阅读说明：本技术 一种半导体材料的制备方法 (Preparation method of semiconductor material ) 是由 武建军 于 2019-08-21 设计创作，主要内容包括：本发明属于半导体技术领域,尤其是一种半导体材料的制备方法,包括以下步骤：S1：称取6～12g固定氧化锌,放入球磨机中球磨,过65～75目筛,得氧化锌粉末；S2：称取34～58g氮化镓加入到120～140mL质量分数92%硫酸溶液中对其进行搅拌,直至固体溶解得溶解液；S3：将氧化锌粉末加入到溶解液中,搅拌混合40～50min后静置2～4h；S4：将碳化硅的溶液加入到静置后的溶液中,对其进行搅拌10-20min,然后再对其进行静置1-3h,将滤渣过滤取出；本发明操作简单,在制造宽带隙半导体材料时,可以简化制造工序,缩短制造时间,提高了生产效率,具有较强的实用性。(The invention belongs to the technical field of semiconductors, and particularly relates to a preparation method of a semiconductor material, which comprises the following steps: s1: weighing 6-12 g of fixed zinc oxide, putting the fixed zinc oxide into a ball mill for ball milling, and sieving the fixed zinc oxide with a 65-75-mesh sieve to obtain zinc oxide powder; s2: weighing 34-58 g of gallium nitride, adding the gallium nitride into 120-140 mL of sulfuric acid solution with the mass fraction of 92%, and stirring until the solid is dissolved to obtain a dissolved solution; s3: adding zinc oxide powder into the dissolved solution, stirring and mixing for 40-50 min, and standing for 2-4 h; s4: adding the solution of the silicon carbide into the solution after standing, stirring the solution for 10-20min, then standing the solution for 1-3h, and filtering and taking out filter residues; the invention has simple operation, can simplify the manufacturing process, shorten the manufacturing time, improve the production efficiency and has stronger practicability when manufacturing the wide-band-gap semiconductor material.)

1. A preparation method of a semiconductor material comprises the following steps:

S1: weighing 6-12 g of fixed zinc oxide, putting the fixed zinc oxide into a ball mill for ball milling, and sieving the fixed zinc oxide with a 65-75-mesh sieve to obtain zinc oxide powder;

S2: weighing 34-58 g of gallium nitride, adding the gallium nitride into 120-140 mL of sulfuric acid solution with the mass fraction of 92%, and stirring until the solid is dissolved to obtain a dissolved solution;

S3: adding zinc oxide powder into the dissolved solution, stirring and mixing for 40-50 min, and standing for 2-4 h;

S4: adding the solution of the silicon carbide into the solution after standing, stirring the solution for 10-20min, then standing the solution for 1-3h, and filtering and taking out filter residues;

S5: adding filter residues into a sodium nitrate solution with the mass fraction of 45% according to the mass ratio of 3:6, soaking for 1-3h, then carrying out centrifugal separation to obtain a precipitate, washing to be neutral by using deionized water, then placing into an oven, drying for 6-8 h at the temperature of 100-125 ℃ to obtain a dried substance, placing into a muffle furnace preheated to the temperature of 850-950 ℃, and carrying out heat preservation and calcination for 3-5 min to obtain a calcined substance;

S6: respectively weighing 85-98 g of ferric sulfate and 13-18 g of ferric chloride, adding the ferric sulfate and the ferric chloride into 550-570 mL of deionized water, stirring until the solid is dissolved, adjusting the pH to 10 by using 6mol/L sodium hydroxide, adding 3-5 g of the calcined substance after adjustment, putting the calcined substance into a water bath, and stirring and mixing for 30-50 min at the temperature of 45-55 ℃ and the rotating speed of 300-500 r/min;

S7: performing heat preservation crystallization on the dispersed mixed solution at 40-50 ℃ for 3-5 h, performing suction filtration after crystallization to obtain filter residue, washing the filter residue for 3-5 times by using deionized water, then placing the filter residue into an oven, drying the filter residue at 60-80 ℃ for 8-10 h, and performing ball milling after drying until the particle size is 0.5-0.7 mu m to obtain a modified wide band gap;

S8: and adding the materials into a mixer for mixing, adding the materials into a double-screw extruder after mixing for 20-30 min, and extruding and granulating at the extrusion temperature of 168-188 ℃ and the die head temperature of 190-220 ℃ to obtain the wide-bandgap semiconductor material.

2. the method for preparing a semiconductor material according to claim 1, wherein in S1, the grinding time of the fixed zinc oxide in the ball mill is 8-15min, and the grinding loss of the fixed zinc oxide is calculated by weighing the ground powder.

3. the method according to claim 1, wherein in step S2, the solution is left for 3-6min before being stirred, so that the 92% sulfuric acid solution can be fully introduced into the powdered gallium nitride, and the stirring and dissolving time can be shortened.

