CN105502313B - A kind of method that gallium nitride nano crystal is prepared using double screw extruder - Google Patents
A kind of method that gallium nitride nano crystal is prepared using double screw extruder Download PDFInfo
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- CN105502313B CN105502313B CN201510978684.7A CN201510978684A CN105502313B CN 105502313 B CN105502313 B CN 105502313B CN 201510978684 A CN201510978684 A CN 201510978684A CN 105502313 B CN105502313 B CN 105502313B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0632—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with gallium, indium or thallium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Abstract
The invention belongs to inorganic compound semiconductor Material Field, more particularly to a kind of method that gallium nitride nano crystal is prepared using double screw extruder.Gallium salt is dissolved in water soluble polymer aqueous solution first and forms slurry, slurry is pumped into double screw extruder, slurry is by disperseing screwing element, gallium salt is made to be coated in the hydrogel network structure of water soluble polymer formation, it is shearing and under hot conditions water soluble polymer is being made to be carbonized, forming the gallium salt coated by carbon network structure；Thermoplastic cement is added in by auxiliary material mouth, reaction is kneaded and forms thin slice by squeezing；Thin slice is placed in tube furnace after drying, tubular type furnace temperature is increased to 900 ~ 1200 DEG C, ammonia is passed through and reacts 120 ~ 150 min, stops logical ammonia and is cooled to room temperature in argon atmosphere, obtain the faint yellow gallium nitride nano crystal of crystal form rule.Gallium nitride surface topography prepared by the present invention is good, crystal form is regular, yield is high, purity is high, is with a wide range of applications.
Description
Technical field
It is more particularly to a kind of to prepare nitrogen using double screw extruder the invention belongs to inorganic compound semiconductor Material Field
Change the method for gallium nanocrystal.
Background technology
Gallium nitride and carborundum（SiC）, the semi-conducting materials such as diamond be known as third generation semi-conducting material, Yu Chuan together
The silicon substrate of system is compared with GaAs base semiconductor material, and the third generations such as gallium nitride semi-conducting material is due to its distinctive forbidden band model
It encloses, excellent light, electrical properties and excellent material property, disclosure satisfy that high-power, high-temperature high-frequency and high-speed semiconductor device
Job requirement, be widely used prospect in terms of automobile and aircraft industry, medical treatment, military affairs and general lighting.
GaN materials belong to direct transition type semiconductor material with wide forbidden band, and wide direct band gap is 3.4eV, while is also one kind
Stabilizer pole, hard materials with high melting point, with electron saturation velocities are high, dielectric coefficient is small, good heat conductivity and radioresistance are strong
High excellent performance is spent, is to make light emitting diode (LED), laser diode (LD) and high temperature high power integrated circuit
Ideal material.GaN also have strong atom key, high thermal conductivity, good chemical stability (hardly by any acid corrosion),
High-breakdown-voltage and strong Radiation hardness etc. are beaten in synthesizing high temperature gas sensor material, high density data storage, high-rate laser
The application aspects such as print, ultraviolet detector, high-frequency microwave device and high density integrated circuit also have wide application potential.Therefore
GaN material becomes the research hotspot of current field of photoelectric material.
Gallium nitride nano crystal has huge application prospect due to its unique structure and photoelectricity performance.At present,
The preparation of GaN material can be obtained by chemical vapour deposition technique, pulsed laser deposition, sol-gal process, molecular beam epitaxy etc.
It arrives, if China Patent Publication No. CN101774552A discloses a kind of preparation method of GaN nanocrystals, first by Ga2O3
It is added in concentrated nitric acid, GaO is thermally formed using microwave hydrothermal2H nanometer rods, then by GaO2H nanometer rods powders are put
Enter in tube furnace, faint yellow GaN nanocrystals are obtained by the reaction under high temperature with ammonia, advantage is that raw material is relatively inexpensive, technique behaviour
Make simply, but due to being needed in preparation process using concentrated nitric acid, safety coefficient is low, and predecessor nanometer rods are unfavorable for gallium nitride crystalline substance
The growth of body is difficult to obtain the gallium nitride of high-quality.
