CN114029484B - Preparation method of tantalum-titanium alloy target - Google Patents

Abstract

The invention relates to a preparation method of a tantalum-titanium alloy target, 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 performing 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 material can effectively solve the problems of holes, uneven components and the like in the target material, improves the density of the target material to more than 99 percent, and improves the purity of the target material to more than 99.95 percent.

Description

Preparation method of tantalum-titanium alloy target

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 a tantalum-titanium alloy target belong to high-temperature metals, and the target is usually manufactured by adopting a powder metallurgy sintering mode. In the process of manufacturing the target, the temperature cannot meet the requirement due to equipment limitation, the target cannot be densified, and the obtained target generally has microscopic defects of more air holes, 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 impurity content in the target is relatively high, impurities are easily introduced during sputtering, so that a short circuit occurs in a sputtered film loop; impurities can also introduce protrusions into the film, reducing the performance of the sputtered film. The common impurities in the target material mainly include O, C, H and the like, and in the thin film sputtering process, the impurities such as O, C, H and the like are easy to discharge in the sputtering process, so that the uniformity of the sputtered thin film is reduced.

CN110952064a discloses a tantalum-silicon alloy sputtering target and a preparation method thereof, wherein the tantalum-silicon alloy sputtering target is obtained by mixing tantalum powder and silicon powder, and then sequentially performing cold isostatic pressing treatment, degassing treatment, hot isostatic pressing treatment and machining. The impurity content of O, C, H and the like in the tantalum powder is relatively high, and impurities in the target are not removed by the method, so that the purity of the obtained tantalum-silicon alloy sputtering target is relatively low.

CN112111714a discloses a method for preparing a tantalum-aluminum alloy sputtering target, which comprises the steps of mixing tantalum powder and aluminum powder, and then performing 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 relatively high, and the density of the obtained target material is relatively low.

Therefore, how to improve the compactness and 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

Compared with the prior art, the preparation method of the tantalum-titanium alloy target can effectively solve the problems of holes, uneven components and the like in the target, improve the density and purity of the target and enable the internal tissue structure to be good.

In order to achieve the aim of the invention, the invention adopts the following technical scheme:

the invention provides a preparation method of a tantalum-titanium alloy target, 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 performing 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 performing 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;

the first heat treatment and the second heat treatment in the step (1) have no sequence relation.

According to the invention, the first heat treatment and the second heat treatment are respectively carried out on the tantalum powder and the titanium powder, 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 through sheath degassing and cold isostatic pressing treatment, then O impurities contained in the target can be further removed through third heat treatment, and the compactness of the target is further improved through hot isostatic pressing treatment. Compared with the traditional target preparation method, the preparation method provided by the invention can effectively remove the impurities such as H, O and the like contained in the target through the first heat treatment, the second heat treatment and the third heat treatment, so that the purity of the target is more than 99.95%; because high sintering temperature is required for high-temperature metals such as tantalum, titanium and the like, 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 density 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. Mu.m, 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 not limited to the values recited, other non-recited values within the range of values being equally applicable.

The invention 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, and can make the internal structure of the target 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 not limited to the recited values, and other non-recited values within the range of values are equally applicable.

Preferably, the particle size of the titanium powder is < 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 not limited to the values recited, other values not recited in the numerical range are equally applicable.

The invention preferably controls the granularity of the titanium powder in a specific range, can ensure the packing density of the powder, improves the density of the target material, and can make the internal structure of the target material more uniform.

Preferably, the purity of the titanium powder is greater than or equal to 99.98%, 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 non-recited values within the range of values are equally applicable.

Preferably, the temperature of the first heat treatment in the step (1) is 850-900 ℃, for example 850 ℃, 860 ℃, 870 ℃, 880 ℃, 890 ℃ or 900 ℃, but the method is not limited to the listed values, and other non-listed values in the numerical range are applicable.

The invention preferably controls the temperature of the first heat treatment in a specific range, can avoid the growth of crystal grains and ensures that the internal structure of the target is more uniform.

