.
4. The method for manufacturing a molybdenum-titanium alloy target according to claim 1, wherein: the purity of the molybdenum powder and the titanium powder is more than 99.9 percent.
5. The method for manufacturing a molybdenum-titanium alloy target according to claim 1, wherein: the content of the selected titanium powder is 40-65 at%, and the rest is molybdenum powder.
6. The method for manufacturing a molybdenum-titanium alloy target according to claim 1, wherein: the pressure sintering operation in the step 4) is hot isostatic pressing, vacuum hot pressing or inert gas hot pressing.
7. The method for manufacturing a molybdenum-titanium alloy target according to claim 1 or 6, wherein: the pressure sintering operation in the step 4) is carried out, the pressure is 150-220MPa, the temperature is 750-900 ℃, and the time is 4-8 hours.
8. The method for manufacturing a molybdenum-titanium alloy target according to claim 1, wherein: the rolling treatment in the step 5) has the rolling temperature of 600-1000 ℃.
9. The method for manufacturing a molybdenum-titanium alloy target according to claim 8, wherein: the rolling treatment in the step 5) has the rolling temperature of 700-900 ℃, and the rolled plate is annealed under the vacuum condition after each rolling, the annealing temperature is 400-700 ℃, and the annealing time is 0.5-3 hours.
10. The method for manufacturing a molybdenum-titanium alloy target according to claim 1, wherein: the heat treatment in the step 6) is carried out under the conditions of gas pressure lower than 100Pa and temperature of 800-1400 ℃, and the treatment time is 2-12 hours.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113463042A (en) * | 2021-05-31 | 2021-10-01 | 洛阳科威钨钼有限公司 | Preparation method of molybdenum-titanium alloy sputtering coating target material |
| CN115502403A (en) * | 2022-09-29 | 2022-12-23 | 宁波江丰电子材料股份有限公司 | Preparation method of large-size and high-density molybdenum target |
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2020
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113463042A (en) * | 2021-05-31 | 2021-10-01 | 洛阳科威钨钼有限公司 | Preparation method of molybdenum-titanium alloy sputtering coating target material |
| CN115502403A (en) * | 2022-09-29 | 2022-12-23 | 宁波江丰电子材料股份有限公司 | Preparation method of large-size and high-density molybdenum target |
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