CN105502313A - Method for preparing gallium nitride nanocrystals by using twin-screw extruder - Google Patents
Method for preparing gallium nitride nanocrystals by using twin-screw extruder Download PDFInfo
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Abstract
The invention belongs to the field of inorganic compound semiconductor materials and particularly relates to a method for preparing gallium nitride nanocrystals by using a twin-screw extruder. Firstly, gallium salt is dissolved in a water-soluble polymer aqueous solution, slurry is formed, is pumped into the twin-screw extruder and passes through a dispersion screw element, so that the gallium salt is coated with a hydrogel network structure formed by water-soluble polymers, the water-soluble polymers are carbonized under shearing and high-temperature conditions, and the gallium salt coated with the carbon network structure is formed; thermoplastic rubber is added via an accessory port for a mixing reaction, and a sheet is formed through extrusion; after the sheet is placed in a tube furnace for drying, the temperature of the tube furnace is increased to 900-1200 DEG C, nitrogen is introduced for a reaction for 120-150 min, nitrogen introduction is stopped, the reactant is cooled to the room temperature in an argon atmosphere, and faint yellow gallium nitride nanocrystals with the regular crystal form are obtained. The prepared gallium nitride nanocrystals have good surface morphology and the regular crystal form, are high in yield and purity and have high application value.
Description
Technical field
The invention belongs to inorganic compound semiconductor Material Field, particularly a kind of method utilizing twin screw extruder to prepare gallium nitride nano crystal.
Background technology
Gan is described as third generation semiconductor material together with the semiconductor materials such as silicon carbide (SiC), diamond, compare in traditional silica-based and GaAs based semiconductor material, the third generation semiconductor materials such as gan are due to the material property of its distinctive forbidden band scope, excellent optical, electrical character and excellence, can meet the job requirement of high-power, high-temperature high-frequency and high-speed semiconductor device, be widely used prospect in automobile and aircraft industry, medical treatment, military affairs and general lighting.
GaN material belongs to direct transition type semiconductor material with wide forbidden band, wide direct band gap is 3.4eV, also be a kind of stabilizer pole, hard materials with high melting point simultaneously, have that electron saturation velocities is high, dielectric coefficient is little, good heat conductivity and the premium properties such as radiation resistance is high, be the ideal material making photodiode (LED), laser diode (LD) and high temperature high power unicircuit.GaN also has strong atomic bond, high thermal conductivity, good chemical stability (hardly by any acid corrosion), high-breakdown-voltage and strong Radiation hardness etc., also has wide application potential in application aspect such as synthesizing high temperature gas sensor material, high density data storage, high-rate laser printing, ultraviolet detector, high frequency microwave device and high density integrated circuits.Therefore GaN material becomes the study hotspot of current field of photoelectric material.
Gallium nitride nano crystal, due to the structure of its uniqueness and photoelectricity performance, has huge application prospect.At present, the preparation of GaN material obtains, as China Patent Publication No. CN101774552A discloses a kind of preparation method of GaN nanocrystal, first by Ga by chemical Vapor deposition process, pulsed laser deposition, sol-gel method, molecular beam epitaxy etc.
2o
3
Join in concentrated nitric acid, utilize microwave hydrothermal to add thermosetting GaO
2h nanometer rod, then by GaO
2h nanometer rod powder puts into tube furnace, faint yellow GaN nanocrystal is obtained with ammonia gas react under high temperature, its advantage is that raw material is relatively inexpensive, technological operation is simple, but owing to needing to use concentrated nitric acid in preparation process, safety coefficient is low, and precursor nanometer rod is unfavorable for the growth of gallium nitride, is difficult to obtain the gallium nitride of high-quality.
China Patent Publication No. CN1944268 discloses a kind of method that sol-gel method prepares gallium nitride nano crystal, first sol-gel method is adopted to prepare gallium oxide/agraphitic carbon mixture, be dissolved in concentrated nitric acid by gallium nitrate, clear gel is become after adding the cooling in 2 hours of citric acid heated and stirred, load after dry in vitrified pipe, faint yellow GaN nanocrystal is obtained with ammonia gas react at temperature 850 ~ 950 DEG C, the method can prepare the gallium nitride nano crystal that particle diameter is less than or equal to Bohr's exciton radii in a large number, but owing to needing to use concentrated nitric acid in preparation process, safety coefficient is low, and the nanocrystal area of preparation is little, affect the performance of gallium nitride, be unfavorable for scale operation.
