Si-doped P-type semiconductor GaSb target material and preparation method thereof

Abstract

The invention discloses a Si-doped P-type semiconductor GaSb target material and a preparation method thereof, the atomic ratio of Ga to Sb in the target material is 1: 1-1.005, and the doping amount of Si is 1-5% of the total mass of the target material. The Si-doped P-type semiconductor GaSb target material can be used for preparing a P-type GaSb thin film through sputtering, the carrier concentration of the P-type GaSb thin film can be improved, the performance of the P-type GaSb thin film is improved, and the preparation process of the P-type GaSb thin film is simplified.

Description

Technical Field

[0001] The present invention belongs to the technical field of alloy targets, and particularly relates to a Si-doped P-type semiconductor GaSb target and a preparation method thereof. Background Art

[0002] As an important III-V group compound semiconductor material, GaSb material is the preferred material for realizing optoelectronic devices in the mid-infrared band. Due to its good performance, GaSb material shows important application prospects in the field of infrared optoelectronics. Gallium antimonide optoelectronic devices are gradually moving towards market application and have become a current development hotspot.

[0003] GaSb thin films in optoelectronic devices mainly include N-type and P-type. P-type GaSb thin films are usually realized by doping element impurities such as Zn, Ga, and Si. Based on the fact that there is no directly element-doped P-type GaSb target on the market, the current preparation method of P-type GaSb thin films is mainly prepared by co-sputtering method, that is, by co-sputtering GaSb target and doping element target to prepare P-type GaSb thin films. However, such a preparation method is relatively complex, and the carrier concentration of the prepared P-type GaSb thin film is relatively low. Summary of the Invention

[0004] Aiming at the above problems, the purpose of the present invention is to provide a Si-doped P-type semiconductor GaSb target and a preparation method thereof.

[0005] In the first aspect, the present invention provides a Si-doped P-type semiconductor GaSb target, wherein the atomic ratio of Ga to Sb is 1:1 to 1.005, and the doping amount of Si is 1% to 5% of the total mass of the target.

[0006] In the second aspect, the present invention provides a preparation method of a Si-doped P-type semiconductor GaSb target, including the following steps: Step (1): Mix Ga and Sb metal raw materials in proportion, and heat them to the melting temperature in an inert atmosphere for melting to obtain an alloy liquid; Step (2): In a mixed atmosphere composed of an inert gas and hydrogen, cool the alloy liquid in step (1) from one end to the first gradient temperature until the alloy liquid is all reduced to the first gradient temperature; then cool the alloy to the second gradient temperature to obtain a GaSb alloy ingot; Step (3): Remove the head and tail of the GaSb alloy ingot, and then perform crushing and ball milling to obtain GaSb alloy powder; Step (4): After pre-treating the Si powder, the treated Si powder is obtained; after mixing the treated Si powder with the GaSb alloy powder in a certain proportion, a mixed powder is obtained; the mixed powder is pressed into an alloy blank, and the alloy blank is subjected to vacuum hot pressing sintering to obtain a Si-doped P-type semiconductor GaSb target.

[0007] Preferably, in the step (1), the melting temperature is 750~850 °C, and the melting holding time is 240~360 min.

[0008] Preferably, in the step (2), the volume ratio of the inert gas to the hydrogen gas is 1:(3~5).

[0009] Preferably, in the step (2), the first gradient temperature is 600~650 °C; the second gradient temperature is 15~35 °C.

[0010] Preferably, in the step (3), the specific steps of crushing and ball milling are as follows: the GaSb alloy ingot is crushed to 1~2 mm, and then added to a vacuum ball milling tank for vacuum ball milling to obtain GaSb alloy powder.

[0011] More preferably, the vacuum degree of the ball milling is 1~10 Pa, the rotation speed of the ball milling is 200~300 r / min, the ball milling time is 0.5~2 h, the diameter of the grinding balls is 2~5 mm, and the mass ratio of the material to the grinding balls is (2~5):1.