The temperature of the second heat treatment is preferably 700 to 800 ℃, and may be 700 ℃, 710 ℃, 720 ℃, 730 ℃, 740 ℃, 750 ℃, 760 ℃, 770 ℃, 780 ℃, 790 ℃, or 800 ℃, for example, but not limited to the values recited, and other values not recited in the numerical range are equally applicable.

The invention preferably controls the temperature of the second heat treatment in a specific range, can avoid the growth of crystal grains and ensures that the internal structure of the target is more uniform.

Preferably, the atomic ratio of tantalum powder to titanium powder in the mixing in the step (1) is (0.9-1.2): 1, for example, may be 0.9:1, 1:1, 1.1:1 or 1.2:1, but is not limited to the recited values, and other non-recited values in the numerical range are equally applicable.

Preferably, the means of mixing in step (1) comprises ball milling.

Preferably, the mass ratio of the tantalum titanium mixed powder to the grinding balls in the ball mill is (9-11): 1, for example, the mass ratio can be 9:1, 9.5:1, 10:1, 10.5:1 or 11:1, but the mass ratio is not limited to the listed values, and other non-listed values in the numerical range are equally 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, and meanwhile, the lining of the ball mill is made of polyurethane or titanium materials in the ball milling process, so that other impurities can be further prevented from being introduced in the powder mixing process.

Preferably, the mixing time is not less than 48 hours, and may be, for example, 48 hours, 50 hours, 52 hours, 54 hours, 56 hours, 58 hours, 60 hours, 62 hours, 64 hours, 66 hours, 68 hours or 70 hours, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.

The invention preferably controls the mixing time in a specific range, so that the tantalum powder and the titanium powder can be fully and uniformly mixed, and large particle agglomeration is avoided.

Preferably, the mixed atmosphere comprises nitrogen and/or an inert gas.

In the present invention, the mixed atmosphere is preferably controlled to include nitrogen and/or inert gas, and the influence of the gas on the purity of the powder can be avoided, and the mixed atmosphere is preferably argon.

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%, so that the tantalum-titanium mixed powder is proved to be uniformly mixed.

Preferably, the degassing of the sheath in the step (2) comprises putting tantalum-titanium mixed powder into a die for degassing.

Preferably, a degassing pipe is arranged at the top of the die.

Preferably, a separation layer is arranged between the degassing pipe orifice and the powder.

Preferably, the barrier layer includes a first barrier layer, a second barrier layer, and a third barrier layer sequentially disposed along an outer surface of the powder.

In the invention, 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 the degassing pipe orifice and the degassing pipe orifice, so that the powder in the die can be prevented from being extracted in the air extraction process.

Preferably, the material of the first isolation layer includes graphite.

Preferably, the material of the second isolation layer includes glass wool.

Preferably, the material of the third isolation layer includes graphite.

In the invention, the first isolation layer, the second isolation layer and the third isolation 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 a target material is improved, and the purity of graphite is more than or equal to 99.999 percent.

Preferably, the temperature of the sheath degassing is 500-600 ℃, for example 500 ℃, 520 ℃, 540 ℃, 560 ℃, 580 ℃ or 600 ℃, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.

Preferably, the sheath is degassed for a period of time ranging from 8 to 20 hours, such as 8 hours, 10 hours, 12 hours, 14 hours, 16 hours, 18 hours, or 20 hours, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.

Preferably, the end point of the degassing of the sheath is equal to or less than 0.003Pa, for example, 0.003Pa, 0.002Pa, 0.001Pa, 0.0008Pa, 0.0006Pa, 0.0004Pa or 0.0002Pa, but the end point is not limited to the recited values, and other non-recited values in the range of values are equally applicable.

Preferably, the pressure of the cold isostatic pressing treatment in step (2) is 130-170MPa, for example 130MPa, 135MPa, 140MPa, 145MPa, 150MPa, 155MPa, 160MPa, 165MPa or 170MPa, but not limited to the values listed, other non-listed values in the range of values are equally applicable, preferably 150-160MPa.

