CN114029484A - Preparation method of tantalum-titanium alloy target material - Google Patents
Preparation method of tantalum-titanium alloy target material Download PDFInfo
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- CN114029484A CN114029484A CN202111315033.1A CN202111315033A CN114029484A CN 114029484 A CN114029484 A CN 114029484A CN 202111315033 A CN202111315033 A CN 202111315033A CN 114029484 A CN114029484 A CN 114029484A
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- 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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- B22F3/14—Both compacting and sintering simultaneously
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- B22F9/00—Making metallic powder or suspensions thereof
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- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- 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
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- 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
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- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
The invention relates to a preparation method of a tantalum-titanium alloy target material, which comprises the following steps: (1) respectively carrying out first heat treatment and second heat treatment on tantalum powder and titanium powder, and then mixing to obtain tantalum-titanium mixed powder; (2) sequentially carrying out sheath degassing and cold isostatic pressing treatment on the tantalum-titanium mixed powder obtained in the step (1) to obtain a tantalum-titanium pressed compact; (3) and (3) sequentially carrying out third heat treatment and hot isostatic pressing treatment on the tantalum-titanium pressed compact obtained in the step (2) to obtain the tantalum-titanium alloy target. The preparation method of the tantalum-titanium alloy target provided by the invention can effectively solve the problems of pores, uneven components and the like in the target, improves the density of the target to more than 99%, and improves the purity of the target to more than 99.95%.
Description
Technical Field
The invention relates to the field of targets, in particular to a preparation method of a tantalum-titanium alloy target.
Background
Tantalum and titanium in the tantalum-titanium alloy target belong to high-temperature metals, and the target is usually manufactured by adopting a powder metallurgy sintering mode. In the target manufacturing process, the temperature cannot meet the requirement due to equipment limitation, so that the target cannot be densified, and the obtained target generally has the micro defects of more pores, uneven components and the like, and cannot meet the requirement of magnetron sputtering.
Meanwhile, the purity of the target directly influences the performance of the sputtered film, and if the content of impurities in the target is high, impurities are easily introduced during sputtering, so that a sputtered film loop is short-circuited; impurities can also introduce protrusions into the film, reducing the performance of the sputtered film. The common impurities in the target material are mainly O, C, H and the like, and in the film sputtering process, O, C, H and other impurities are easy to discharge in the sputtering process, so that the uniformity of the sputtered film is reduced.
CN110952064A discloses a tantalum-silicon alloy sputtering target and a preparation method thereof, and the method comprises the steps of mixing tantalum powder and silicon powder, and then sequentially carrying out cold isostatic pressing treatment, degassing treatment, hot isostatic pressing treatment and machining to obtain the tantalum-silicon alloy sputtering target. Because the content of O, C, H and other impurities in the tantalum powder is high, the impurities in the target material are not removed by the method, and the purity of the obtained tantalum-silicon alloy sputtering target material is low.
CN112111714A discloses a preparation method of a tantalum-aluminum alloy sputtering target, which comprises the steps of mixing tantalum powder and aluminum powder, and then carrying out hot-pressing sintering treatment and machining to obtain the tantalum-aluminum alloy sputtering target. Because tantalum belongs to high-temperature metal, the sintering temperature of the method is higher, and the compactness of the obtained target is lower.
Therefore, how to improve the compactness and the purity of the tantalum-titanium alloy target and reduce the impurity content of the target is a problem to be solved at present.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a method for preparing a tantalum-titanium alloy target, which can effectively solve the problems of pores, uneven components, etc. in the target, improve the density and purity of the target, and make the internal structure good, compared with the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a tantalum-titanium alloy target material, which comprises the following steps:
(1) respectively carrying out first heat treatment and second heat treatment on tantalum powder and titanium powder, and then mixing to obtain tantalum-titanium mixed powder;
(2) sequentially carrying out sheath degassing and cold isostatic pressing treatment on the tantalum-titanium mixed powder obtained in the step (1) to obtain a tantalum-titanium pressed compact;
(3) sequentially carrying out third heat treatment and hot isostatic pressing treatment on the tantalum-titanium pressed compact obtained in the step (2) to obtain a tantalum-titanium alloy target material;
the first heat treatment and the second heat treatment in the step (1) have no sequential relation.
