阅读说明：本技术 一种铌合金溅射靶材及其制备方法 (Niobium alloy sputtering target material and preparation method thereof ) 是由 方宏 张雪凤 孙虎民 于 2021-07-16 设计创作，主要内容包括：本发明公开了一种铌合金溅射靶材及其制备方法,铌合金溅射靶材中含铌元素40～80份、钛元素20～60份；铌合金溅射靶材的制备方法为：将铌粉、钛粉、活性碳粉在保护气体作用下充分混合均匀得到混合粉末；然后将混合粉末装入胶套内,进行冷等静压成型,得到坯体；之后将坯体装入包套并进行真空除气,对除气后的包套进行热等静压处理,得到烧结坯；将烧结坯在保护气氛下加热,然后热轧、校平、退火,得到铌合金板坯；最后对铌合金板坯进行磨削加工,即得到铌合金溅射靶材。采用该方法生产的铌合金溅射靶材,纯度高,晶粒细小,可以用于制作在TFT-LCD制程中与铜膜层配套使用的过渡层材料,在耐蚀性、热稳定性等方面与铜膜层具有良好的匹配性,改善TFT-LCD制程中的不良。(The invention discloses a niobium alloy sputtering target material and a preparation method thereof, wherein the niobium alloy sputtering target material contains 40-80 parts of niobium element and 20-60 parts of titanium element; the preparation method of the niobium alloy sputtering target material comprises the following steps: fully and uniformly mixing niobium powder, titanium powder and activated carbon powder under the action of protective gas to obtain mixed powder; then, the mixed powder is filled into a rubber sleeve and is subjected to cold isostatic pressing to obtain a blank; then, the green body is put into a sheath, vacuum degassing is carried out, and hot isostatic pressing treatment is carried out on the sheath after the degassing to obtain a sintered blank; heating the sintered blank in a protective atmosphere, and then carrying out hot rolling, leveling and annealing to obtain a niobium alloy plate blank; and finally, grinding the niobium alloy plate blank to obtain the niobium alloy sputtering target. The niobium alloy sputtering target material produced by the method has high purity and fine crystal grains, can be used for manufacturing a transition layer material matched with a copper film layer in the TFT-LCD manufacturing process, has good matching property with the copper film layer in the aspects of corrosion resistance, thermal stability and the like, and improves the defects in the TFT-LCD manufacturing process.)

1. The preparation method of the niobium alloy sputtering target is characterized in that the niobium alloy sputtering target comprises, by mass, 40-80 parts of niobium element and 20-60 parts of titanium element;

the preparation method of the niobium alloy sputtering target mainly comprises the following steps:

taking 40-80 parts by mass of niobium powder, 20-60 parts by mass of titanium powder and 0.1-0.3 part by mass of activated carbon powder, carrying out ball milling and mixing under the atmosphere of protective gas, and fully and uniformly mixing to obtain mixed powder;

step two, filling the mixed powder obtained in the step one into a rubber sleeve, and then carrying out cold isostatic pressing to obtain a blank;

step three, the green body obtained in the step two is placed into a sheath and sealed, vacuum degassing is carried out, and hot isostatic pressing treatment is carried out on the sheath after the degassing to obtain a sintered blank;

step four, heating the sintered blank obtained in the step three under a protective atmosphere, then carrying out hot rolling and leveling, and finally carrying out annealing to obtain a niobium alloy plate blank;

and step five, grinding the niobium alloy plate blank obtained in the step four to obtain the niobium alloy sputtering target material.

2. The method for preparing a niobium alloy sputtering target according to claim 1, wherein the method comprises the following steps: in the first step, the purity of niobium powder and titanium powder is not lower than 99.9%, and the niobium powder and the titanium powder are sieved by a 200-mesh sieve; the purity of the activated carbon powder is not less than 99.9 percent, and the activated carbon powder is sieved by a 100-mesh sieve.

3. The method for preparing a niobium alloy sputtering target according to claim 1, wherein the method comprises the following steps: in the first step, the ball milling and mixing process comprises the following steps: placing niobium powder, titanium powder and activated carbon powder in a V-shaped mixer, introducing argon as protective gas, and mixing according to a ball-to-material ratio of 1: 1-1.5 for 12-48 h.

4. The method for preparing a niobium alloy sputtering target according to claim 1, wherein the method comprises the following steps: and step two, after the mixed powder is filled into a rubber sleeve, compacting the rubber sleeve on a vibration platform, and reinforcing the rubber sleeve by using a steel plate.

5. The method for preparing a niobium alloy sputtering target according to claim 1, wherein the method comprises the following steps: and in the second step, the cold isostatic pressure is 100-300 MPa, and the pressure maintaining time is 3-10 min.