In the present invention, the pressure of the cold isostatic pressing treatment is preferably controlled within a specific range, and the target material can be preformed and preliminarily densified.

Preferably, the cold isostatic pressing is performed for a period of time ranging from 10 to 20 minutes, for example, from 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 recited values, and other non-recited values within the range of values are equally applicable, preferably from 15 to 18 minutes.

Preferably, the temperature of the third heat treatment in the step (3) is 900 to 1000 ℃, for example, 900 ℃, 910 ℃, 920 ℃, 930 ℃, 940 ℃, 950 ℃, 960 ℃, 970 ℃, 980 ℃, 990 ℃ or 1000 ℃, but the temperature is not limited to the values listed, and other values not listed in the numerical range are equally applicable.

In the invention, the temperature of the third heat treatment is preferably controlled in a specific range, so that the growth of crystal grains caused by the overhigh heating temperature of the target can be avoided, and meanwhile, the O impurity contained in the target can be effectively removed, and the purity of the target is improved.

Preferably, the temperature of the hot isostatic pressing treatment in step (3) is 1200-1300 ℃, for example 1200 ℃, 1210 ℃, 1220 ℃, 1230 ℃, 1240 ℃, 1250 ℃, 1260 ℃, 1270 ℃, 1280 ℃, 1290 ℃ or 1300 ℃, but not limited to the values listed, other values not listed in the numerical range are equally applicable.

In the invention, the temperature of the hot isostatic pressing treatment is preferably controlled within a specific range, so that the target material can be more densified and the compactness is higher.

Preferably, the pressure of the hot isostatic pressing treatment is 130-150MPa, for example 130MPa, 132MPa, 134MPa, 136MPa, 138MPa, 140MPa, 142MPa, 144MPa, 146MPa, 148MPa or 150MPa, but not limited to the values listed, and other values not listed in the numerical range are equally applicable.

In the invention, the pressure of the hot isostatic pressing treatment is preferably controlled within a specific range, so that the target material can be more densified and the compactness is higher.

Preferably, the time of the hot isostatic pressing treatment is 3-5h, for example, 3h, 3.2h, 3.4h, 3.6h, 3.8h, 4h, 4.2h, 4.4h, 4.6h, 4.8h or 5h, but not limited to the recited values, other non-recited values in the range of values are equally applicable.

As a preferred technical scheme of the invention, the preparation method comprises the following steps:

(1) Carrying out first heat treatment on tantalum powder with the granularity less than 46 mu m and the purity more than or equal to 99.95 percent at 850-900 ℃, carrying out second heat treatment on titanium powder with the granularity less than 48 mu m and the purity more than or equal to 99.98 percent at 700-800 ℃, and then carrying out ball milling on the obtained tantalum powder and 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 the grinding balls in the ball milling is (9-11): 1, the ball milled 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) Putting the tantalum-titanium mixed powder obtained in the step (1) into a die, degassing at 500-600 ℃ for 8-20h until the absolute vacuum degree is less than or equal to 0.003Pa, and then performing cold isostatic pressing at 130-170MPa for 10-20 min to obtain a tantalum-titanium pressed compact; the top of the die is provided with a degassing pipe, a first isolation layer, a second isolation layer and a third isolation layer are sequentially arranged between the degassing pipe orifice and 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) performing third heat treatment on the tantalum-titanium pressed compact obtained in the step (2) at 900-1000 ℃, and performing hot isostatic pressing treatment for 3-5h at 1200-1300 ℃ and 130-150MPa to obtain the tantalum-titanium alloy target.

Compared with the prior art, the invention has the following beneficial effects:

(1) The preparation method of the tantalum-titanium alloy target material 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 can reduce the content of H, O and other impurity elements in the target material and improve the purity of the target material to more than 99.95 percent.

Drawings

FIG. 1 is a process flow diagram of a method for preparing a tantalum-titanium alloy target in accordance with an embodiment of the invention.