According to the invention, the tantalum powder and the titanium powder are respectively subjected to the first heat treatment and the second heat treatment, so that H impurities contained in the tantalum powder and the titanium powder can be removed, the purity of a tantalum-titanium target product is improved, the target can be preformed by further performing sheath degassing and cold isostatic pressing treatment, then O impurities contained in the target can be further removed by the third heat treatment, and the density of the target is further improved by the hot isostatic pressing treatment. Compared with the traditional preparation method of the target material, the preparation method provided by the invention can effectively remove impurities such as H, O and the like contained in the target material through the first heat treatment, the second heat treatment and the third heat treatment, so that the purity of the target material reaches more than 99.95%; because high-temperature metals such as tantalum, titanium and the like need high sintering temperature, the invention reduces the heat treatment temperature in the traditional target preparation process through three times of heat treatment, reduces the equipment requirement and ensures that the compactness of the obtained tantalum-titanium alloy target reaches more than 99 percent.
Preferably, the tantalum powder of step (1) has a particle size of < 46 μm, and may be, for example, 45 μm, 42 μm, 40 μm, 38 μm, 34 μm, 32 μm, 30 μm, 28 μm, 26 μm, 24 μm, 22 μm, 20 μm, 18 μm, 16 μm, 14 μm, 12 μm or 10 μm, but is not limited to the values listed, and other values not listed within the range of values are equally applicable.
The method preferably controls the granularity of the tantalum powder within a specific range, can ensure the packing density of the powder, improves the compactness of the target material, and simultaneously can ensure that the internal structure of the target material is more uniform.
Preferably, the tantalum powder has a purity of 99.95% or more, such as 99.95%, 99.96%, 99.97%, 99.98%, 99.99%, 99.991%, 99.992%, 99.993%, 99.994%, or 99.995%, but is not limited to the recited values, and other values not recited in the numerical range are equally applicable.
Preferably, the titanium powder has a particle size of < 48 μm, for example 46 μm, 44 μm, 42 μm, 40 μm, 38 μm, 36 μm, 34 μm, 32 μm, 30 μm, 28 μm, 26 μm, 24 μm, 22 μm, 20 μm, 18 μm, 16 μm, 14 μm, 12 μm or 10 μm, but is not limited to the values listed, and other values not listed in the numerical range are equally applicable.
The invention preferably controls the granularity of the titanium powder within a specific range, can ensure the packing density of the powder, improves the compactness of the target material and simultaneously ensures that the internal structure of the target material is more uniform.
Preferably, the titanium powder has a purity of 99.98% or more, and may be, for example, 99.98%, 99.99%, 99.991%, 99.992%, 99.993%, 99.994% or 99.995%, but is not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the temperature of the first heat treatment in step (1) is 850-.
The temperature of the first heat treatment is preferably controlled within a specific range, so that the growth of crystal grains can be avoided, and the internal structure of the target material is more uniform.
Preferably, the temperature of the second heat treatment is 700-800 ℃, and may be, for example, 700 ℃, 710 ℃, 720 ℃, 730 ℃, 740 ℃, 750 ℃, 760 ℃, 770 ℃, 780 ℃, 790 ℃ or 800 ℃, but is not limited to the recited values, and other values not recited in the numerical range are also applicable.
The temperature of the second heat treatment is preferably controlled within a specific range, so that the growth of crystal grains can be avoided, and the internal structure of the target material is more uniform.