[0012] Preferably, in the step (4), the specific steps of the pre-treatment are as follows: the Si powder is added to a mixed acid solution, heated and ultrasonically treated, filtered and dried to obtain the treated Si powder.

[0013] More preferably, the mixed acid is composed of sulfuric acid and hydrochloric acid, and the volume ratio of sulfuric acid to hydrochloric acid is (1~2):(1~2); the heating temperature is 40~60 °C, and the ultrasonic treatment time is 20~40 min.

[0014] Preferably, the mixing is carried out by a vacuum double-motion mixer, wherein: during mixing, the rotation speed of the material barrel is 25~30 r / min; the rotation speed of the spiral blade is 50~70 r / min, the homogenization time is 30~60 min, and the vacuum degree is 1~10 Pa.

[0015] Preferably, in the step (4), the specific steps of pressing into an alloy blank are as follows: the mixed powder is placed in a mold, pressed for 3~5 min under a pre-pressing pressure of 5~10 MPa, and the pressure is released to obtain an alloy blank.

[0016] Preferably, in the step (3), the specific steps of vacuum pressure sintering are as follows: Place the alloy blank in a vacuum sintering furnace. When the vacuum is pumped to a vacuum degree of 5-10 Pa, start heating, and heat it up to 650-700 °C at a rate of 5-10 °C / min, and keep it warm for 30-80 min; then pressurize it to 40-45 MPa, keep the pressure and temperature for 60-90 min, and then slowly reduce the pressure to 8-12 MPa, and cool it with the furnace to obtain an Si-doped P-type semiconductor GaSb target.

[0017] Compared with the prior art, one or more of the above technical solutions can achieve at least one of the following beneficial effects: (1) In the present invention, the Si-doped P-type semiconductor GaSb target can be used to prepare a P-type GaSb thin film by sputtering, and can increase the carrier concentration of the P-type GaSb thin film, improve the performance of the P-type GaSb thin film, and simplify the preparation process of the P-type GaSb thin film.

[0018] (2) In the preparation process of the GaSb alloy ingot in the present invention, the alloy liquid is cooled starting from one end, realizing the directional solidification of the alloy liquid. The directional solidification method can make the impurities in the GaSb alloy ingot relatively concentrated at both ends. Therefore, after removing the head and tail, it can play a role in purifying the alloy ingot.

[0019] (3) The preparation method of the Si-doped P-type semiconductor GaSb target in the present invention does not require vacuum encapsulation, so the consumables can be reused, reducing the production cost of the target. Detailed implementation manners

[0020] As described above, on the first hand, the present invention provides an Si-doped P-type semiconductor GaSb target, wherein the atomic ratio of Ga to Sb is 1:1-1.005, and the Si doping amount is 1-5% of the total mass of the target, including but not limited to 1%, 1.5%, 2.0%, 2.5%, 3.0%, 3.5%, 4.0%, 4.5%, 5.0%, etc.

[0021] In the present invention, a P-type GaSb target is prepared by directly doping Si element into the GaSb target, filling the blank of the prior art. In addition, doping Si element into the GaSb target can simplify the preparation process of the P-type GaSb thin film, increase the carrier concentration in the P-type GaSb thin film, and improve the performance of the P-type GaSb thin film.

[0022] On the second hand, the present invention provides a preparation method of an Si-doped P-type semiconductor GaSb target, including the following steps: Step (1): Mix Ga and Sb metal raw materials in proportion, and heat them to the melting temperature in an inert atmosphere for melting to obtain an alloy liquid; Step (2): Under a mixed atmosphere composed of an inert gas and hydrogen, cool the alloy liquid in step (1) from one end to the first gradient temperature until the entire alloy liquid is reduced to the first gradient temperature; then cool the alloy liquid to the second gradient temperature to obtain a GaSb alloy ingot. Step (3): Remove the head and tail of the GaSb alloy ingot, and then perform crushing and ball milling to obtain GaSb alloy powder. Step (4): After pre-treating the Si powder, obtain the treated Si powder; mix the treated Si powder and the GaSb alloy powder in a certain proportion to obtain a mixed powder; press the mixed powder into an alloy green body, and perform vacuum hot pressing sintering on the alloy green body to obtain an Si-doped P-type semiconductor GaSb target.