China Patent Publication No. CN1944268 discloses a kind of side that gallium nitride nano crystal is prepared with sol-gal process
Method prepares gallium oxide/agraphitic carbon mixture using sol-gal process first, i.e., gallium nitrate is dissolved into concentrated nitric acid, addition
Become clear gel after being cooled down when citric acid heating stirring 2 is small, be packed into after dry in ceramic tube, at 850~950 DEG C of temperature with
Faint yellow GaN nanocrystals are obtained by the reaction in ammonia, and this method can largely prepare grain size less than or equal to Bohr's exciton radii
Gallium nitride nano crystal, but due to being needed in preparation process using concentrated nitric acid, safety coefficient is low, and the nanocrystalline dignity prepared
Product is small, influences the performance of gallium nitride, is unfavorable for mass producing.
But since crystal growth rate is low in the above method, the cycle is long, and the crystal shape generated is irregular, influences
The quality of gallium nitride nano crystal is not easy to popularize the large-scale industrial production of gallium nitride nano crystal, therefore, finds a kind of letter
The GaN nanocrystals of single, quick, cheap preparation high quality become the mesh of the unremitting pursuit of field of photoelectric material researcher
Mark.
The content of the invention
The present invention is in view of the above-mentioned problems, propose a kind of method that gallium nitride nano crystal is prepared using double screw extruder.
Gallium salt is dissolved in water soluble polymer aqueous solution first and forms slurry by this method, and slurry is pumped into double screw extruder,
Slurry by disperse screwing element, make gallium salt be coated on water soluble polymer formation hydrogel network structure in, shearing and
Under hot conditions water soluble polymer is made to be carbonized, form the gallium salt coated by carbon network structure；Thermoplasticity is added in by auxiliary material mouth
Glue is kneaded reaction and forms thin slice by squeezing, and the template in thin slice as gallium source and crystal growth to obtain prepares gallium nitride crystalline substance
Body.Preparation method of the present invention is reproducible, at low cost, no catalysis, no template, nitridation that is also environmentally friendly, and growing
Gallium crystal morphology is preferable, crystal form is regular, yield is high, purity is high, there is preferable application prospect.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of method that gallium nitride nano crystal is prepared using double screw extruder, it is characterised in that：It is squeezed using twin-screw
Go out machine and prepare gallium nitride nano crystal for reactor, comprise the following steps：
（1）Water soluble polymer and water are configured to the water soluble polymer aqueous solution that concentration is 60 ~ 120 g/L, by gold
Belong to gallium salt powder to be mixed to join in water soluble polymer aqueous solution, with the speed of 3000 ~ 5000 rpm in homogenizer
It is stirred 10 ~ 20min and obtains mixed slurry；
（2）By step（1）In obtained slurry be pumped into double screw extruder charge door, set scattered screwing element section anti-
Answering temperature, slurry makes gallium salt be coated on the hydrogel network of water soluble polymer formation by disperseing screwing element for 100 ~ 150 DEG C
In network structure；Then by shearing the screwing element that is carbonized, this section of reaction temperature is set for 180 ~ 240 DEG C, in shearing and high temperature item
Under part water soluble polymer is made to be carbonized, form the gallium salt coated by carbon network structure；Thermoplastic cement is added in by auxiliary material mouth, is set
Reaction temperature is 250 ~ 300 DEG C, is kneaded 10 ~ 15min of reaction, then forms thin slice by squeezing；
（3）By step（2）In obtained thin slice be placed in alundum (Al2O3) crucible, be put into the middle part flat-temperature zone of tube furnace,
Dry 15 ~ 30min under 180 ~ 250 DEG C of air atmosphere；
（4）The argon gas that flow is 50sccm is passed through into tube furnace, the temperature of tube furnace is warming up to 900 ~ 1200 DEG C, control
Heating rate processed is 8 ~ 20 DEG C/min, stops logical argon gas, is passed through the ammonia that flow is 50 ~ 100 sccm and reacts 120 ~ 150 min,
The logical ammonia of stopping changes argon gas into and is protected, and is cooled to room temperature in argon atmosphere, obtains faint yellow gallium nitride nano crystal.