Preferably, the atomic ratio of tantalum powder to titanium powder in the mixing in step (1) is (0.9-1.2):1, and may be, for example, 0.9:1, 1:1, 1.1:1 or 1.2:1, but is not limited to the values recited, and other values not recited in the range of values are equally applicable.
Preferably, the mixing in step (1) comprises ball milling.
Preferably, the mass ratio of the tantalum-titanium mixed powder to the grinding balls in the ball milling is (9-11):1, and may be, for example, 9:1, 9.5:1, 10:1, 10.5:1 or 11:1, but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
Preferably, the grinding balls comprise titanium balls and/or tantalum balls.
The grinding balls are preferably titanium balls and/or tantalum balls, so that other impurities can be prevented from being introduced in the powder mixing process.
Preferably, the mixing time is 48h or more, for example 48h, 50h, 52h, 54h, 56h, 58h, 60h, 62h, 64h, 66h, 68h or 70h, but is not limited to the values listed, and other values not listed in the numerical range are equally applicable.
In the invention, the mixing time is preferably controlled within a specific range, so that the tantalum powder and the titanium powder can be fully and uniformly mixed, and the agglomeration of large particles is avoided.
Preferably, the mixed atmosphere comprises nitrogen and/or an inert gas.
In the present invention, it is preferable that the atmosphere for controlling the mixing, preferably argon, includes nitrogen and/or inert gas, so that the gas does not affect the purity of the powder.
In the invention, after the mixing is finished, more than 3 parts of tantalum-titanium mixed powder is randomly taken, the atomic percentage content of titanium element in the tantalum-titanium mixed powder is detected, and the fluctuation of the atomic percentage content of titanium is +/-10 percent, so that the tantalum-titanium mixed powder is proved to be uniformly mixed.
Preferably, the degassing of the sheath in the step (2) comprises degassing by placing tantalum-titanium mixed powder into a die.
Preferably, a degassing tube is arranged on the top of the mould.
Preferably, a separation layer is arranged between the degassing nozzle and the powder.
Preferably, the isolation layer includes a first isolation layer, a second isolation layer, and a third isolation layer sequentially disposed along an outer surface of the powder.
According to the invention, the tantalum-titanium mixed powder is filled into the die with the degassing pipe arranged at the top, and the isolating layer is arranged between the powder contacting with the degassing pipe opening and the degassing pipe opening, so that the powder in the die can be prevented from being pumped out in the air pumping process.
Preferably, the material of the first isolation layer comprises graphite.
Preferably, the material of the second isolation layer comprises glass wool.
Preferably, the material of the third isolation layer comprises graphite.
In the invention, a first isolating layer, a second isolating layer and a third isolating layer are preferably arranged between the degassing pipe orifice and the powder, and can be combined with oxygen removed from the pressed compact in the subsequent third heat treatment process, so that O impurities contained in the pressed compact can be removed, the purity of the target material is improved, and the purity of the graphite is more than or equal to 99.999%.
Preferably, the temperature at which the jacket is degassed is 500-600 deg.C, and may be, for example, 500 deg.C, 520 deg.C, 540 deg.C, 560 deg.C, 580 deg.C or 600 deg.C, but is not limited to the recited values, and other values not recited within the range of values are equally applicable.
Preferably, the time for degassing the sheath is 8-20h, for example 8h, 10h, 12h, 14h, 16h, 18h or 20h, but is not limited to the values listed, and other values not listed in the range of values are equally applicable.
Preferably, the end point of degassing of the jacket is an absolute vacuum degree of 0.003Pa or less, and may be, for example, 0.003Pa, 0.002Pa, 0.001Pa, 0.0008Pa, 0.0006Pa, 0.0004Pa or 0.0002Pa, but is not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the pressure of the cold isostatic pressing in step (2) is 130-170MPa, such as 130MPa, 135MPa, 140MPa, 145MPa, 150MPa, 155MPa, 160MPa, 165MPa or 170MPa, but not limited to the values listed, and other values not listed in the numerical range are equally applicable, preferably 150-160 MPa.