[0023] In the melting process of the GaSb alloy in the present invention, heating and melting are carried out under an inert atmosphere; generally, it can be directly carried out in a tube furnace. Put the prepared Ga and Sb into a quartz crucible, place the quartz crucible in the tube furnace, then cover it with a quartz tail cap, and introduce an inert gas to remove the air in the quartz tube to form an inert gas environment, and then heating and melting can be carried out. Moreover, during cooling in the present invention, the directional solidification technology is adopted, and the temperature is lowered from one end of the alloy liquid. Therefore, a conventional tube furnace with a multi-temperature zone controller can be used. By controlling the temperature drop of each temperature zone of the tube furnace through the multi-temperature zone controller, the alloy liquid is directionally solidified, realizing the enrichment of impurities at both ends of the alloy ingot. Thus, after removing the head and tail, the purification of the alloy ingot can be achieved. Therefore, in the method of the present invention, not only is there no need for vacuum encapsulation, the consumables can be reused, saving costs; but also there is no need to take out at high temperature, which can reduce the risk factor.

[0024] Preferably, in step (1), the melting temperature is 750 - 850 °C, including but not limited to 750 °C, 760 °C, 770 °C, 780 °C, 790 °C, 800 °C, 810 °C, 820 °C, 830 °C, 840 °C, 850 °C, etc.; the melting holding time is 240 - 360 min, including but not limited to 240 min, 250 min, 260 min, 270 min, 280 min, 290 min, 300 min, 310 min, 320 min, 330 min, 340 min, 350 min, 360 min, etc.

[0025] Preferably, in step (2), the volume ratio of the inert gas to hydrogen is 1:(3 - 5), including but not limited to 1:3, 1:3.5, 1:4, 1:4.5, 1:5, etc.

[0026] Preferably, in the step (2), the first gradient temperature is 600 - 650 °C, including but not limited to 600 °C, 610 °C, 620 °C, 630 °C, 640 °C, 650 °C, etc.; the second gradient temperature is 15 - 35 °C, including but not limited to 15 °C, 18 °C, 20 °C, 22 °C, 25 °C, 28 °C, 30 °C, 32 °C, 35 °C, etc.

[0027] In the method of the present invention, the first gradient temperature is below the melting point of the alloy. The molten metal will gradually solidify from one end to form an alloy. During the progressive directional solidification process, impurities will accumulate at both ends, thus playing a role in purification.

[0028] Preferably, in the step (3), the specific steps of crushing and ball milling are as follows: the GaSb alloy ingot is crushed to 1 - 2 mm, and then added to a vacuum ball milling tank for vacuum ball milling to obtain GaSb alloy powder.

[0029] More preferably, the vacuum degree of the ball milling is 1 - 10 Pa, including but not limited to 1 Pa, 2 Pa, 3 Pa, 4 Pa, 5 Pa, 6 Pa, 7 Pa, 8 Pa, 9 Pa, 10 Pa, etc.; the rotation speed of the ball milling is 200 - 300 r / min, including but not limited to 200 r / min, 210 r / min, 220 r / min, 230 r / min, 240 r / min, 250 r / min, 260 r / min, 270 r / min, 280 r / min, 290 r / min, 300 r / min, etc.; the ball milling time is 0.5 - 2 h, including but not limited to 0.5 h, 0.75 h, 1 h, 1.25 h, 1.5 h, 1.75 h, 2.0 h, etc.; the diameter of the grinding balls is 2 - 5 mm, including but not limited to 2 mm, 3 mm, 4 mm, 5 mm, etc.; the mass ratio of the material to the grinding balls is (2 - 5):1, including but not limited to 2:1, 3:1, 4:1, 5:1, etc.