6. The method for preparing a niobium alloy sputtering target according to claim 1, wherein the method comprises the following steps: in the third step, the sheath material is a carbon steel plate or a stainless steel plate, the vacuum degassing heating temperature is 400-700 ℃, the vacuum degree is lower than 10-2Pa, and the vacuumizing retention time is 2-6 h.

7. The method for preparing a niobium alloy sputtering target according to claim 1, wherein the method comprises the following steps: in the third step, the technological parameters of the hot isostatic pressing operation are as follows: argon is used as a medium, the pressure is 100-200 MPa, the temperature is 1000-1500 ℃, and the holding time is 3-10 h.

8. The method for preparing a niobium alloy sputtering target according to claim 1, wherein the method comprises the following steps: and in the fourth step, argon is used as protective gas for heating before hot rolling, the heating temperature is 300-1000 ℃, the hot rolling is divided into 3-5 rolling passes, and the rolling deformation of each pass is not lower than 20%.

9. The method for preparing a niobium alloy sputtering target according to claim 1, wherein the method comprises the following steps: in the fourth step, the annealing temperature is 800-.

10. A niobium alloy sputtering target material, which is prepared by the preparation method according to any one of claims 1 to 9.

Technical Field

The invention relates to the field of preparation of high-purity metal targets, in particular to a niobium alloy sputtering target and a preparation method thereof.

Background

The TFT-LCD (thin film transistor liquid crystal display) occupies an important position in the technology of large-sized display panels due to its mature process and relatively low price. At present, the technology of large-size TFT-LCD display panels develops towards the directions of high resolution, high refresh rate, low delay and the like. The conductivity requirements for the TFT electrode wiring materials that carry the signal transmission are correspondingly increasing. Copper has gradually replaced aluminum as a signal transmission layer due to its excellent conductive properties. However, due to the material characteristics of copper, it is often necessary to match the transition layer to improve the application characteristics of the material. The transition layer materials commonly used at present are pure molybdenum, molybdenum alloy and the like, but the materials are easy to be poor due to the mismatching of certain physical and chemical properties of the materials and the copper film layer.

Therefore, a new transition layer material is needed to improve the matching performance with the physical and chemical properties of the copper film and improve the defects in the TFT-LCD process.

Disclosure of Invention

In order to overcome the defects in the prior art, the invention provides the niobium alloy sputtering target material and the preparation method thereof. The copper-based composite material can be used for manufacturing a transition layer material matched with a copper film layer in a TFT-LCD (thin film transistor-liquid crystal display) manufacturing process, has good matching property with the copper film layer in the aspects of corrosion resistance, thermal stability and the like, and improves the defects in the TFT-LCD manufacturing process. The preparation method provided by the invention is simple in process and suitable for batch production.

In order to achieve the purpose, the invention adopts the specific scheme that:

the preparation method of the niobium alloy sputtering target comprises the following steps of (by mass), 40-80 parts of niobium element and 20-60 parts of titanium element in the niobium alloy sputtering target;

the preparation method of the niobium alloy sputtering target mainly comprises the following steps:

taking 40-80 parts by mass of niobium powder, 20-60 parts by mass of titanium powder and 0.1-0.3 part by mass of activated carbon powder, carrying out ball milling and mixing under the atmosphere of protective gas, and fully and uniformly mixing to obtain mixed powder;

step two, filling the mixed powder obtained in the step one into a rubber sleeve, and then carrying out cold isostatic pressing to obtain a blank;

step three, the green body obtained in the step two is placed into a sheath and sealed, vacuum degassing is carried out, and hot isostatic pressing treatment is carried out on the sheath after the degassing to obtain a sintered blank;

step four, heating the sintered blank obtained in the step three under a protective atmosphere, then carrying out hot rolling and leveling, and finally carrying out annealing to obtain a niobium alloy plate blank;

and step five, grinding the niobium alloy plate blank obtained in the step four to obtain the niobium alloy sputtering target material.

Further, in the first step, the purity of the niobium powder and the titanium powder is not lower than 99.9 percent, and the niobium powder and the titanium powder are sieved by a 200-mesh sieve; the purity of the activated carbon powder is not less than 99.9 percent, and the activated carbon powder is sieved by a 100-mesh sieve.

Further, in the step one, the ball milling and mixing process comprises the following steps: placing niobium powder, titanium powder and activated carbon powder in a V-shaped mixer, introducing argon as protective gas, and mixing according to a ball-to-material ratio of 1: 1-1.5 for 12-48 h.

And further, in the second step, after the mixed powder is filled into a rubber sleeve, the rubber sleeve is vibrated and compacted on a vibration platform and is reinforced by a steel plate.

Further, in the second step, the cold isostatic pressure is 100-300 MPa, and the pressure maintaining time is 3-10 min.