In the present invention, it is preferable to control the pressure of the cold isostatic pressing within a specific range so that the target material can be preformed and preliminarily densified.
Preferably, the cold isostatic pressing is carried out for a time of 10 to 20 minutes, such as 10 minutes, 11 minutes, 12 minutes, 13 minutes, 14 minutes, 15 minutes, 16 minutes, 17 minutes, 18 minutes, 19 minutes or 20 minutes, but not limited to the cited values, within which other values not cited apply, preferably 15 to 18 minutes.
Preferably, the temperature of the third heat treatment in step (3) is 900-.
In the invention, the temperature of the third heat treatment is preferably controlled within a specific range, so that the growth of crystal grains caused by overhigh heating temperature of the target material can be avoided, O impurities contained in the target material can be effectively removed, and the purity of the target material is improved.
Preferably, the hot isostatic pressing treatment in step (3) is carried out at 1200-1300 ℃, for example, 1200 ℃, 1210 ℃, 1220 ℃, 1230 ℃, 1240 ℃, 1250 ℃, 1260 ℃, 1270 ℃, 1280 ℃, 1290 ℃ or 1300 ℃, but not limited to the recited values, and other values not recited in the range of values are also applicable.
In the invention, the temperature of the hot isostatic pressing treatment is preferably controlled in a specific range, so that the target material can be more densified and has higher density.
Preferably, the pressure of the hot isostatic pressing treatment is 130-150MPa, and may be 130MPa, 132MPa, 134MPa, 136MPa, 138MPa, 140MPa, 142MPa, 144MPa, 146MPa, 148MPa or 150MPa, for example, but not limited to the recited values, and other values not recited in the numerical range are also applicable.
In the invention, the pressure of the hot isostatic pressing treatment is preferably controlled in a specific range, so that the target material can be more densified and has higher density.
Preferably, the hot isostatic pressing is carried out for a period of time of 3 to 5 hours, for example 3 hours, 3.2 hours, 3.4 hours, 3.6 hours, 3.8 hours, 4 hours, 4.2 hours, 4.4 hours, 4.6 hours, 4.8 hours or 5 hours, but not limited to the values listed, and other values not listed within the numerical ranges are equally applicable.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) performing first heat treatment on tantalum powder with the granularity of less than 46 mu m and the purity of more than or equal to 99.95% at the temperature of 850-900 ℃, performing second heat treatment on titanium powder with the granularity of less than 48 mu m and the purity of more than or equal to 99.98% at the temperature of 700-800 ℃, and then performing ball milling on the obtained tantalum powder and the titanium powder according to the atomic ratio of (0.9-1.2):1 to obtain tantalum-titanium mixed powder, wherein the mass ratio of the tantalum-titanium mixed powder to grinding balls in the ball milling is (9-11):1, the ball milling grinding balls comprise titanium balls and/or tantalum balls, the ball milling time is more than or equal to 48 hours, and the ball milling atmosphere comprises nitrogen and/or inert gas;
(2) placing the tantalum-titanium mixed powder obtained in the step (1) into a mold, degassing at the temperature of 500-; a degassing pipe is arranged at the top of the die, a first isolation layer, a second isolation layer and a third isolation layer are sequentially arranged between the degassing pipe opening and the powder along the outer surface of the powder, the first isolation layer is made of graphite, the second isolation layer is made of glass wool, and the third isolation layer is made of graphite;
(3) and (3) carrying out third heat treatment on the tantalum titanium compact obtained in the step (2) at the temperature of 900-.
Compared with the prior art, the invention has the following beneficial effects:
(1) the preparation method of the tantalum-titanium alloy target material provided by the invention can effectively solve the problems of holes, uneven components and the like in the target material, and can improve the density of the target material to more than 99%.
(2) The preparation method of the tantalum-titanium alloy target material provided by the invention can reduce the content of impurity elements such as H, O in the target material and improve the purity of the target material to more than 99.95%.