[0030] Preferably, in the step (4), the specific steps of the pretreatment are as follows: Si powder is added to a mixed acid solution, heated and ultrasonically treated, filtered and dried to obtain the pretreated Si powder.

[0031] In the present invention, acid treatment of Si powder can remove impurities in the Si powder and improve the purity of the target; moreover, after pretreatment, the affinity between the Si powder and the GaSb alloy powder can be increased, and the mixing uniformity of the two can be improved.

[0032] Further preferably, the mixed acid is composed of sulfuric acid and hydrochloric acid, and the volume ratio of sulfuric acid to hydrochloric acid is (1-2):(1-2), including but not limited to 1:1, 1.5:1, 2:1, 1:1.5, 1:2, etc.; the heating temperature is 40-60°C, including but not limited to 40°C, 42°C, 45°C, 48°C, 50°C, 52°C, 55°C, 58°C, 60°C, etc.; the ultrasonic treatment time is 20-40 min, including but not limited to 20 min, 25 min, 30 min, 35 min, 40 min, etc.

[0033] Preferably, the mixing is carried out by a vacuum double-motion mixer, wherein: during mixing, the rotation speed of the material barrel is 25-30 r / min, including but not limited to 25 r / min, 26 r / min, 27 r / min, 28 r / min, 29 r / min, 30 r / min, etc.; the rotation speed of the spiral blade is 50-70 r / min, including but not limited to 50 r / min, 55 r / min, 60 r / min, 65 r / min, 70 r / min, etc.; the homogenization time is 30-60 min, including but not limited to 30 min, 35 min, 40 min, 45 min, 50 min, 55 min, 60 min, etc.; the vacuum degree is 1-10 Pa, including but not limited to 1 Pa, 2 Pa, 3 Pa, 4 Pa, 5 Pa, 6 Pa, 7 Pa, 8 Pa, 9 Pa, 10 Pa, etc.

[0034] In the present invention, vacuum double-motion homogenization mixing is adopted, which can improve the mixing uniformity of the pretreated Si powder and GaSb alloy powder, thereby enhancing the uniformity of the target.

[0035] Preferably, in the step (4), the specific steps of pressing into an alloy blank are: placing the mixed powder in a mold, pressing for 3-5 min under a pre-pressing pressure of 5-10 MPa, and then releasing the pressure to obtain the alloy blank.

[0036] Preferably, in the step (3), the specific steps of vacuum pressure sintering are: placing the alloy blank in a vacuum sintering furnace, evacuating to a vacuum degree of 5-10 Pa, then starting to heat, heating to 650-700°C at a rate of 5-10°C / min, and holding for 30-80 min; then pressurizing to 40-45 MPa, holding the pressure for 60-90 min, and then slowly reducing the pressure to 8-12 MPa, and cooling with the furnace to obtain the Si-doped P-type semiconductor GaSb target.

[0037] In the present invention, the vacuum pressure sintering method can improve the density of the target.

[0038] For the convenience of understanding the present invention, the following will describe the present invention in a more comprehensive and detailed manner with preferred embodiments, but the protection scope of the present invention is not limited to the following specific embodiments.

[0039] Example 1 In this example, the atomic ratio of Ga to Sb in the Si-doped P-type semiconductor GaSb target is 1:1.003, and the doping amount of Si is 1% of the total mass of the target raw materials. The specific preparation method is as follows: (1) Select Ga and Sb particles with a purity of 5N or above as raw materials, and perform raw material batching according to 1:1.003, with Sb slightly in excess. Put the prepared materials into a quartz crucible, place the quartz crucible in a multi-temperature zone tube furnace, cover it with a quartz tail cap, and introduce nitrogen at a speed of 2 L / min to remove the air in the quartz tube. Then control the heater to raise the temperature of the temperature zone where the quartz crucible is located to 780 °C and keep it warm for 300 min to melt and react antimony and gallium to obtain an alloy liquid.