But, because crystal growth rate is low in aforesaid method, cycle is long, and the crystal shape generated is irregular, affect the quality of gallium nitride nano crystal, not easily the large-scale industrial production of universal gallium nitride nano crystal, therefore, finds the target that the high-quality GaN nanocrystal of a kind of simple, quick, cheap preparation becomes field of photoelectric material researcher unremitting pursue.
Summary of the invention
The present invention is directed to the problems referred to above, propose a kind of method utilizing twin screw extruder to prepare gallium nitride nano crystal.First gallium salt is dissolved in the water-soluble polymer aqueous solution and forms slurry by the method, slurry is pumped into twin screw extruder, slurry is by dispersion screwing element, gallium salt is made to be coated in the hydrogel network structure of water-soluble polymer formation, under shearing and hot conditions, make water-soluble polymer carbonization, formed by the coated gallium salt of carbon network structure; Add thermoplastic cement by auxiliary material mouth, mixing reaction forms thin slice by extruding, using the thin slice obtained as the Template preparation gallium nitride of gallium source and crystal growth.Preparation method of the present invention is reproducible, and cost is low, without catalysis, without template, also environmentally friendly, and the gallium nitride pattern grown is better, crystal formation is regular, output is high, purity is high, has good application prospect.
For achieving the above object, the present invention adopts following technical scheme:
Utilize twin screw extruder to prepare a method for gallium nitride nano crystal, it is characterized in that: utilize twin screw extruder to prepare gallium nitride nano crystal for reactor, comprise the following steps:
(1) water-soluble polymer and water are mixed with the water-soluble polymer aqueous solution that concentration is 60 ~ 120g/L, gallium salt powder is mixed to join in the water-soluble polymer aqueous solution, in homogenizer, is uniformly mixed 10 ~ 20min with the speed of 3000 ~ 5000rpm obtains mixed slurry;
(2) slurry obtained in step (1) is pumped in twin screw extruder charging opening, arranging dispersion screwing element section temperature of reaction is 100 ~ 150 DEG C, slurry, by dispersion screwing element, makes gallium salt be coated in the hydrogel network structure of water-soluble polymer formation; Then by shearing carbonization screwing element, arranging this section of temperature of reaction is 180 ~ 240 DEG C, makes water-soluble polymer carbonization, formed by the coated gallium salt of carbon network structure under shearing and hot conditions; Add thermoplastic cement by auxiliary material mouth, arranging temperature of reaction is 250 ~ 300 DEG C, mixing reaction 10 ~ 15min, then forms thin slice by extruding;
(3) thin slice obtained in step (2) is placed in aluminium sesquioxide crucible, puts into the flat-temperature zone, middle part of tube furnace, dry 15 ~ 30min under the air atmosphere of 180 ~ 250 DEG C;
(4) in tube furnace, the argon gas that flow is 50sccm is passed into; by the temperature to 900 of tube furnace ~ 1200 DEG C; controlling temperature rise rate is 8 ~ 20 DEG C/min; stop logical argon gas; pass into ammonia gas react 120 ~ 150min that flow is 50 ~ 100sccm; stop logical ammonia to change argon gas protection into, in argon atmosphere, be cooled to room temperature, obtain faint yellow gallium nitride nano crystal.
Water-soluble polymer described in above-mentioned steps (1) is at least one in polyacrylamide, polyacrylic acid, polyoxyethylene glycol, Walocel MT 20.000PV; Described gallium salt is at least one in gallium nitrate, gallium chloride, acetic acid gallium, oxalic acid gallium; The consumption of described water-soluble polymer is 12 ~ 20% of gallium salt quality.
Thermoplastic cement described in above-mentioned steps (2) is at least one in thermoplastic polyurethane, thermoplastic acrylic, thermoplastic styrene butadiene rubber; The consumption of thermoplastic cement is 4 ~ 8% of water-soluble polymer quality.
Twin screw extruder described in above-mentioned steps (2), screw slenderness ratio is 40 ~ 45:1; Screw rod is once set to dispersion screwing element by feed end terminad, shears carbonization screwing element, is compressed screwing element, reverse-flight elements, wherein between compression screwing element and reverse-flight elements, arranges sheet die.