4. the method according to claim 1, wherein 33 to 45g of the zinc oxide powder is weighed in the solution in S3, and the zinc oxide powder is stirred and mixed until completely dissolved.

5. the method for preparing a semiconductor material according to claim 1, wherein in the step S4, a 55-70 mesh sieve is used for filtering the filter residue.

6. the method for preparing the semiconductor material according to claim 1, wherein in S5, after the filter residue is added into a sodium nitrate solution with a mass fraction of 45% according to a mass ratio of 3:6 and soaked for 1-3 hours, the solution is poured into a centrifugal barrel, then a driving device is used for driving the solution to rotate, and the centrifugal barrel can separate out the precipitate.

7. The method for preparing a semiconductor material according to claim 1, wherein in S6, after stirring, the pH is adjusted to 11.5 by using 1mol/L sodium hydroxide, and after adjustment, ultrasonic dispersion is performed for 6-12 min.

8. The method for preparing a semiconductor material according to claim 1, wherein in S7, the dispersed mixture is crystallized at 45 ℃ for 4 hours, and then filtered to obtain a residue, which is washed with deionized water for 6 times, and then dried in an oven at 85 ℃ for 11 hours, and then ball-milled to a particle size of 0.8 μm to obtain the modified wide band gap.

9. The method for preparing semiconductor material according to claim 1, wherein in S8, the material is mixed in a mixer, and the mixture is mixed for 30min and then fed into a twin-screw extruder for output;

The method of claim 9, wherein in S8, the twin-screw extruder outputs material at 188 ℃ and the die temperature is 220 ℃ for extrusion granulation, so as to obtain the wide band gap semiconductor material.

Technical Field

the invention relates to the technical field of semiconductor materials, in particular to a preparation method of a semiconductor material.

background

Semiconductor materials are a class of electronic materials that have semiconducting properties (electrical conductivity between conductor and insulator, and resistivity in the range of about 1m Ω -cm to 1G Ω -cm) and are useful in the fabrication of semiconductor devices and integrated circuits. Semiconductor materials can be classified by chemical composition, and amorphous and liquid semiconductors with special structures and properties are individually classified into one category. Semiconductor materials can be classified into elemental semiconductors, inorganic compound semiconductors, organic compound semiconductors, and amorphous and liquid semiconductors according to such classification methods.

at room temperature, a wide-bandgap semiconductor has a bandgap of 1.1eV for Si and 1.43eV for GaAs, and a semiconductor material having a bandgap greater than 2.0eV at room temperature is generally classified as a wide-bandgap semiconductor, which is widely used in blue, violet and ultraviolet photoelectronic devices, high-frequency, high-temperature, high-power electronic devices and field emission devices.

Disclosure of Invention

The invention aims to solve the defects of the prior art, and provides a preparation method of a semiconductor material.

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

A preparation method of a semiconductor material comprises the following steps:

s1: weighing 6-12 g of fixed zinc oxide, putting the fixed zinc oxide into a ball mill for ball milling, and sieving the fixed zinc oxide with a 65-75-mesh sieve to obtain zinc oxide powder;

s2: weighing 34-58 g of gallium nitride, adding the gallium nitride into 120-140 mL of sulfuric acid solution with the mass fraction of 92%, and stirring until the solid is dissolved to obtain a dissolved solution;

S3: adding zinc oxide powder into the dissolved solution, stirring and mixing for 40-50 min, and standing for 2-4 h;

S4: adding the solution of the silicon carbide into the solution after standing, stirring the solution for 10-20min, then standing the solution for 1-3h, and filtering and taking out filter residues;

S5: adding filter residues into a sodium nitrate solution with the mass fraction of 45% according to the mass ratio of 3:6, soaking for 1-3h, then carrying out centrifugal separation to obtain a precipitate, washing to be neutral by using deionized water, then placing into an oven, drying for 6-8 h at the temperature of 100-125 ℃ to obtain a dried substance, placing into a muffle furnace preheated to the temperature of 850-950 ℃, and carrying out heat preservation and calcination for 3-5 min to obtain a calcined substance;

S6: respectively weighing 85-98 g of ferric sulfate and 13-18 g of ferric chloride, adding the ferric sulfate and the ferric chloride into 550-570 mL of deionized water, stirring until the solid is dissolved, adjusting the pH to 10 by using 6mol/L sodium hydroxide, adding 3-5 g of the calcined substance after adjustment, putting the calcined substance into a water bath, and stirring and mixing for 30-50 min at the temperature of 45-55 ℃ and the rotating speed of 300-500 r/min;

S7: performing heat preservation crystallization on the dispersed mixed solution at 40-50 ℃ for 3-5 h, performing suction filtration after crystallization to obtain filter residue, washing the filter residue for 3-5 times by using deionized water, then placing the filter residue into an oven, drying the filter residue at 60-80 ℃ for 8-10 h, and performing ball milling after drying until the particle size is 0.5-0.7 mu m to obtain a modified wide band gap;

S8: and adding the materials into a mixer for mixing, adding the materials into a double-screw extruder after mixing for 20-30 min, and extruding and granulating at the extrusion temperature of 168-188 ℃ and the die head temperature of 190-220 ℃ to obtain the wide-bandgap semiconductor material.