[0040] (2) Continuously introduce a mixed gas composed of nitrogen and hydrogen into the multi-temperature zone tube furnace, where the volume ratio of nitrogen to hydrogen is 1:3. Then control the heater to start cooling from one end of the quartz crucible to 650 °C (the specific steps are: gradually control the temperature of each temperature zone from left to right to drop to 650 °C, that is, first reduce the temperature of the leftmost first temperature zone to 650 °C, and then control the temperature of the second temperature zone on the left to drop to 650 °C, and so on until the temperatures of all temperature zones drop to 650 °C and solidify into an alloy). Then cool the alloy in the quartz crucible to room temperature to obtain a GaSb alloy ingot, and cut off the head and tail of the GaSb alloy ingot for purification (about 10 mm at the head and tail are cut off).

[0041] (3) Hammer the purified GaSb alloy ingot into particles with a size of 1-2 mm using a tungsten carbide hammer. Then put the alloy particles into a vacuum ball milling tank, seal it after charging according to a material ratio of 2:1, and perform ball milling to make powder. After ball milling, pass through a 325-mesh stainless steel sieve to obtain GaSb alloy powder with a D50 particle size of about 15 microns. Among them: the vacuum degree of ball milling is 10 Pa, the rotation speed of ball milling is 200 r / min, the ball milling time is 2 h, the diameter of the grinding balls is 2.0 mm, and the grinding balls are zirconia balls.

[0042] (4) Add Si powder to a mixed acid composed of sulfuric acid and hydrochloric acid with a volume ratio of 1:1, heat to 50 °C, perform ultrasonic treatment for 30 min, then filter and wash with ultrapure water, and vacuum dry at 90 °C for 5 h to obtain pretreated Si powder.

[0043] (5) Add the GaSb alloy powder and the pretreated Si powder to a vacuum double-motion mixer for homogeneous mixing for 45 min to obtain a mixed powder. Among them, the mass of Si powder accounts for 1% of the total mass of the mixed powder, the rotation speed of the material barrel is 28 r / min, the rotation speed of the internal spiral blade is 60 r / min, and the vacuum degree is 10 Pa.

[0044] (6) Put the mixed powder into a clean graphite mold. First, increase the pressure to 7.5 MPa at a pressure increase rate of 2 T / min for pre-pressing to remove the air in the graphite mold. After maintaining the pressure for 3 min, release the pressure to obtain an alloy billet. Place the alloy billet in a sintering furnace, close the furnace door, evacuate to a vacuum degree of 10 Pa in the furnace chamber, then start heating, increase the temperature to 650 °C at a rate of 5 °C / min, hold for 70 min, then apply pressure to 45 MPa at this temperature, and then hold the pressure for 80 min. After the holding of pressure is completed, slowly reduce the pressure to 10 MPa and cool with the furnace. After demolding, a Si-doped P-type semiconductor GaSb target is obtained.

[0045] Example 2 It is basically the same as Example 1, except that the mass of Si is 3% of the total mass of the target material raw materials.

[0046] Example 3 It is basically the same as Example 1, except that the mass of Si is 5% of the total mass of the target material raw materials.

[0047] Example 4 In this example, the atomic ratio of Ga to Sb in the Si-doped P-type semiconductor GaSb target is 1:1.005, and the doping amount of Si is 3% of the total mass of the target material raw materials. The specific preparation method is as follows: (1) Select Ga and Sb particles with a purity of 5N or above as raw materials, and perform raw material batching according to 1:1.005, with Sb slightly in excess. Put the prepared materials into a quartz crucible, place the quartz crucible in a multi-temperature zone tube furnace, cover it with a quartz tail cap, and introduce nitrogen at a speed of 3 L / min to remove the air in the quartz tube. Then control the heater to raise the temperature of the temperature zone where the quartz crucible is located to 750 °C and hold for 360 min to make the antimony and gallium melt and react to obtain an alloy liquid.