A kind of method utilizing twin screw extruder to prepare gallium nitride nano crystal of the present invention, first gallium salt is dissolved in the water-soluble polymer aqueous solution, slurry is formed under high-speed stirring state, slurry is pumped into twin screw extruder, slurry is by dispersion screwing element, make gallium salt be coated in the hydrogel network structure of water-soluble polymer formation, under shearing and hot conditions, make water-soluble polymer carbonization, formed by the coated gallium salt of carbon network structure; Thermoplastic cement is added by auxiliary material mouth, mixing reaction forms thin slice by extruding, thin slice is placed in tube furnace as the template of gallium source and crystal growth, under hot conditions, ammonia is evenly diffused into thin slice inside by carbon network structure, with parcel gallium salt generation nitrogenizing reaction in the network architecture, make gallium nitride nano crystal homoepitaxial in thin slice template.The mixture thin slice formed by twin-screw extrusion has carbon network structure, be conducive to gallium source to distribute uniformly, increase the surface-area of reactant, ammonia is enable with gallium source, nitrogenizing reaction to occur completely fast, and the growth that thin slice is gallium nitride provides template, make crystal homoepitaxial on thin slice, form the nanocrystal that pattern is better, crystalline structure is regular.Thermoplastic cement simultaneously under the high temperature conditions in thin slice decomposes carbonization, can not affect the purity of gallium nitride nano crystal.Not only purity is high for the gallium nitride adopting the present invention to prepare, reaction is fast, and the nanocrystal generated has good pattern and complete crystalline structure.
A kind of method utilizing twin screw extruder to prepare gallium nitride nano crystal of the present invention, compared with prior art outstanding feature and useful effect are:
1, a kind of method utilizing twin screw extruder to prepare gallium nitride nano crystal of the present invention, gallium salt is coated in the hydrogel network structure of water-soluble polymer formation, twin-screw extrusion is utilized to react, formed by the coated gallium salt thin slice of carbon network structure, using thin slice as gallium source and Template preparation gallium nitride, increase the surface-area of reactant, ammonia is enable with gallium source, nitrogenizing reaction to occur completely fast, and the growth that thin slice is gallium nitride provides template, make crystal homoepitaxial on thin slice, formation pattern is better, the nanocrystal of crystalline structure rule.
2, the gallium nitride pattern prepared of the present invention is better, crystal formation is regular, output is high, purity is high, and crystal growth rate is high, and generated time is short, has good application prospect.
3, the method preparing gallium nitride nano crystal provided by the invention, have preparation method reproducible, material cost is cheap, and production specifications require low, without catalysis, without template, also environmentally friendly, is easy to the advantages such as popularization and large-scale production.
Embodiment
Below in conjunction with embodiment, the present invention is explained in detail, is not restricted to the present invention.When not departing from aforesaid method thought of the present invention, the various replacement made according to ordinary skill knowledge and customary means or improvement, all should be included within protection scope of the present invention.
embodiment 1
(1) polyacrylamide and water are mixed with the polyacrylamide solution that concentration is 60g/L, are mixed to join in polyacrylamide solution by gallium nitrate powder, the consumption of polyacrylamide is 12% of gallium nitrate consumption; In homogenizer, be uniformly mixed 20min with the speed of 3000rpm obtain mixed slurry;
(2) pumped in twin screw extruder charging opening by the slurry obtained in step (1), arranging dispersion screwing element section temperature of reaction is 100 DEG C, and slurry, by dispersion screwing element, makes gallium salt be coated in the hydrogel network structure of polyacrylamide formation; Then by shearing carbonization screwing element, arranging this section of temperature of reaction is 240 DEG C, makes the carbonization of polyacrylamide molecule, formed by the coated gallium salt of carbon network structure under shearing and hot conditions; Add by auxiliary material mouth the thermoplastic polyurethane that consumption is 4% of water-soluble polymer consumption, arranging temperature of reaction is 250 DEG C, mixing reaction 15min, then forms thin slice by extruding;
(3) thin slice obtained in step (2) is placed in aluminium sesquioxide crucible, puts into the flat-temperature zone, middle part of tube furnace, dry 30min under the air atmosphere of 180 DEG C;
(4) in tube furnace, the argon gas that flow is 50sccm is passed into; by the temperature to 900 of tube furnace DEG C; controlling temperature rise rate is 8 DEG C/min; stop logical argon gas; pass into the ammonia gas react 120min that flow is 100sccm; stop logical ammonia to change argon gas protection into, in argon atmosphere, be cooled to room temperature, obtain faint yellow gallium nitride nano crystal.
