CN110544721A - Preparation method of semiconductor material - Google Patents
Preparation method of semiconductor material Download PDFInfo
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- CN110544721A CN110544721A CN201910771575.6A CN201910771575A CN110544721A CN 110544721 A CN110544721 A CN 110544721A CN 201910771575 A CN201910771575 A CN 201910771575A CN 110544721 A CN110544721 A CN 110544721A
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- 239000000463 material Substances 0.000 title claims abstract description 55
- 239000004065 semiconductor Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 86
- 238000003756 stirring Methods 0.000 claims abstract description 46
- 239000011787 zinc oxide Substances 0.000 claims abstract description 31
- 238000002156 mixing Methods 0.000 claims abstract description 27
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910002601 GaN Inorganic materials 0.000 claims abstract description 23
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000005303 weighing Methods 0.000 claims abstract description 23
- 238000000498 ball milling Methods 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 12
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 9
- 238000007873 sieving Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 79
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 23
- 229910021641 deionized water Inorganic materials 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 22
- 239000000126 substance Substances 0.000 claims description 21
- 239000002244 precipitate Substances 0.000 claims description 14
- 238000002425 crystallisation Methods 0.000 claims description 12
- 230000008025 crystallization Effects 0.000 claims description 12
- 238000004321 preservation Methods 0.000 claims description 12
- 235000010344 sodium nitrate Nutrition 0.000 claims description 12
- 239000004317 sodium nitrate Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 238000001125 extrusion Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 9
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 9
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 9
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 239000007788 liquid Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
Abstract
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.
Description
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.
Example one
a preparation method of a semiconductor material comprises the following steps:
S1: weighing 6g 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-mesh sieve to obtain zinc oxide powder;
S2: weighing 34g of gallium nitride, adding the gallium nitride into 120mL of sulfuric acid solution with the mass fraction of 92%, and stirring the gallium nitride until the solid is dissolved to obtain a dissolved solution;
S3: adding zinc oxide powder into the dissolved solution, stirring and mixing for 40min, and standing for 2 h;
S4: adding the solution of the silicon carbide into the solution after standing, stirring the solution for 10min, then standing the solution for 1h, 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 3:4, soaking for 1h, then carrying out centrifugal separation to obtain a precipitate, washing to be neutral by using deionized water, then placing into a drying oven, drying for 6h at the temperature of 100 ℃ to obtain a dried substance, placing into a muffle furnace preheated to the temperature of 850 ℃, and carrying out heat preservation and calcination for 3min to obtain a calcined substance;
s6: respectively weighing 85g of ferric sulfate and 13g of ferric chloride, adding into 550mL of deionized water, stirring until the solid is dissolved, adjusting the pH to 10 by using 6mol/L sodium hydroxide, adding 3g of the calcined substance after adjustment, putting into a water bath, and stirring and mixing for 30min at 45 ℃ and 300 r/min;
s7: performing heat preservation and crystallization on the dispersed mixed solution at 40 ℃ for 3h, performing suction filtration after crystallization to obtain filter residue, washing the filter residue for 3 times by using deionized water, putting the filter residue into an oven, drying the filter residue at 60 ℃ for 8h, and performing ball milling after drying until the particle size is 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 20min, and extruding and granulating under the conditions that the extrusion temperature is 168 ℃ and the die head temperature is 190 ℃ to obtain the wide-band-gap semiconductor material.
in this example, in S1, the grinding time of fixed zinc oxide in the ball mill was 8min, and the amount of grinding loss of the fixed zinc oxide was calculated by weighing the powder after grinding.
In this embodiment, in S2, the solution is left standing for 3min 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.
in this example, 33g of zinc oxide powder was weighed in S3 and put into the solution, followed by stirring and mixing until the zinc oxide powder was completely dissolved.
in this example, in S4, a 55-mesh sieve was used for filtration of the residue.