Drawings
Fig. 1 is a process flow chart of a method for preparing a tantalum-titanium alloy target in an embodiment of the invention.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Specifically, a preparation method of a tantalum-titanium alloy target is provided, as shown in fig. 1, tantalum powder and titanium powder are subjected to first heat treatment and second heat treatment respectively and then mixed to obtain tantalum-titanium mixed powder; and sequentially carrying out sheath degassing, cold isostatic pressing, third heat treatment and hot isostatic pressing on the tantalum-titanium mixed powder to obtain the tantalum-titanium alloy target material.
Example 1
The embodiment provides a preparation method of a tantalum-titanium alloy target, which comprises the following steps:
(1) performing first heat treatment on tantalum powder with the granularity of 10-20 microns and the purity of 99.95% at 880 ℃, performing second heat treatment on titanium powder with the granularity of 10-20 microns and the purity of 99.98% at 750 ℃, and then performing ball milling on the obtained tantalum powder and titanium powder according to the atomic ratio of 1:1 to obtain tantalum-titanium mixed powder, wherein the mass ratio of the tantalum-titanium mixed powder to grinding balls in the ball milling is 10:1, the ball milling is performed on the titanium balls, the ball milling time is 60 hours, and the ball milling atmosphere is argon;
(2) placing the tantalum-titanium mixed powder obtained in the step (1) into a mold, degassing at 550 ℃ for 14h until the absolute vacuum degree is 0.001Pa, and then carrying out cold isostatic pressing at 150MPa for 15 minutes to obtain a tantalum-titanium pressed blank; a degassing pipe is arranged at the top of the die, a first isolation layer, a second isolation layer and a third isolation layer are sequentially arranged between the degassing pipe opening and the powder along the outer surface of the powder, the first isolation layer is made of graphite, the second isolation layer is made of glass wool, and the third isolation layer is made of graphite;
(3) and (3) carrying out third heat treatment on the tantalum titanium pressed compact obtained in the step (2) at 950 ℃, and then carrying out hot isostatic pressing treatment for 4h at 1250 ℃ and 140MPa to obtain the tantalum titanium alloy target.
Example 2
The embodiment provides a preparation method of a tantalum-titanium alloy target, which comprises the following steps:
(1) performing first heat treatment on tantalum powder with the granularity of 20-30 microns and the purity of 99.95% at 850 ℃, performing second heat treatment on titanium powder with the granularity of 20-30 microns and the purity of 99.98% at 700 ℃, and then performing ball milling on the obtained tantalum powder and titanium powder according to the atomic ratio of 0.9:1 to obtain tantalum-titanium mixed powder, wherein the mass ratio of the tantalum-titanium mixed powder to grinding balls in the ball milling is 11:1, the ball milling is performed on the titanium balls, the ball milling time is 50 hours, and the ball milling atmosphere is nitrogen;
(2) placing the tantalum-titanium mixed powder obtained in the step (1) into a mold, degassing at 500 ℃ for 20 hours until the absolute vacuum degree is 0.003Pa, and then carrying out cold isostatic pressing at 130MPa for 20 minutes to obtain a tantalum-titanium pressed compact; a degassing pipe is arranged at the top of the die, a first isolation layer, a second isolation layer and a third isolation layer are sequentially arranged between the degassing pipe opening and the powder along the outer surface of the powder, the first isolation layer is made of graphite, the second isolation layer is made of glass wool, and the third isolation layer is made of graphite;
(3) and (3) carrying out third heat treatment on the tantalum titanium compact obtained in the step (2) at 900 ℃, and then carrying out hot isostatic pressing treatment for 5h at 1300 ℃ and 130MPa to obtain the tantalum titanium alloy target.