embodiment 2
(1) polyacrylic acid and water are mixed with the polyacrylic acid aqueous solution that concentration is 90g/L, are mixed to join by gallium chloride powder in the polyacrylic acid aqueous solution, polyacrylic consumption is 15% of gallium chloride consumption; In homogenizer, be uniformly mixed 15min with the speed of 3500rpm obtain mixed slurry;
(2) pumped in twin screw extruder charging opening by the slurry obtained in step (1), arranging dispersion screwing element section temperature of reaction is 120 DEG C, and slurry, by dispersion screwing element, makes gallium salt be coated in the hydrogel network structure of polyacrylic acid formation; Then by shearing carbonization screwing element, arranging this section of temperature of reaction is 200 DEG C, makes the carbonization of polyacrylic acid molecule, formed by the coated gallium salt of carbon network structure under shearing and hot conditions; Add by auxiliary material mouth the thermoplastic acrylic that consumption is 5% of water-soluble polymer consumption, arranging temperature of reaction is 250 DEG C, mixing reaction 15min, then forms thin slice by extruding;
(3) thin slice obtained in step (2) is placed in aluminium sesquioxide crucible, puts into the flat-temperature zone, middle part of tube furnace, dry 25min under the air atmosphere of 200 DEG C;
(4) in tube furnace, the argon gas that flow is 50sccm is passed into; by the temperature to 1000 of tube furnace DEG C; controlling temperature rise rate is 10 DEG C/min; stop logical argon gas; pass into the ammonia gas react 120min that flow is 80sccm; stop logical ammonia to change argon gas protection into, in argon atmosphere, be cooled to room temperature, obtain faint yellow gallium nitride nano crystal.
embodiment 3
(1) polyoxyethylene glycol and water are mixed with the Aqueous Solutions of Polyethylene Glycol that concentration is 100g/L, are mixed to join in Aqueous Solutions of Polyethylene Glycol by acetic acid gallium powder, the consumption of polyoxyethylene glycol is 18% of acetic acid gallium consumption; In homogenizer, be uniformly mixed 15min with the speed of 4000rpm obtain mixed slurry;
(2) pumped in twin screw extruder charging opening by the slurry obtained in step (1), arranging dispersion screwing element section temperature of reaction is 150 DEG C, and slurry, by dispersion screwing element, makes gallium salt be coated in the hydrogel network structure of polyoxyethylene glycol formation; Then by shearing carbonization screwing element, arranging this section of temperature of reaction is 200 DEG C, makes peg molecule carbonization, formed by the coated gallium salt of carbon network structure under shearing and hot conditions; Add by auxiliary material mouth the thermoplastic styrene butadiene rubber that consumption is 6% of water-soluble polymer consumption, arranging temperature of reaction is 280 DEG C, mixing reaction 12min, then forms thin slice by extruding;
(3) thin slice obtained in step (2) is placed in aluminium sesquioxide crucible, puts into the flat-temperature zone, middle part of tube furnace, dry 20min under the air atmosphere of 230 DEG C;
(4) in tube furnace, the argon gas that flow is 50sccm is passed into; by the temperature to 1100 of tube furnace DEG C; controlling temperature rise rate is 15 DEG C/min; stop logical argon gas; pass into the ammonia gas react 150min that flow is 60sccm; stop logical ammonia to change argon gas protection into, in argon atmosphere, be cooled to room temperature, obtain faint yellow gallium nitride nano crystal.