In this embodiment, in S5, after the filter residue is added to a 45% sodium nitrate solution by mass ratio of 3:6 and soaked for 1 hour, the solution is poured into a centrifuge bucket, and then the centrifuge bucket is driven by a driving device to rotate, so that the precipitate can be separated out.
In this example, in S6, pH was adjusted to 11.5 with 1mol/L NaOH after stirring, and ultrasonic dispersion was performed for 6min after adjustment.
In this embodiment, 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 then ball-milled to a particle size of 0.8 μm, thereby obtaining a modified wide band gap.
In this example, in S8, the materials were mixed in a blender, mixed for 30min, and then fed into a twin-screw extruder for output.
In this example, in S8, the wide bandgap semiconductor material was obtained by extrusion granulation at a material temperature of 188 ℃ and a die temperature of 220 ℃ from a twin-screw extruder.
example two
A preparation method of a semiconductor material comprises the following steps:
s1: weighing 10g of fixed zinc oxide, putting the fixed zinc oxide into a ball mill for ball milling, and sieving the fixed zinc oxide with a 70-mesh sieve to obtain zinc oxide powder;
S2: weighing 45g of gallium nitride, adding the gallium nitride into 130mL of sulfuric acid solution with the mass fraction of 92%, and stirring the gallium nitride until the solid is dissolved to obtain a dissolved solution;
s3: adding zinc oxide powder into the dissolved solution, stirring and mixing for 45min, and standing for 3 h;
S4: adding the solution of the silicon carbide into the solution after standing, stirring the solution for 15min, then standing the solution for 2h, 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 3:5, soaking for 2 hours, then carrying out centrifugal separation to obtain a precipitate, washing to be neutral by using deionized water, then placing into a drying oven, drying for 7 hours at the temperature of 115 ℃ to obtain a dried substance, placing into a muffle furnace preheated to the temperature of 900 ℃, and carrying out heat preservation and calcination for 4 minutes to obtain a calcined substance;
S6: respectively weighing 90g of ferric sulfate and 15g of ferric chloride, adding into 560mL of deionized water, stirring until the solid is dissolved, adjusting the pH to 10 by using 6mol/L sodium hydroxide, adding 4g of the calcined substance after adjustment, putting into a water bath, and stirring and mixing for 40min at 50 ℃ and 400 r/min;
S7: performing heat preservation and crystallization on the dispersed mixed solution at 45 ℃ for 4h, performing suction filtration after crystallization to obtain filter residue, washing the filter residue with deionized water for 4 times, putting the filter residue into an oven, drying the filter residue at 70 ℃ for 9h, and performing ball milling after drying until the particle size is 0.6 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 25min, and extruding and granulating under the conditions that the extrusion temperature is 175 ℃ and the die head temperature is 210 ℃ to obtain the wide-band-gap semiconductor material.
in this example, in S1, the fixed zinc oxide was ground in a ball mill for 12min, and the ground powder was weighed to calculate the grinding loss of the fixed zinc oxide.
In this embodiment, in S2, the solution is left standing for 4min 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.
in this example, 40g of zinc oxide powder was weighed in S3 and put into the solution, followed by stirring and mixing until the zinc oxide powder was completely dissolved.
In this example, in S4, a 65-mesh sieve was used for filtration of the residue.
In this embodiment, in S5, after the filter residue is added to a 45% sodium nitrate solution by mass ratio of 3:5 and soaked for 2 hours, the solution is poured into a centrifuge bucket, and then the centrifuge bucket is driven by a driving device to rotate, so that the precipitate can be separated out.
in this example, in S6, pH was adjusted to 11.5 with 1mol/L NaOH after stirring, and ultrasonic dispersion was carried out for 10min after adjustment.
In this embodiment, 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 then ball-milled to a particle size of 0.8 μm, thereby obtaining a modified wide band gap.
in this example, in S8, the materials were mixed in a blender, mixed for 30min, and then fed into a twin-screw extruder for output.
in this example, in S8, the wide bandgap semiconductor material was obtained by extrusion granulation at a material temperature of 188 ℃ and a die temperature of 220 ℃ from a twin-screw extruder.