Example 3
The embodiment provides a preparation method of a tantalum-titanium alloy target, which comprises the following steps:
(1) performing first heat treatment on tantalum powder with the granularity of 30-40 microns and the purity of 99.96% at 900 ℃, performing second heat treatment on titanium powder with the granularity of 30-40 microns and the purity of more than or equal to 99.99% at 800 ℃, and then performing ball milling on the obtained tantalum powder and titanium powder according to the atomic ratio of 1.2:1 to obtain tantalum-titanium mixed powder, wherein the mass ratio of the tantalum-titanium mixed powder to grinding balls in the ball milling is 9:1, the ball milling is performed on the grinding balls for 55 hours, and the ball milling atmosphere is argon;
(2) placing the tantalum-titanium mixed powder obtained in the step (1) into a mold, degassing at 600 ℃ for 8 hours until the absolute vacuum degree is 0.003Pa, and then carrying out cold isostatic pressing at 170MPa for 10 minutes to obtain a tantalum-titanium pressed compact; a degassing pipe is arranged at the top of the die, a first isolation layer, a second isolation layer and a third isolation layer are sequentially arranged between the degassing pipe opening and the powder along the outer surface of the powder, the first isolation layer is made of graphite, the second isolation layer is made of glass wool, and the third isolation layer is made of graphite;
(3) and (3) carrying out third heat treatment on the tantalum titanium pressed compact obtained in the step (2) at 1000 ℃, and then carrying out hot isostatic pressing treatment for 3h at 1200 ℃ and 150MPa to obtain the tantalum titanium alloy target.
Example 4
The embodiment provides a preparation method of a tantalum-titanium alloy target, which is only characterized in that the granularity of tantalum powder is 50-60 mu m compared with that of embodiment 1.
Example 5
The embodiment provides a preparation method of a tantalum-titanium alloy target, which is only characterized in that the granularity of titanium powder is 60-70 μm compared with that of embodiment 1.
Example 6
This example provides a method for preparing a tantalum-titanium alloy target, which only includes removing the second isolation layer and the third isolation layer compared to example 1.
Example 7
This example provides a method for preparing a tantalum-titanium alloy target, which only includes the step of hot isostatic pressing treatment at 1150 ℃ as compared with example 1.
Example 8
This example provides a method for preparing a tantalum-titanium alloy target, which only involves a hot isostatic pressing pressure of 120MPa compared to example 1.
Comparative example 1
The present comparative example provides a method for preparing a tantalum-titanium alloy target material, which is only characterized by removing the first heat treatment compared with example 1.
Comparative example 2
The present comparative example provides a method for preparing a tantalum-titanium alloy target material, which is only characterized by removing the second heat treatment compared with example 1.
Comparative example 3
The comparative example provides a preparation method of a tantalum-titanium alloy target, which only eliminates cold isostatic pressing treatment compared with example 1.
Comparative example 4
The comparative example provides a method for preparing a tantalum-titanium alloy target, which only eliminates the third heat treatment compared with example 1.
Comparative example 5
The comparative example provides a preparation method of a tantalum-titanium alloy target, which is only used for removing hot isostatic pressing treatment compared with example 1.
The compactness of the tantalum-titanium alloy targets obtained in examples 1 to 8 and comparative examples 1 to 5 was tested by a metal material density tester, and the results are shown in table 1.
The purity of the tantalum-titanium alloy target materials obtained in examples 1 to 8 and comparative examples 1 to 5 was measured by Glow Discharge Mass Spectrometry (GDMS), and the results are shown in table 1.