embodiment 4
(1) Walocel MT 20.000PV and water are mixed with the Walocel MT 20.000PV aqueous solution that concentration is 120g/L, are mixed to join in the Walocel MT 20.000PV aqueous solution by oxalic acid gallium powder, the consumption of Walocel MT 20.000PV is 20% of oxalic acid gallium consumption; In homogenizer, be uniformly mixed 10min with the speed of 4500rpm obtain mixed slurry;
(2) pumped in twin screw extruder charging opening by the slurry obtained in step (1), arranging dispersion screwing element section temperature of reaction is 150 DEG C, and slurry, by dispersion screwing element, makes gallium salt be coated in the hydrogel network structure of Walocel MT 20.000PV formation; Then by shearing carbonization screwing element, arranging this section of temperature of reaction is 180 DEG C, makes the carbonization of Walocel MT 20.000PV molecule, formed by the coated gallium salt of carbon network structure under shearing and hot conditions; Add by auxiliary material mouth the thermoplastic cement that consumption is 7% of water-soluble polymer consumption, arranging temperature of reaction is 300 DEG C, mixing reaction 10min, then forms thin slice by extruding;
(3) thin slice obtained in step (2) is placed in aluminium sesquioxide crucible, puts into the flat-temperature zone, middle part of tube furnace, dry 15min under the air atmosphere of 250 DEG C;
(4) in tube furnace, the argon gas that flow is 50sccm is passed into; by the temperature to 1150 of tube furnace DEG C; controlling temperature rise rate is 20 DEG C/min; stop logical argon gas; pass into the ammonia gas react 150min that flow is 50sccm; stop logical ammonia to change argon gas protection into, in argon atmosphere, be cooled to room temperature, obtain faint yellow gallium nitride nano crystal.
embodiment 5
(1) polyoxyethylene glycol and water are mixed with the Aqueous Solutions of Polyethylene Glycol that concentration is 120g/L, are mixed to join in Aqueous Solutions of Polyethylene Glycol by gallium nitrate powder, the consumption of polyoxyethylene glycol is 20% of gallium nitrate consumption; In homogenizer, be uniformly mixed 10min with the speed of 5000rpm obtain mixed slurry;
(2) pumped in twin screw extruder charging opening by the slurry obtained in step (1), arranging dispersion screwing element section temperature of reaction is 150 DEG C, and slurry, by dispersion screwing element, makes gallium salt be coated in the hydrogel network structure of polyoxyethylene glycol formation; Then by shearing carbonization screwing element, arranging this section of temperature of reaction is 200 DEG C, makes peg molecule carbonization, formed by the coated gallium salt of carbon network structure under shearing and hot conditions; Add by auxiliary material mouth the thermoplastic polyurethane that consumption is 8% of polyoxyethylene glycol consumption, arranging temperature of reaction is 300 DEG C, mixing reaction 10min, then forms thin slice by extruding;
(3) thin slice obtained in step (2) is placed in aluminium sesquioxide crucible, puts into the flat-temperature zone, middle part of tube furnace, dry 20min under the air atmosphere of 250 DEG C;
(4) in tube furnace, the argon gas that flow is 50sccm is passed into; by the temperature to 1200 of tube furnace DEG C; controlling temperature rise rate is 20 DEG C/min; stop logical argon gas; pass into the ammonia gas react 120min that flow is 80sccm; stop logical ammonia to change argon gas protection into, in argon atmosphere, be cooled to room temperature, obtain faint yellow gallium nitride nano crystal.
Claims (4)
1. utilize twin screw extruder to prepare a method for gallium nitride nano crystal, it is characterized in that: utilize twin screw extruder to prepare gallium nitride nano crystal for reactor, concrete preparation method comprises the following steps:
(1) water-soluble polymer and water are mixed with the water-soluble polymer aqueous solution that concentration is 60 ~ 120g/L, gallium salt powder is mixed to join in the water-soluble polymer aqueous solution, in homogenizer, is uniformly mixed 10 ~ 20min with the speed of 3000 ~ 5000rpm obtains mixed slurry;
(2) slurry obtained in step (1) is pumped in twin screw extruder charging opening, arranging dispersion screwing element section temperature of reaction is 100 ~ 150 DEG C, slurry, by dispersion screwing element, makes gallium salt be coated in the hydrogel network structure of water-soluble polymer formation; Then by shearing carbonization screwing element, arranging this section of temperature of reaction is 180 ~ 240 DEG C, makes water-soluble polymer carbonization, formed by the coated gallium salt of carbon network structure under shearing and hot conditions; Add thermoplastic cement by auxiliary material mouth, arranging temperature of reaction is 250 ~ 300 DEG C, mixing reaction 10 ~ 15min, then forms thin slice by extruding;
(3) thin slice obtained in step (2) is placed in aluminium sesquioxide crucible, puts into the flat-temperature zone, middle part of tube furnace, dry 15 ~ 30min under the air atmosphere of 180 ~ 250 DEG C;
(4) in tube furnace, the argon gas that flow is 50sccm is passed into; by the temperature to 900 of tube furnace ~ 1200 DEG C; controlling temperature rise rate is 8 ~ 20 DEG C/min; stop logical argon gas; pass into ammonia gas react 120 ~ 150min that flow is 50 ~ 100sccm; stop logical ammonia to change argon gas protection into, in argon atmosphere, be cooled to room temperature, obtain faint yellow gallium nitride nano crystal.