Further, in the third step, the sheath material is a carbon steel plate or a stainless steel plate, the vacuum degassing heating temperature is 400-700 ℃, and the vacuum degree is lower than 10^-2Pa，The vacuumizing and maintaining time is 2-6 h.

Further, in the third step, the process parameters of the hot isostatic pressing operation are as follows: argon is used as a medium, the pressure is 100-200 MPa, the temperature is 1000-1500 ℃, and the holding time is 3-10 h.

Further, in the fourth step, argon is used as protective gas for heating before hot rolling, the heating temperature is 300-1000 ℃, the hot rolling is carried out by 3-5 passes, and the rolling deformation of each pass is not lower than 20%.

Further, in the fourth step, the annealing temperature is 800-.

The niobium alloy sputtering target material is prepared by the preparation method.

Has the advantages that:

1. the niobium alloy sputtering target material produced by the invention has fine crystal grains, the average crystal grain size is less than 100 microns, the relative density of the target material is not less than 99.5 percent, the purity of the target material is not less than 99.9 percent, the niobium alloy sputtering target material can be used for manufacturing a transition layer material matched with a copper film layer in a TFT-LCD (thin film transistor-liquid crystal display) manufacturing process, has good matching property with the copper film layer in the aspects of corrosion resistance, thermal stability and the like, and improves the defects in the TFT manufacturing process. The preparation method provided by the invention is simple in process and suitable for batch production.

2. The invention adds the activated carbon powder in the process of preparing the niobium alloy sputtering target, and aims to effectively remove oxygen impurities in powder blanks in the vacuum degassing stage before hot isostatic pressing.

3. The niobium alloy sputtering target material disclosed by the invention contains a titanium element in addition to a niobium element, and has the effects of adjusting the corrosion resistance of the material, achieving better matching with a copper film layer and simultaneously enabling the material to have good thermal stability.

Detailed Description

The technical solutions of the present invention will be described clearly and completely with reference to specific embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, belong to the scope of the present invention.

The preparation method of the niobium alloy sputtering target comprises the following steps of (by mass), 40-80 parts of niobium element and 20-60 parts of titanium element in the niobium alloy sputtering target;

the preparation method of the niobium alloy sputtering target mainly comprises the following steps:

taking 40-80 parts of niobium powder, 20-60 parts of titanium powder and 0.1-0.3 part of activated carbon powder by mass, wherein the purity of the niobium powder and the purity of the titanium powder are not lower than 99.9%, and sieving the niobium powder and the titanium powder by a 200-mesh sieve; the purity of the activated carbon powder is not lower than 99.9%, the activated carbon powder is sieved by a 100-mesh sieve, the activated carbon powder is placed in a V-shaped mixer under the atmosphere of protective gas, argon is introduced as protective gas, the materials are mixed according to the ball-to-material ratio of 1: 1-1.5, and the materials are fully and uniformly mixed for 12-48 hours to obtain mixed powder;

step two, filling the mixed powder obtained in the step one into a rubber sleeve, compacting the rubber sleeve on a vibration platform, reinforcing the rubber sleeve by using a steel plate, and then performing cold isostatic pressing, wherein the cold isostatic pressing pressure is 100-300 MPa, and the pressure maintaining time is 3-10 min, so as to obtain a blank;

step three, the blank obtained in the step two is placed into a carbon steel plate or stainless steel plate sheath and sealed, vacuum degassing is carried out, the heating temperature of the vacuum degassing is 400-700 ℃, and the vacuum degree is lower than 10^-2Pa, vacuumizing for 2-6 h, and performing hot isostatic pressing treatment on the degassed sheath to obtain a sintered blank; wherein the technological parameters of the hot isostatic pressing operation are as follows: argon is used as a medium, the pressure is 100-200 MPa, the temperature is 1000-1500 ℃, and the holding time is 3-10 h;

step four, heating the sintered blank obtained in the step three to 300-1000 ℃ under the argon protective atmosphere, then carrying out hot rolling and leveling, finally carrying out annealing at the annealing temperature of 800-1300 ℃ for 0.5-2 h, and then naturally cooling to room temperature to obtain a niobium alloy plate blank;

and step five, grinding the niobium alloy plate blank obtained in the step four to obtain the niobium alloy sputtering target material.

In the fourth step, hot rolling is carried out in 3-5 passes, and the rolling deformation of each pass is not lower than 15%.

The niobium alloy sputtering target material is prepared by the preparation method.