[0048] (2) Continuously introduce a mixed gas composed of nitrogen and hydrogen into the multi-temperature zone tube furnace, where the volume ratio of nitrogen to hydrogen is 1:4. Then control the heater to start cooling from one end of the quartz crucible, cool down to 600 °C (the specific steps are: gradually control the temperature of each temperature zone from left to right to drop to 600 °C, that is, first reduce the temperature of the leftmost first temperature zone to 600 °C, then control the temperature of the second temperature zone from the left to drop to 600 °C, and so on until the temperatures of all temperature zones drop to 600 °C and solidify into an alloy). Then cool the alloy in the quartz crucible to room temperature to obtain a GaSb alloy ingot, and cut off the head and tail of the GaSb alloy ingot for purification (about 12 mm of the head and tail are cut off).

[0049] (3) Hammer the purified GaSb alloy ingot into particles of 1 - 2 mm with a tungsten carbide hammer. Then, put the alloy particles into a vacuum ball milling tank. After feeding according to a material ratio of 3:1, seal it and conduct ball milling for powder making. After ball milling, pass through a 325 - mesh stainless - steel sieve to obtain GaSb alloy powder with a particle size D50 of about 10 microns. Among them: the vacuum degree of ball milling is 5 Pa, the rotation speed of ball milling is 250 r / min, the ball milling time is 1.5 h, the diameter of the grinding balls is 1.5 mm, and the grinding balls are zirconia balls.

[0050] (4) Add Si powder to a mixed acid composed of sulfuric acid and hydrochloric acid with a volume ratio of 1:1, heat it to 60 °C, perform ultrasonic treatment for 20 min, then filter and wash with ultrapure water, and vacuum - dry at 80 °C for 6 h to obtain pretreated Si powder.

[0051] (5) Add GaSb alloy powder and pretreated Si powder to a vacuum double - motion mixer for homogeneous mixing for 60 min to obtain mixed powder. Among them, the mass of Si powder accounts for 3% of the total mass of the mixed powder, the rotation speed of the material barrel is 30 r / min, the rotation speed of the internal spiral blade is 70 r / min, and the vacuum degree is 5 Pa.

[0052] (6) Put the mixed powder into a clean graphite mold. First, increase the pressure to 10 MPa at a pressure - rising rate of 2 T / min to remove the air in the graphite mold, then keep the pressure for 4 min and then relieve the pressure to obtain an alloy billet. Place the alloy billet in a sintering furnace, close the furnace door, evacuate to a vacuum degree of 5 Pa in the furnace chamber, then start heating, raise the temperature to 680 °C at a rate of 10 °C / min, hold for 60 min, then pressurize to 45 MPa at this temperature, and then hold the pressure for 70 min. After the holding of pressure is completed, slowly reduce the pressure to 10 MPa and cool with the furnace. After demolding, obtain an Si - doped P - type semiconductor GaSb target.

[0053] Example 5 In the Si - doped P - type semiconductor GaSb target of this example, the atomic ratio of Ga to Sb is 1:1.002, and the doping amount of Si is 3% of the total mass of the target materials. The specific preparation method is as follows: (1) Select Ga and Sb particles with a purity of 5N or above as raw materials, conduct raw material batching according to 1:1.002, with Sb slightly in excess. Put the prepared materials into a quartz crucible, place the quartz crucible in a multi - temperature - zone tube furnace, then cover it with a quartz tail cap, and introduce nitrogen at a speed of 3 L / min to remove the air in the quartz tube. Then, control the heater to raise the temperature of the temperature zone where the quartz crucible is located to 850 °C and hold for 240 min to make the antimony and gallium melt and react to obtain an alloy liquid.