2. a kind of method utilizing twin screw extruder to prepare gallium nitride nano crystal according to claim 1, is characterized in that the water-soluble polymer described in step (1) is at least one in polyacrylamide, polyacrylic acid, polyoxyethylene glycol, Walocel MT 20.000PV; Described gallium salt is at least one in gallium nitrate, gallium chloride, acetic acid gallium, oxalic acid gallium; The consumption of described water-soluble polymer is 12 ~ 20% of gallium salt quality.
3. a kind of method utilizing twin screw extruder to prepare gallium nitride nano crystal according to claim 1, is characterized in that the thermoplastic cement described in step (2) is at least one in thermoplastic polyurethane, thermoplastic acrylic, thermoplastic styrene butadiene rubber; The consumption of thermoplastic cement is 4 ~ 8% of water-soluble polymer quality.
4. a kind of method utilizing twin screw extruder to prepare gallium nitride nano crystal according to claim 1, it is characterized in that the twin screw extruder described in step (2), screw slenderness ratio is 40 ~ 45:1; Screw rod is once set to dispersion screwing element by feed end terminad, shears carbonization screwing element, is compressed screwing element, reverse-flight elements, wherein between compression screwing element and reverse-flight elements, arranges sheet die.
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| CN110544721A (en) * | 2019-08-21 | 2019-12-06 | 大同新成新材料股份有限公司 | Preparation method of semiconductor material |
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| US4851203A (en) * | 1986-04-03 | 1989-07-25 | Atochem | Metal carbide and nitride powders |
| CN1944268A (en) * | 2006-10-25 | 2007-04-11 | 国家纳米技术与工程研究院 | Method for preparing gallium nitride nano crystal using sol-gel method |
| CN102933520A (en) * | 2010-06-08 | 2013-02-13 | 电气化学工业株式会社 | Aluminium nitride substrate for circuit board and production method thereof |
| CN104629276A (en) * | 2013-11-12 | 2015-05-20 | 珠海市红旌发展有限公司 | Preparation method for nanocrystal cellulose composite material, product and application thereof |
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| GB9113789D0 (en) * | 1991-06-26 | 1991-08-14 | Stork Protecon Bv | Controlled shear cell and method |
| US6832735B2 (en) * | 2002-01-03 | 2004-12-21 | Nanoproducts Corporation | Post-processed nanoscale powders and method for such post-processing |
| WO2011044554A1 (en) * | 2009-10-09 | 2011-04-14 | Soraa, Inc. | Method for synthesis of high quality large area bulk gallium based crystals |
| CN102001170B (en) * | 2010-03-12 | 2013-11-20 | 北京化工大学 | High molecular material balanced extruder and axial force balancing method thereof |
| CN104009229B (en) * | 2014-05-21 | 2016-01-13 | 成都新柯力化工科技有限公司 | LiFePO4 of a kind of morphology controllable and preparation method thereof |
| CN104445108A (en) * | 2014-11-28 | 2015-03-25 | 中国科学院物理研究所 | GaN microcrystalline and synthetic method thereof |
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|---|---|---|---|---|
| US4851203A (en) * | 1986-04-03 | 1989-07-25 | Atochem | Metal carbide and nitride powders |
| CN1944268A (en) * | 2006-10-25 | 2007-04-11 | 国家纳米技术与工程研究院 | Method for preparing gallium nitride nano crystal using sol-gel method |
| CN102933520A (en) * | 2010-06-08 | 2013-02-13 | 电气化学工业株式会社 | Aluminium nitride substrate for circuit board and production method thereof |
| CN104629276A (en) * | 2013-11-12 | 2015-05-20 | 珠海市红旌发展有限公司 | Preparation method for nanocrystal cellulose composite material, product and application thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110544721A (en) * | 2019-08-21 | 2019-12-06 | 大同新成新材料股份有限公司 | Preparation method of semiconductor material |
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