Above-mentioned steps（1）Described in water soluble polymer for polyacrylamide, polyacrylic acid, polyethylene glycol, methylol
At least one of cellulose；The gallium salt is at least one of gallium nitrate, gallium chloride, acetic acid gallium, oxalic acid gallium；Institute
The dosage for the water soluble polymer stated is the 12 ~ 20% of gallium salt quality.
Above-mentioned steps（2）Described in thermoplastic cement for thermoplastic polyurethane, thermoplastic acrylic, thermoplastic styrene butadiene rubber
At least one of；The dosage of thermoplastic cement is the 4 ~ 8% of water soluble polymer quality.
Above-mentioned steps（2）Described in double screw extruder, screw slenderness ratio be 40 ~ 45:1；Screw rod is from feed end to end
End is once arranged to scattered screwing element, shearing carbonization screwing element, compression screwing element, reverse-flight elements, wherein pressing
Sheet die is set between contracting screwing element and reverse-flight elements.
A kind of method that gallium nitride nano crystal is prepared using double screw extruder of the present invention, is first dissolved gallium salt
In water soluble polymer aqueous solution, slurry is formed under high-speed stirred state, slurry is pumped into double screw extruder, slurry passes through
Scattered screwing element, makes gallium salt be coated in the hydrogel network structure of water soluble polymer formation, in shearing and hot conditions
Under water soluble polymer is made to be carbonized, form the gallium salt coated by carbon network structure；Thermoplastic cement is added in by auxiliary material mouth, is kneaded anti-
Thin slice should be formed by squeezing, be placed in thin slice as the template in gallium source and crystal growth in tube furnace, ammonia under hot conditions
It is uniformly diffused by carbon network structure inside thin slice, nitridation reaction occurs for the gallium salt with wrapping up in the network architecture, makes nitridation
Gallium nanocrystal homoepitaxial in thin slice template.The mixture thin slice formed by twin-screw extrusion has carbon network structure,
Be conducive to gallium source to be uniformly distributed, increase the surface area of reactant, ammonia is enable quickly to be nitrogenized completely with gallium source
Reaction, and thin slice provides template for the growth of gallium nitride, makes crystal homoepitaxial on thin slice, formed pattern it is preferable,
The nanocrystal of crystalline structure rule.The thermoplastic cement under the high temperature conditions in thin slice decomposes carbonization simultaneously, does not interfere with nitridation
The purity of gallium nanocrystal.Not only purity is high for the gallium nitride prepared using the present invention, reaction nanocrystal that is fast, and generating
With preferable pattern and complete crystalline structure.
A kind of method that gallium nitride nano crystal is prepared using double screw extruder of the present invention, is protruded compared with prior art
The characteristics of and beneficial effect be：
1st, a kind of method that gallium nitride nano crystal is prepared using double screw extruder of the present invention, gallium salt is coated on water-soluble
Property macromolecule formed hydrogel network structure in, reacted using twin-screw extrusion, form the gallium salt coated by carbon network structure
Thin slice prepares gallium nitride using thin slice as gallium source and template, increases the surface area of reactant, enables ammonia completely fast
With gallium source nitridation reaction occurs for speed, and thin slice provides template for the growth of gallium nitride, makes crystal uniform on thin slice
Growth forms the nanocrystal that pattern is preferable, crystalline structure is regular.
2nd, the gallium nitride pattern for preparing of the present invention is preferable, crystal form is regular, yield is high, purity is high, crystal growth rate
Height, generated time is short, there is preferable application prospect.
3rd, the method provided by the invention for preparing gallium nitride nano crystal, have preparation method it is reproducible, raw material into
This is cheap, and production specifications require low, no catalysis, and no template is also environmentally friendly, and easy to spread and large-scale production etc. is excellent
Point.