Detailed Description

The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.

Specifically, as shown in fig. 1, tantalum powder and titanium powder are mixed after being subjected to first heat treatment and second heat treatment respectively, so as to obtain tantalum-titanium mixed powder; and carrying out sheath degassing, cold isostatic pressing treatment, third heat treatment and hot isostatic pressing treatment on the tantalum-titanium mixed powder in sequence to obtain the tantalum-titanium alloy target.

Example 1

The embodiment provides a preparation method of a tantalum-titanium alloy target, which comprises the following steps:

(1) Carrying out first heat treatment on tantalum powder with the granularity of 10-20 mu m and the purity of 99.95% at 880 ℃, carrying out second heat treatment on titanium powder with the granularity of 10-20 mu m and the purity of 99.98% at 750 ℃, and then carrying out 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 grinding balls in the ball milling are titanium balls, the ball milling time is 60h, and the ball milling atmosphere is argon;

(2) Putting the tantalum-titanium mixed powder obtained in the step (1) into a die, degassing at 550 ℃ for 14h until the absolute vacuum degree is 0.001Pa, and then performing cold isostatic pressing treatment at 150MPa for 15 minutes to obtain a tantalum-titanium pressed compact; the top of the die is provided with a degassing pipe, a first isolation layer, a second isolation layer and a third isolation layer are sequentially arranged between the degassing pipe orifice and 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) performing third heat treatment on the tantalum-titanium pressed compact obtained in the step (2) at 950 ℃, and performing hot isostatic pressing treatment for 4 hours 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) Carrying out first heat treatment on tantalum powder with the granularity of 20-30 mu m and the purity of 99.95% at 850 ℃, carrying out second heat treatment on titanium powder with the granularity of 20-30 mu m and the purity of 99.98% at 700 ℃, and then carrying out 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 grinding balls in the ball milling are titanium balls, the ball milling time is 50h, and the ball milling atmosphere is nitrogen;

(2) Putting the tantalum-titanium mixed powder obtained in the step (1) into a die, degassing at 500 ℃ for 20 hours until the absolute vacuum degree is 0.003Pa, and then performing cold isostatic pressing treatment at 130MPa for 20 minutes to obtain a tantalum-titanium pressed compact; the top of the die is provided with a degassing pipe, a first isolation layer, a second isolation layer and a third isolation layer are sequentially arranged between the degassing pipe orifice and 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) performing third heat treatment on the tantalum-titanium pressed compact obtained in the step (2) at 900 ℃, and performing hot isostatic pressing treatment for 5 hours 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) Carrying out first heat treatment on tantalum powder with the granularity of 30-40 mu m and the purity of 99.96 percent at 900 ℃, carrying out second heat treatment on titanium powder with the granularity of 30-40 mu m and the purity of more than or equal to 99.99 percent at 800 ℃, and then carrying out 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 grinding balls in the ball milling are tantalum balls, the ball milling time is 55h, and the ball milling atmosphere is argon;

(2) Putting the tantalum-titanium mixed powder obtained in the step (1) into a die, degassing at 600 ℃ for 8 hours until the absolute vacuum degree is 0.003Pa, and then performing cold isostatic pressing treatment at 170MPa for 10 minutes to obtain a tantalum-titanium pressed compact; the top of the die is provided with a degassing pipe, a first isolation layer, a second isolation layer and a third isolation layer are sequentially arranged between the degassing pipe orifice and 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) performing third heat treatment on the tantalum-titanium pressed compact obtained in the step (2) at 1000 ℃, and performing hot isostatic pressing treatment for 3 hours at 1200 ℃ and 150MPa to obtain the tantalum-titanium alloy target.

Example 4

The present example provides a method for preparing tantalum-titanium alloy targets, which is characterized in that the particle size of tantalum powder is 50-60 μm as compared with example 1.