Example 1

A preparation method of a niobium alloy sputtering target comprises the following steps:

step one, adding 60 parts by mass and 40 parts by mass of niobium powder and titanium powder into a V-shaped mixer, and adding activated carbon powder accounting for 0.2% of the total weight of the metal powder. The purity of the niobium powder and the titanium powder is not lower than 99.9 percent, and the niobium powder and the titanium powder are sieved by a 200-mesh sieve; the purity of the activated carbon powder is not less than 99.9 percent, and the activated carbon powder is sieved by a 100-mesh sieve. Introducing argon gas as protective gas into the mixer, starting the mixer, mixing the materials for 18 hours, and stopping the mixer to obtain mixed powder;

step two, selecting a rubber sleeve with a proper size as required, filling the mixed powder obtained in the step one into the rubber sleeve, filling while compacting, sealing the rubber sleeve after powder filling is finished, and then shaping the rubber sleeve to keep the rubber sleeve in a cuboid shape; placing the rubber sleeve filled with the powder into a cold isostatic press for pressing, slowly increasing the pressure, keeping the maximum pressure at 200MPa for 5 minutes to obtain a blank, then releasing the pressure, and taking the blank out of the rubber sleeve;

step three, stainless steel sheathing the blank in the step two, heating to 600 ℃, and keeping the vacuum degree lower than 10^-2Pa, vacuumizing for 5 h. Then placing the mixture into a hot isostatic pressing furnace, using argon as a medium, heating to 1100 ℃, keeping the pressure at 150MPa for 5 hours, and then naturally cooling to room temperature to obtain a sintered blank;

step four, putting the sintered blank obtained in the step three into an argon protection heating furnace for heating, wherein the heating temperature is 600 ℃, the heat preservation time is 2 hours, then rolling is carried out, the deformation of the first pass of rolling is not less than 25%, the deformation of the other passes of rolling is not less than 20%, the sintered blank is rolled to the required size through 4 passes of rolling, and then leveling is carried out; and then carrying out vacuum annealing at the annealing temperature of 1000 ℃ for 1 hour to obtain the niobium alloy plate blank.

And step five, performing machining operation on the niobium alloy plate blank obtained in the step four to obtain the niobium alloy sputtering target.

The niobium alloy sputtering target prepared by the embodiment has fine grains, the average grain size is 50 microns, the relative density of the target is not less than 99%, and the purity of the target is not less than 99.9%.

Example 2

A preparation method of a niobium alloy sputtering target comprises the following steps:

step one, adding 70 parts by mass and 30 parts by mass of niobium powder and titanium powder into a V-shaped mixer, and adding activated carbon powder accounting for 0.3% of the total weight of the metal powder. The purity of the niobium powder and the titanium powder is not lower than 99.9 percent, and the niobium powder and the titanium powder are sieved by a 200-mesh sieve; the purity of the activated carbon powder is not less than 99.9 percent, and the activated carbon powder is sieved by a 100-mesh sieve. Introducing argon gas as protective gas into the mixer, starting the mixer, mixing the materials for 18 hours, and stopping the mixer to obtain mixed powder;

step two, selecting a rubber sleeve with a proper size as required, filling the mixed powder obtained in the step one into the rubber sleeve, filling while compacting, sealing the rubber sleeve after powder filling is finished, and then shaping the rubber sleeve to keep the rubber sleeve in a cuboid shape; placing the rubber sleeve filled with the powder into a cold isostatic press for pressing, slowly increasing the pressure, keeping the maximum pressure at 180MPa for 8 minutes to obtain a blank, then releasing the pressure, and taking the blank out of the rubber sleeve;

step three, stainless steel sheathing the blank in the step two, heating to 680 ℃, and keeping the vacuum degree lower than 10^-2Pa, vacuumizing for 4 h. Then placing the mixture into a hot isostatic pressing furnace, using argon as a medium, heating to 1150 ℃, keeping the pressure at 160MPa for 5 hours, and then naturally cooling to room temperature to obtain a sintered blank;

step four, putting the sintered blank obtained in the step three into an argon protection heating furnace for heating, wherein the heating temperature is 650 ℃, the heat preservation time is 2 hours, then rolling is carried out, the deformation of the first pass of rolling is not less than 25%, the deformation of the other passes of rolling is not less than 20%, the sintered blank is rolled to the required size through 4 passes of rolling, and then leveling is carried out; and then carrying out vacuum annealing at the annealing temperature of 1100 ℃ for 1 hour to obtain the niobium alloy plate blank.

And step five, performing machining operation on the niobium alloy plate blank obtained in the step four to obtain the niobium alloy sputtering target.

The niobium alloy sputtering target prepared by the embodiment has fine grains, the average grain size is 60 microns, the relative density of the target is not less than 99%, and the purity of the target is not less than 99.9%.

The foregoing is merely a preferred embodiment of the invention and is not to be construed as limiting the invention in any way. All equivalent changes or modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.