Specific embodiment
The present invention is explained in detail below in conjunction with specific embodiment, is not restricted to the present invention.It is not departing from
In the case of above method thought of the present invention, the various replacements made according to ordinary skill knowledge and customary means or change
Into should all be included in the protection scope of the present invention.
Embodiment 1
（1）Polyacrylamide and water are configured to the polyacrylamide solution that concentration is 60 g/L, by gallium nitrate powder
It is mixed to join in polyacrylamide solution, the dosage of polyacrylamide is the 12% of gallium nitrate dosage；In homogenizer
20 min are stirred with the speed of 3000 rpm and obtain mixed slurry；
（2）By step（1）In obtained slurry be pumped into double screw extruder charge door, set scattered screwing element section anti-
Answering temperature, slurry makes gallium salt be coated on the hydrogel network structure of polyacrylamide formation by disperseing screwing element for 100 DEG C
In；Then by shearing the screwing element that is carbonized, this section of reaction temperature is set for 240 DEG C, is shearing and is making poly- third under hot conditions
Acrylamide molecule is carbonized, and forms the gallium salt coated by carbon network structure；Dosage is added in by auxiliary material mouth to use for water soluble polymer
4% thermoplastic polyurethane of amount, it is 250 DEG C to set reaction temperature, is kneaded reaction 15min, then forms thin slice by squeezing；
（3）By step（2）In obtained thin slice be placed in alundum (Al2O3) crucible, be put into the middle part flat-temperature zone of tube furnace,
Dry 30min under 180 DEG C of air atmosphere；
（4）The argon gas that flow is 50sccm is passed through into tube furnace, the temperature of tube furnace is warming up to 900 DEG C, control rises
Warm rate is 8 DEG C/min, stops logical argon gas, is passed through the ammonia that flow is 100 sccm and reacts 120 min, stops logical ammonia and change into
Argon gas is protected, and is cooled to room temperature in argon atmosphere, obtains faint yellow gallium nitride nano crystal.
Embodiment 2
（1）Polyacrylic acid and water are configured to the polyacrylic acid aqueous solution that concentration is 90 g/L, gallium chloride powder is mixed
It is added in polyacrylic acid aqueous solution, the dosage of polyacrylic acid is the 15% of gallium chloride dosage；With 3500 in homogenizer
The speed of rpm is stirred 15 min and obtains mixed slurry；
（2）By step（1）In obtained slurry be pumped into double screw extruder charge door, set scattered screwing element section anti-
Answering temperature, slurry makes gallium salt be coated on the hydrogel network structure of polyacrylic acid formation by disperseing screwing element for 120 DEG C
In；Then by shearing the screwing element that is carbonized, this section of reaction temperature is set for 200 DEG C, is shearing and is making poly- third under hot conditions
Olefin(e) acid molecule is carbonized, and forms the gallium salt coated by carbon network structure；It is water soluble polymer dosage to add in dosage by auxiliary material mouth
5% thermoplastic acrylic, set reaction temperature be 250 DEG C, be kneaded reaction 15min, then by squeeze form thin slice；
（3）By step（2）In obtained thin slice be placed in alundum (Al2O3) crucible, be put into the middle part flat-temperature zone of tube furnace,
Dry 25 min under 200 DEG C of air atmosphere；
（4）The argon gas that flow is 50sccm is passed through into tube furnace, the temperature of tube furnace is warming up to 1000 DEG C, control rises
Warm rate is 10 DEG C/min, stops logical argon gas, is passed through the ammonia that flow is 80 sccm and reacts 120 min, stops logical ammonia and change into
Argon gas is protected, and is cooled to room temperature in argon atmosphere, obtains faint yellow gallium nitride nano crystal.