[0054] (2) Continuously introduce a mixed gas composed of nitrogen and hydrogen into the multi-temperature zone tube furnace, where the volume ratio of nitrogen to hydrogen is 1:3; then control the heater to start cooling from one end of the quartz crucible, cooling down to 630 °C (the specific steps are: gradually control the temperature of each temperature zone to drop to 630 °C from left to right, that is, first lower the temperature of the leftmost first temperature zone to 630 °C, then control the temperature of the second temperature zone from the left to drop to 630 °C, and cool down in turn until the temperatures of all temperature zones drop to 630 °C and solidify into an alloy), and then cool the alloy in the quartz crucible to room temperature to obtain a GaSb alloy ingot. Cut off the head and tail of the GaSb alloy ingot for purification (about 12 mm of the head and tail are cut off).

[0055] (3) Use a tungsten carbide hammer to knock the purified GaSb alloy ingot into particles with a size of 1 - 2 mm. Then put the alloy particles into a vacuum ball milling tank. After feeding according to a material ratio of 2:1, seal it and carry out ball milling to make powder. After ball milling, pass through a 325-mesh stainless steel sieve to obtain GaSb alloy powder with a particle size D50 of about 10 microns; among them: the vacuum degree of ball milling is 1 Pa, the rotation speed of ball milling is 300 r / min, the ball milling time is 0.5 h, the diameter of the grinding balls is 2.0 mm, and the grinding balls are zirconia balls.

[0056] (4) Add Si powder to a mixed acid composed of sulfuric acid and hydrochloric acid with a volume ratio of 1:1, heat to 60 °C, perform ultrasonic treatment for 20 min, then after filtration and washing with ultrapure water, carry out vacuum drying at 80 °C for 6 h to obtain pretreated Si powder.

[0057] (5) Add GaSb alloy powder and pretreated Si powder to a vacuum double-motion mixer for homogeneous mixing for 60 min to obtain a mixed powder; among them, the mass of Si powder accounts for 3% of the total mass of the mixed powder, the rotation speed of the material barrel is 30 r / min, the rotation speed of the internal spiral blade is 70 r / min, and the vacuum degree is 5 Pa.

[0058] (6) Put the mixed powder into a clean graphite mold. First, increase the pressure to 5 MPa at a rate of 2 T / min for pre-pressing to remove the air in the graphite mold. After maintaining this pressure for 3 min, release the pressure to obtain an alloy billet. Place the alloy billet in a sintering furnace, close the furnace door, evacuate to a vacuum degree of 10 Pa in the furnace chamber, then start heating, increase the temperature to 700 °C at a rate of 10 °C / min, hold for 60 min, then apply pressure to 45 MPa at this temperature, and then hold the pressure for 60 min. After the pressure holding ends, slowly reduce the pressure to 12 MPa and cool with the furnace. After demolding, obtain an Si-doped P-type semiconductor GaSb target.

[0059] The density, composition, and carrier concentration of the Si-doped p-type semiconductor GaSb targets prepared in Examples 1 to 5 were detected. The test results are shown in Table 1, and the specific detection methods are as follows.

[0060] For density detection, the Archimedes principle was specifically used for detection.

[0061] For composition detection, an ICP-OES instrument (fully named inductively coupled plasma-optical emission spectroscopy, referring to an inductively coupled plasma emission spectrometer) was used for testing.

[0062] For carrier concentration detection, a Hall tester (hall9900) was used for testing.

[0063] Table 1 Note: The increase in carrier concentration in Table 1 refers to the increase in the carrier concentration of the Si-doped p-type semiconductor GaSb target in the example compared to the GaSb target.

[0064] As can be seen from Table 1, the densities of the Si-doped p-type semiconductor GaSb targets prepared in Examples 1 to 5 all reached over 97%, and their carrier concentrations increased by over 22% compared to the undoped GaSb targets. From the data in Examples 1 to 3, it can be seen that when the Si doping amount was 3%, the increase rate of the carrier concentration was the largest.

[0065] The above are only the preferred embodiments of the present invention. It should be noted that for those of ordinary skill in the art, without departing from the principle of the present invention, several improvements and refinements can be made, and these improvements and refinements should also be regarded as the protection scope of the present invention.