Example 5

The present example provides a method for preparing a tantalum-titanium alloy target, which is characterized in that the particle size of the titanium powder is 60-70 μm as compared with example 1.

Example 6

This example provides a method for preparing a tantalum-titanium alloy target, which is compared with example 1 only in that the second isolation layer and the third isolation layer are removed.

Example 7

The present example provides a method for preparing a tantalum-titanium alloy target, which is characterized in that the temperature of the hot isostatic pressing treatment is 1150 ℃ compared with example 1.

Example 8

The present example provides a method for preparing a tantalum-titanium alloy target, which is characterized in that the pressure of the hot isostatic pressing treatment is 120MPa as compared with example 1.

Comparative example 1

This comparative example provides a method of preparing a tantalum titanium alloy target with only the removal of the first heat treatment as compared to example 1.

Comparative example 2

This comparative example provides a method of preparing a tantalum titanium alloy target with only the removal of the second heat treatment as compared to example 1.

Comparative example 3

This comparative example provides a method for preparing a tantalum titanium alloy target, which is compared with example 1 only in that the cold isostatic pressing treatment is removed.

Comparative example 4

This comparative example provides a method for preparing a tantalum titanium alloy target with only the elimination of the third heat treatment compared to example 1.

Comparative example 5

This comparative example provides a method for preparing a tantalum titanium alloy target with only the removal of the hot isostatic pressing treatment compared to example 1.

The density of the tantalum-titanium alloy targets obtained in examples 1 to 8 and comparative examples 1 to 5 was measured by a metal material density tester, and the results are shown in Table 1.

The purity of the tantalum-titanium alloy targets 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 embodiment 1-3, the preparation method of the tantalum-titanium alloy target material in the embodiment 1-3 can improve the density of the target material to more than 99.80%, and can improve the purity of the target material to more than 99.96%.

(2) It can be seen from a combination of examples 1 and 4-5 that the tantalum powder of example 1 has a particle size of 10-20 μm and the titanium powder has a particle size of 10-20 μm, and that the tantalum titanium alloy target of example 1 has a density of 99.90% and the tantalum titanium alloy target of examples 4 and 5 has a density of 99.20% and 99.00%, respectively, compared to the tantalum powder of example 4 having a particle size of 50-60 μm and the titanium powder of example 5 having a particle size of 60-70 μm, thus indicating that the invention preferably controls the particle sizes of tantalum powder and titanium powder within a specific range, and can improve the density of the target.

(3) It can be seen from the combination of example 1 and example 6 that example 6 is only to remove the second isolation layer and the third isolation layer compared with example 1, the density of the tantalum-titanium alloy target material in example 1 is 99.90%, the purity is 99.99%, and the density of the tantalum-titanium alloy target material in example 6 is only 99.70%, and the purity is 99.96%, thus indicating that the invention preferably provides three isolation layers, and the density and purity of the target material can be improved.

(4) It can be seen from the combination of examples 1 and examples 7 to 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 material in example 1 is 99.90% and the density of the target material in examples 7 and 8 is only 99.00% 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, thus showing that the invention can improve the density of the target material by preferably controlling the temperature and the pressure of the hot isostatic pressing treatment in a specific range.

(5) It can be seen from the combination of examples 1 and comparative examples 1 to 5 that the first heat treatment, the second heat treatment, the cold isostatic pressing treatment, the third heat treatment and the hot isostatic pressing treatment are removed from comparative examples 1 to 5, respectively, the tantalum titanium alloy target material in example 1 has a density of 99.90% and a purity of 99.99%, and the targets in comparative examples 1 to 2 and 4 have a purity lower than that in example 1 and the targets in comparative examples 3 to 5 have a density lower than that in example 1, respectively, thereby indicating that the invention can improve the density and purity of the target material 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 purity of the target material, and has higher application value.

The applicant declares that the above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that are easily conceivable within the technical scope of the present invention disclosed by the present invention fall within the scope of the present invention and the disclosure.