Embodiment 3
（1）Polyethylene glycol and water are configured to the Aqueous Solutions of Polyethylene Glycol that concentration is 100 g/L, acetic acid gallium powder is mixed
It is added in Aqueous Solutions of Polyethylene Glycol, the dosage of polyethylene glycol is the 18% of acetic acid gallium dosage；With 4000 in homogenizer
The speed of rpm is stirred 15 min and obtains mixed slurry；
（2）By step（1）In obtained slurry be pumped into double screw extruder charge door, set scattered screwing element section anti-
Answering temperature, slurry makes gallium salt be coated on the hydrogel network structure of polyethylene glycol formation by disperseing screwing element for 150 DEG C
In；Then by shearing the screwing element that is carbonized, this section of reaction temperature is set for 200 DEG C, is shearing and is making poly- second under hot conditions
Glycol molecules are carbonized, and form the gallium salt coated by carbon network structure；It is water soluble polymer dosage to add in dosage by auxiliary material mouth
6% thermoplastic styrene butadiene rubber, set reaction temperature be 280 DEG C, be kneaded reaction 12 min, then by squeeze formed it is thin
Piece；
（3）By step（2）In obtained thin slice be placed in alundum (Al2O3) crucible, be put into the middle part flat-temperature zone of tube furnace,
Dry 20 min under 230 DEG C of air atmosphere；
（4）The argon gas that flow is 50sccm is passed through into tube furnace, the temperature of tube furnace is warming up to 1100 DEG C, control rises
Warm rate is 15 DEG C/min, stops logical argon gas, is passed through the ammonia that flow is 60 sccm and reacts 150 min, stops logical ammonia and change
It is protected into argon gas, is cooled to room temperature in argon atmosphere, obtain faint yellow gallium nitride nano crystal.
Embodiment 4
（1）Hydroxymethyl cellulose and water are configured to the hydroxymethyl cellulose aqueous solution that concentration is 120 g/L, by oxalic acid gallium
Powder is mixed to join in hydroxymethyl cellulose aqueous solution, and the dosage of hydroxymethyl cellulose is the 20% of oxalic acid gallium dosage；At a high speed
10 min are stirred with the speed of 4500 rpm in mixer and obtain mixed slurry；
（2）By step（1）In obtained slurry be pumped into double screw extruder charge door, set scattered screwing element section anti-
Answering temperature, slurry makes gallium salt be coated on the hydrogel network knot of hydroxymethyl cellulose formation by disperseing screwing element for 150 DEG C
In structure；Then by shearing the screwing element that is carbonized, this section of reaction temperature is set for 180 DEG C, is shearing and is making hydroxyl under hot conditions
Methylcellulose molecule is carbonized, and forms the gallium salt coated by carbon network structure；It is water-soluble high score to add in dosage by auxiliary material mouth
7% thermoplastic cement of sub- dosage, it is 300 DEG C to set reaction temperature, is kneaded 10 min of reaction, is then formed by extruding thin
Piece；
（3）By step（2）In obtained thin slice be placed in alundum (Al2O3) crucible, be put into the middle part flat-temperature zone of tube furnace,
Dry 15 min under 250 DEG C of air atmosphere；
（4）The argon gas that flow is 50sccm is passed through into tube furnace, the temperature of tube furnace is warming up to 1150 DEG C, control rises
Warm rate is 20 DEG C/min, stops logical argon gas, is passed through the ammonia that flow is 50 sccm and reacts 150 min, stops logical ammonia and change into
Argon gas is protected, and is cooled to room temperature in argon atmosphere, obtains faint yellow gallium nitride nano crystal.
Embodiment 5
（1）Polyethylene glycol and water are configured to the Aqueous Solutions of Polyethylene Glycol that concentration is 120 g/L, gallium nitrate powder is mixed
It is added in Aqueous Solutions of Polyethylene Glycol, the dosage of polyethylene glycol is the 20% of gallium nitrate dosage；With 5000 in homogenizer
The speed of rpm is stirred 10min and obtains mixed slurry；
（2）By step（1）In obtained slurry be pumped into double screw extruder charge door, set scattered screwing element section anti-
Answering temperature, slurry makes gallium salt be coated on the hydrogel network structure of polyethylene glycol formation by disperseing screwing element for 150 DEG C
In；Then by shearing the screwing element that is carbonized, this section of reaction temperature is set for 200 DEG C, is shearing and is making poly- second under hot conditions
Glycol molecules are carbonized, and form the gallium salt coated by carbon network structure；Dosage is added in as the 8% of polyethylene glycol dosage by auxiliary material mouth
Thermoplastic polyurethane, set reaction temperature be 300 DEG C, be kneaded reaction 10 min, then by squeeze form thin slice；
（3）By step（2）In obtained thin slice be placed in alundum (Al2O3) crucible, be put into the middle part flat-temperature zone of tube furnace,
Dry 20 min under 250 DEG C of air atmosphere；
（4）The argon gas that flow is 50sccm is passed through into tube furnace, the temperature of tube furnace is warming up to 1200 DEG C, control rises
Warm rate is 20 DEG C/min, stops logical argon gas, is passed through the ammonia that flow is 80 sccm and reacts 120 min, stops logical ammonia and change
It is protected into argon gas, is cooled to room temperature in argon atmosphere, obtain faint yellow gallium nitride nano crystal.