Claims

1. A Si-doped P-type semiconductor GaSb target, characterized in that, The atomic ratio of Ga to Sb in the target material is 1:1 to 1.005, and the doping amount of Si is 1 to 5% of the total mass of the target material.

2. A method for preparing an Si-doped P-type semiconductor GaSb target according to claim 1, characterized in that, It includes the following steps: Step (1): After mixing Ga and Sb metal raw materials in proportion, heat them to the melting temperature in an inert atmosphere for melting to obtain an alloy liquid. Step (2): In a mixed atmosphere composed of an inert gas and hydrogen, cool the alloy liquid in step (1) from one end to the first gradient temperature until the alloy liquid is completely cooled to the first gradient temperature; then cool the alloy to the second gradient temperature to obtain a GaSb alloy ingot. Step (3): Remove the head and tail of the GaSb alloy ingot, and then perform crushing and ball milling to obtain GaSb alloy powder. Step (4): After pre-treating Si powder, obtain the treated Si powder; mix the treated Si powder and GaSb alloy powder in proportion to obtain a mixed powder; press the mixed powder into an alloy green body, and perform vacuum hot pressing sintering on the alloy green body to obtain an Si-doped P-type semiconductor GaSb target material.

3. The preparation method of the Si-doped P-type semiconductor GaSb target according to claim 2, characterized in that, In step (1), the melting temperature is 750 - 850 °C, and the melting holding time is 240 - 360 min.

4. The preparation method of the Si-doped P-type semiconductor GaSb target according to claim 2, characterized in that, In step (2), the volume ratio of the inert gas to hydrogen is 1:(3 - 5); the first gradient temperature is 600 - 650 °C; the second gradient temperature is 15 - 35 °C.

5. The preparation method of the Si-doped P-type semiconductor GaSb target according to claim 2, wherein, In step (3), the specific steps of crushing and ball milling are: crush the GaSb alloy ingot to 1 - 2 mm, and then add it to a vacuum ball milling tank for vacuum ball milling to obtain GaSb alloy powder.

6. The preparation method of the Si-doped P-type semiconductor GaSb target according to claim 5, characterized in that, The vacuum degree of the ball milling is 1 - 10 Pa, the rotation speed of the ball milling is 200 - 300 r / min, the ball milling time is 0.5 - 2 h, the diameter of the grinding balls is 2 - 5 mm, and the mass ratio of the material to the grinding balls is (2 - 5):

1.

7. The preparation method of the Si-doped P-type semiconductor GaSb target according to claim 2, characterized in that, In step (4), the specific steps of the pre-treatment are: add Si powder to a mixed acid solution, perform heating and ultrasonic treatment, filter and dry to obtain the treated Si powder.

8. The preparation method of the Si-doped P-type semiconductor GaSb target according to claim 2, wherein The mixing is carried out using a vacuum double-motion mixer, where: during mixing, the rotation speed of the material barrel is 25 - 30 r / min; the rotation speed of the spiral blade is 50 - 70 r / min, the homogenization time is 30 - 60 min, and the vacuum degree is 1 - 10 Pa.

9. The preparation method of the Si-doped P-type semiconductor GaSb target according to claim 2, characterized in that, In step (4), the specific steps of pressing into an alloy green body are: place the mixed powder in a mold, press it for 3 - 5 min under a pre-pressing pressure of 5 - 10 MPa, relieve the pressure to obtain an alloy green body.

10. The preparation method of the Si-doped P-type semiconductor GaSb target according to claim 2, wherein, In step (4), the specific steps of vacuum pressure sintering are: place the alloy green body in a vacuum sintering furnace, evacuate to a vacuum degree in the furnace chamber reaching 5 - 10 Pa, start heating, heat up to 650 - 700 °C at a rate of 5 - 10 °C / min, and hold for 30 - 80 min; then pressurize to 40 - 45 MPa, hold the pressure for 60 - 90 min, and then slowly reduce the pressure to 8 - 12 MPa, and cool with the furnace to obtain an Si-doped P-type semiconductor GaSb target material.

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