Preferably, in S1, the grinding time of the fixed zinc oxide in the ball mill is 8-15min, and the grinding loss of the fixed zinc oxide is calculated by weighing the powder after grinding.

Preferably, in S2, the solution is left standing for 3-6min before being stirred, so that the 92% sulfuric acid solution can fully enter the powdered gallium nitride, and the stirring and dissolving time can be shortened.

Preferably, in S3, 33 to 45g of zinc oxide powder is weighed and put into the solution, and the solution is stirred and mixed until completely dissolved.

preferably, in the step S4, when the filter residue is filtered, a 55-70 mesh sieve is used for filtering.

preferably, in the step S5, after the filter residue is added into a sodium nitrate solution with a mass fraction of 45% according to a mass ratio of 3:6 and soaked for 1-3 hours, the solution is poured into a centrifugal barrel, and then the centrifugal barrel is driven by a driving device to rotate, so that the precipitate can be separated out.

preferably, in S6, after stirring, the pH is adjusted to 11.5 by using 1mol/L sodium hydroxide, and after adjustment, ultrasonic dispersion is carried out for 6-12 min.

preferably, in S7, the dispersed mixture is crystallized at 45 ℃ for 4 hours, and then filtered to obtain a filter residue, which is washed with deionized water for 6 times, and then dried in an oven at 85 ℃ for 11 hours, and finally ball-milled to a particle size of 0.8 μm to obtain the modified wide band gap.

preferably, in the step S8, the materials are added into a mixer to be mixed, and after being mixed for 30min, the mixture is added into a twin-screw extruder to be output.

Preferably, in S8, the wide bandgap semiconductor material is obtained by extruding and granulating the material output by the twin-screw extruder at 188 ℃ and 220 ℃ respectively.

Weighing 6-12 g of fixed zinc oxide, placing the fixed zinc oxide into a ball mill for ball milling, sieving the fixed zinc oxide with a sieve of 65-75 meshes to obtain zinc oxide powder, weighing 34-58 g of gallium nitride, adding the gallium nitride into 120-140 mL of sulfuric acid solution with the mass fraction of 92%, stirring the gallium nitride until the solid is dissolved to obtain a dissolved solution, adding the zinc oxide powder into the dissolved solution, stirring and mixing the zinc oxide powder and the dissolved solution for 40-50 min, standing the mixed solution for 2-4 h, adding a silicon carbide solution into the standing solution, stirring the silicon carbide solution for 10-20min, standing the silicon carbide solution for 1-3h, filtering and taking out filter residues, adding the filter residues into a 45% sodium nitrate solution with the mass fraction of 3:6, soaking the sodium nitrate solution for 1-3h, centrifuging the mixture to obtain precipitates, washing the precipitates with deionized water to be neutral, placing the precipitates into a drying oven, drying the precipitates for 6-8 h at the temperature of 100-125 ℃ to obtain dried products, placing the dried products into, calcining for 3-5 min at a heat preservation condition to obtain a calcined substance, respectively weighing 85-98 g of ferric sulfate and 13-18 g of ferric chloride, adding the weighed ferric sulfate and ferric chloride into 550-570 mL of deionized water, stirring until the solid is dissolved, adjusting the pH value to 10 by using 6mol/L sodium hydroxide, adding 3-5 g of the calcined substance after adjustment, putting the calcined substance into a water bath kettle, stirring and mixing for 30-50 min at the temperature of 45-55 ℃ and the rotating speed of 300-500 r/min, performing heat preservation and crystallization on the dispersed mixed solution for 3-5 h at the temperature of 40-50 ℃, performing suction filtration after crystallization to obtain filter residue, washing for 3-5 times by using the deionized water, putting the filter residue into an oven, drying for 8-10 h at the temperature of 60-80 ℃, performing wide band drying, performing ball milling until the particle size is 0.5-0.7 mu m to obtain a modified gap, adding the material into a mixer, mixing for 20-30 min, adding into a double-screw extruder 188, extruding and granulating at the extrusion temperature of 168-220 ℃, thereby obtaining the wide band gap semiconductor material.

The invention has simple operation, can simplify the manufacturing process, shorten the manufacturing time, improve the production efficiency and has stronger practicability when manufacturing the wide-band-gap semiconductor material.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the methods in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.