TABLE 1
| Density/% | Purity/%) | |
| Example 1 | 99.90 | 99.99 |
| Example 2 | 99.87 | 99.96 |
| Example 3 | 99.80 | 99.97 |
| Example 4 | 99.20 | 99.99 |
| Example 5 | 99.00 | 99.98 |
| Example 6 | 99.70 | 99.96 |
| Example 7 | 99.00 | 99.99 |
| Example 8 | 99.00 | 99.99 |
| Comparative example 1 | 99.90 | 99.90 |
| Comparative example 2 | 99.90 | 99.91 |
| Comparative example 3 | 97.90 | 99.99 |
| Comparative example 4 | 98.20 | 99.90 |
| Comparative example 5 | 81.60 | 99.99 |
From table 1, the following points can be seen:
(1) from the examples 1 to 3, it can be seen that the compactness of the target can be improved to more than 99.80% and the purity of the target can be improved to more than 99.96% by using the preparation method of the tantalum-titanium alloy target described in the examples 1 to 3.
(2) It can be seen from the combination of example 1 and examples 4-5 that the particle size of the tantalum powder in example 1 is 10-20 μm, the particle size of the titanium powder is 10-20 μm, and the compactness of the tantalum-titanium alloy target in example 1 is 99.90% compared with the particle size of the tantalum powder in example 4 being 50-60 μm, and the particle size of the titanium powder in example 5 being 60-70 μm, while the compactness of the tantalum-titanium alloy target in examples 4 and 5 is 99.20% and 99.00%, respectively, thereby showing that the invention preferably controls the particle sizes of the tantalum powder and the titanium powder in specific ranges, and can improve the compactness of the target.
(3) It can be seen from the combination of example 1 and example 6 that, in example 6, compared with example 1, only the second isolation layer and the third isolation layer are removed, the density of the tantalum-titanium alloy target material in example 1 is 99.90% and the purity is 99.99%, whereas the density of the tantalum-titanium alloy target material in example 6 is only 99.70% and the purity is 99.96%, which shows that the density and the purity of the target material can be improved by preferably providing three isolation layers in the present invention.
(4) It can be seen from the combination of example 1 and examples 7-8 that the temperature of the hot isostatic pressing treatment in example 1 is 1250 ℃ and the pressure is 140MPa, and the density of the tantalum-titanium alloy target in example 1 is 99.90% compared with the temperature of the hot isostatic pressing treatment in example 7 being 1150 ℃ and the pressure of the hot isostatic pressing treatment in example 8 being 120MPa, while the density of the target in examples 7 and 8 is only 99.00%, thereby showing that the density of the target can be improved by controlling the temperature and the pressure of the hot isostatic pressing treatment in specific ranges preferably.
(5) Combining example 1 and comparative examples 1-5, it can be seen that comparative examples 1-5 eliminate the first heat treatment, the second heat treatment, the cold isostatic pressing treatment, the third heat treatment and the hot isostatic pressing treatment, respectively, and the density of the tantalum-titanium alloy target material in example 1 is 99.90% and the purity is 99.99%, while the purity of the target material in comparative examples 1-2 and comparative example 4 is lower than that in example 1, and the density of the target material in comparative examples 3-5 is lower than that in example 1, thereby showing that the compactness and purity of the target material can be improved by the combined operation of the first heat treatment, the second heat treatment, the cold isostatic pressing treatment, the third heat treatment and the hot isostatic pressing treatment.
In conclusion, the preparation method of the tantalum-titanium alloy target material provided by the invention can provide the compactness and the purity of the target material, and has higher application value.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. The preparation method of the tantalum-titanium alloy target is characterized by comprising the following steps:
(1) respectively carrying out first heat treatment and second heat treatment on tantalum powder and titanium powder, and then mixing to obtain tantalum-titanium mixed powder;
(2) sequentially carrying out sheath degassing and cold isostatic pressing treatment on the tantalum-titanium mixed powder obtained in the step (1) to obtain a tantalum-titanium pressed compact;
(3) sequentially carrying out third heat treatment and hot isostatic pressing treatment on the tantalum-titanium pressed compact obtained in the step (2) to obtain a tantalum-titanium alloy target material;
the first heat treatment and the second heat treatment in the step (1) have no sequential relation.