Claims (3)
- A kind of 1. method that gallium nitride nano crystal is prepared using double screw extruder, it is characterised in that:Utilize twin-screw extrusion Machine prepares gallium nitride nano crystal for reactor, and specific preparation method comprises the following steps：（1）Water soluble polymer and water are configured to the water soluble polymer aqueous solution that concentration is 60 ~ 120 g/L, by gallium Salt powder is mixed to join in water soluble polymer aqueous solution, is stirred in homogenizer with the speed of 3000 ~ 5000 rpm 10 ~ 20 min of mixing obtain mixed slurry；（2）By step（1）In obtained slurry be pumped into double screw extruder charge door, scattered screwing element section reaction temperature is set It spends for 100 ~ 150 DEG C, slurry makes gallium salt be coated on the hydrogel network knot of water soluble polymer formation by disperseing screwing element In structure；Then by shearing the screwing element that is carbonized, this section of reaction temperature is set for 180 ~ 240 DEG C, under shearing and hot conditions Water soluble polymer is made to be carbonized, forms the gallium salt coated by carbon network structure；Thermoplastic cement is added in by auxiliary material mouth, reaction is set Temperature is 250 ~ 300 DEG C, is kneaded 10 ~ 15min of reaction, then forms thin slice by squeezing；The wherein described double screw extruder, Screw slenderness ratio is 40 ~ 45:1；Screw rod is once arranged to scattered screwing element, shearing carbonization screw thread member by feed end terminad Part, compression screwing element, reverse-flight elements, wherein setting sheet die between compression screwing element and reverse-flight elements；（3）By step（2）In obtained thin slice be placed in alundum (Al2O3) crucible, be put into the middle part flat-temperature zone of tube furnace, 180 ~ Dry 15 ~ 30min under 250 DEG C of air atmosphere；（4）The argon gas that flow is 50sccm is passed through into tube furnace, the temperature of tube furnace is warming up to 900 ~ 1200 DEG C, control rises Warm rate is 8 ~ 20 DEG C/min, stops logical argon gas, is passed through the ammonia that flow is 50 ~ 100 sccm and reacts 120 ~ 150 min, stops Logical ammonia changes argon gas into and is protected, and is cooled to room temperature in argon atmosphere, obtains faint yellow gallium nitride nano crystal.
- 2. a kind of method that gallium nitride nano crystal is prepared using double screw extruder according to claim 1, feature It is step（1）Described in water soluble polymer be polyacrylamide, polyacrylic acid, polyethylene glycol, in hydroxymethyl cellulose At least one；The gallium salt is at least one of gallium nitrate, gallium chloride, acetic acid gallium, oxalic acid gallium；Described is water-soluble Property high molecular dosage be gallium salt quality 12 ~ 20%.
- 3. a kind of method that gallium nitride nano crystal is prepared using double screw extruder according to claim 1, feature It is step（2）Described in thermoplastic cement be thermoplastic polyurethane, thermoplastic acrylic, in thermoplastic styrene butadiene rubber at least It is a kind of；The dosage of thermoplastic cement is the 4 ~ 8% of water soluble polymer quality.
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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 |
| US9175418B2 (en) * | 2009-10-09 | 2015-11-03 | 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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