EXAMPLE III
A preparation method of a semiconductor material comprises the following steps:
S1: weighing 12g of fixed zinc oxide, putting the fixed zinc oxide into a ball mill for ball milling, and sieving the fixed zinc oxide with a 75-mesh sieve to obtain zinc oxide powder;
s2: weighing 58g of gallium nitride, adding the gallium nitride into 140mL of sulfuric acid solution with the mass fraction of 92%, and stirring the gallium nitride until the solid is dissolved to obtain a dissolved solution;
s3: adding zinc oxide powder into the dissolved solution, stirring and mixing for 50min, and standing for 4 h;
s4: adding the solution of the silicon carbide into the solution after standing, stirring the solution for 20min, then standing the solution for 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 3 hours, then carrying out centrifugal separation to obtain a precipitate, washing to be neutral by using deionized water, then placing into a drying oven, drying for 8 hours at the temperature of 125 ℃ to obtain a dried substance, placing into a muffle furnace preheated to the temperature of 950 ℃, and carrying out heat preservation and calcination for 5 minutes to obtain a calcined substance;
s6: respectively weighing 98g of ferric sulfate and 18g of ferric chloride, adding into 570mL of deionized water, stirring until the solid is dissolved, adjusting the pH to 10 by using 6mol/L sodium hydroxide, adding 5g of the calcined substance after adjustment, putting into a water bath, and stirring and mixing for 50min at 55 ℃ and 500 r/min;
s7: performing heat preservation and crystallization on the dispersed mixed solution at 50 ℃ for 5 hours, performing suction filtration after crystallization to obtain filter residue, washing the filter residue for 5 times by using deionized water, putting the filter residue into an oven, drying the filter residue at the temperature of 80 ℃ for 10 hours, and performing ball milling after drying until the particle size is 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 30min, and extruding and granulating under the conditions that the extrusion temperature is 188 ℃ and the die head temperature is 220 ℃ to obtain the wide-band-gap semiconductor material.
in this example, in S1, the fixed zinc oxide was ground in a ball mill for 15min, and the ground powder was weighed to calculate the grinding loss of the fixed zinc oxide.
In this embodiment, in S2, the solution is left standing for 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.
In this example, 45g of zinc oxide powder was weighed in S3 and put into the solution, followed by stirring and mixing until the zinc oxide powder was completely dissolved.
in this example, in S4, a 70-mesh sieve was used for filtration of the residue.
In this embodiment, in S5, after the filter residue is added to a 45% sodium nitrate solution by mass ratio of 3:6 and soaked for 3 hours, the solution is poured into a centrifuge bucket, and then the centrifuge bucket is driven by a driving device to rotate, so that the precipitate can be separated out.
in this example, in S6, pH was adjusted to 11.5 with 1mol/L NaOH after stirring, and ultrasonic dispersion was carried out for 12min after adjustment.
in this embodiment, 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 then ball-milled to a particle size of 0.8 μm, thereby obtaining a modified wide band gap.
In this example, in S8, the materials were mixed in a blender, mixed for 30min, and then fed into a twin-screw extruder for output.
In this example, in S8, the wide bandgap semiconductor material was obtained by extrusion granulation at a material temperature of 188 ℃ and a die temperature of 220 ℃ from a twin-screw extruder.
Comparative experiments of the properties of examples 1 to 3 were carried out in comparison with conventional wide band gap semiconductors, the experimental data being shown in the following table:
| Examples | A | II | III | |
| Percent production rate | 42% | 46% | 50% | |
| Percentage of mass stability | 35% | 36% | 37% |
as can be seen from the above table, the present invention can improve the production speed of the wide bandgap semiconductor and improve the quality stability, and the third embodiment is the most preferred embodiment.
the above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical scope of the present invention and the equivalent alternatives or modifications according to the technical solution and the inventive concept of the present invention within the technical scope of the present invention.
Claims (9)
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.
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