2. The method according to claim 1, wherein the tantalum powder of step (1) has a particle size of < 46 μm;
preferably, the purity of the tantalum powder is more than or equal to 99.95 percent;
preferably, the particle size of the titanium powder is less than 48 μm;
preferably, the purity of the titanium powder is more than or equal to 99.98 percent.
3. The method as claimed in claim 1 or 2, wherein the temperature of the first heat treatment in step (1) is 850-;
preferably, the temperature of the second heat treatment is 700-.
4. The production method according to any one of claims 1 to 3, wherein the atomic ratio of tantalum powder to titanium powder in the mixing in step (1) is (0.9-1.2): 1.
5. The method of any one of claims 1 to 4, wherein the mixing of step (1) comprises ball milling;
preferably, the mass ratio of the tantalum-titanium mixed powder to the grinding balls in the ball milling is (9-11): 1;
preferably, the grinding balls comprise titanium balls and/or tantalum balls;
preferably, the mixing time is more than or equal to 48 hours;
preferably, the mixed atmosphere comprises nitrogen and/or an inert gas.
6. The manufacturing method according to any one of claims 1 to 5, wherein the degassing of the capsule in the step (2) includes degassing by placing the tantalum-titanium mixed powder into a mold;
preferably, a degassing pipe is arranged at the top of the mold;
preferably, an isolating layer is arranged between the degassing pipe orifice and the powder;
preferably, the isolation layer comprises a first isolation layer, a second isolation layer and a third isolation layer which are sequentially arranged along the outer surface of the powder;
preferably, the material of the first isolation layer comprises graphite;
preferably, the material of the second isolation layer comprises glass wool;
preferably, the material of the third isolation layer comprises graphite;
preferably, the degassing temperature of the sheath is 500-600 ℃;
preferably, the degassing time of the sheath is 8-20 h;
preferably, the end point of degassing of the sheath is that the absolute vacuum degree is less than or equal to 0.003 Pa.
7. The preparation method according to any one of claims 1 to 6, wherein the pressure of the cold isostatic pressing treatment in step (2) is 130-170MPa, preferably 150-160 MPa;
preferably, the cold isostatic pressing treatment time is 10-20 minutes, preferably 15-18 minutes.
8. The method according to any one of claims 1 to 7, wherein the temperature of the third heat treatment in step (3) is 900-1000 ℃.
9. The method according to any one of claims 1 to 8, wherein the temperature of the hot isostatic pressing treatment in step (3) is 1200-1300 ℃;
preferably, the pressure of the hot isostatic pressing treatment is 130-150 MPa;
preferably, the hot isostatic pressing treatment time is 3-5 h.
10. The method of any one of claims 1 to 9, comprising the steps of:
(1) performing first heat treatment on tantalum powder with the granularity of less than 46 mu m and the purity of more than or equal to 99.95% at the temperature of 850-900 ℃, performing second heat treatment on titanium powder with the granularity of less than 48 mu m and the purity of more than or equal to 99.98% at the temperature of 700-800 ℃, and then performing ball milling on the obtained tantalum powder and the titanium powder according to the atomic ratio of (0.9-1.2):1 to obtain tantalum-titanium mixed powder, wherein the mass ratio of the tantalum-titanium mixed powder to grinding balls in the ball milling is (9-11):1, the ball milling grinding balls comprise titanium balls and/or tantalum balls, the ball milling time is more than or equal to 48 hours, and the ball milling atmosphere comprises nitrogen and/or inert gas;
(2) placing the tantalum-titanium mixed powder obtained in the step (1) into a mold, degassing at the temperature of 500-; a degassing pipe is arranged at the top of the die, a first isolation layer, a second isolation layer and a third isolation layer are sequentially arranged between the degassing pipe opening and the powder along the outer surface of the powder, the first isolation layer is made of graphite, the second isolation layer is made of glass wool, and the third isolation layer is made of graphite;
(3) and (3) carrying out third heat treatment on the tantalum titanium compact obtained in the step (2) at the temperature of 900-.
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