Claims (22)

1. The preparation method of the tantalum-titanium alloy target is characterized by comprising the following steps of:

(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; the temperature of the first heat treatment is 850-900 ℃, and the temperature of the second heat treatment is 700-800 ℃;

(2) Sequentially performing 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;

the method comprises the steps that the packaging and degassing are carried out by putting tantalum-titanium mixed powder into a die, a degassing pipe is arranged at the top of the die, an isolation layer is arranged between a degassing pipe orifice and the powder, 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, 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) Sequentially performing 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;

the temperature of the third heat treatment is 900-1000 ℃;

the first heat treatment and the second heat treatment in the step (1) have no sequence relation.

2. The method of claim 1, wherein the tantalum powder of step (1) has a particle size of < 46 μm.

3. The method of claim 1, wherein the tantalum powder has a purity of 99.95% or more.

4. The method according to claim 1, wherein the particle size of the titanium powder is < 48 μm.

5. The method according to claim 1, wherein the purity of the titanium powder is not less than 99.98%.

6. The method according to claim 1, wherein the atomic ratio of tantalum powder to titanium powder in the mixing of step (1) is (0.9-1.2): 1.

7. The method of claim 1, wherein the means of mixing in step (1) comprises ball milling.

8. The method according to claim 7, wherein the mass ratio of the tantalum titanium mixed powder to the grinding balls in the ball mill is (9-11): 1.

9. The method of manufacturing according to claim 8, characterized in that the grinding balls comprise titanium balls and/or tantalum balls.

10. The method according to claim 1, wherein the mixing time is not less than 48 hours.

11. The method of claim 1, wherein the mixed atmosphere comprises nitrogen and/or an inert gas.

12. The method of claim 1, wherein the temperature of the sheath degassing in step (2) is 500-600 ℃.

13. The method of claim 1, wherein the sheath is degassed for a period of 8 to 20 hours.

14. The method of claim 1, wherein the end point of the sheath degassing is at an absolute vacuum of 0.003Pa or less.

15. The method according to claim 1, wherein the cold isostatic pressure treatment in step (2) is performed at a pressure of 130-170MPa.

16. The method of claim 15, wherein the cold isostatic pressure treatment in step (2) is performed at a pressure of 150-160MPa.

17. The method of claim 1, wherein the cold isostatic pressing is performed for a period of 10 to 20 minutes.

18. The method of claim 17, wherein the cold isostatic pressing is performed for a period of 15-18 minutes.

19. The method of claim 1, wherein the temperature of the hot isostatic pressing treatment in step (3) is 1200-1300 ℃.

20. The method according to claim 1, wherein the hot isostatic pressure treatment is performed at a pressure of 130-150MPa.

21. The method of claim 1, wherein the hot isostatic pressing is performed for a period of 3-5 hours.

22. The preparation method according to claim 1, characterized in that the preparation method comprises the steps of:

(1) Carrying out first heat treatment on tantalum powder with the granularity less than 46 mu m and the purity more than or equal to 99.95 percent at 850-900 ℃, carrying out second heat treatment on titanium powder with the granularity less than 48 mu m and the purity more than or equal to 99.98 percent at 700-800 ℃, and then carrying out ball milling on the obtained tantalum powder and 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 the grinding balls in the ball milling is (9-11): 1, the ball milled 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) Putting the tantalum-titanium mixed powder obtained in the step (1) into a die, degassing at 500-600 ℃ for 8-20h until the absolute vacuum degree is less than or equal to 0.003Pa, and then performing cold isostatic pressing at 130-170MPa for 10-20 min to obtain a tantalum-titanium pressed compact; the top of the die is provided with a degassing pipe, a first isolation layer, a second isolation layer and a third isolation layer are sequentially arranged between the degassing pipe orifice and 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) performing third heat treatment on the tantalum-titanium pressed compact obtained in the step (2) at 900-1000 ℃, and performing hot isostatic pressing treatment for 3-5h at 1200-1300 ℃ and 130-150MPa to obtain the tantalum-titanium alloy target.