CN108357070A - A kind of double screw extruder and its application - Google Patents
A kind of double screw extruder and its application Download PDFInfo
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- CN108357070A CN108357070A CN201810069573.8A CN201810069573A CN108357070A CN 108357070 A CN108357070 A CN 108357070A CN 201810069573 A CN201810069573 A CN 201810069573A CN 108357070 A CN108357070 A CN 108357070A
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- screwing element
- gallium
- screw extruder
- double screw
- network structure
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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 discloses a kind of double screw extruder, the screw slenderness ratio is 40~45:1；Screw rod is once set as dispersion screwing element, shearing carbonization screwing element, compression screwing element, reverse-flight elements by feed end terminad, wherein sheet die is arranged between compression screwing element and reverse-flight elements.The gallium nitride nano crystal surface topography of dual-screw-stem machine preparation disclosed by the invention is good, crystal form is regular, yield is high, purity is high, is with a wide range of applications.
Description
The application is application No. is 2015109786847, and the applying date is on December 24th, 2015, and invention and created name is
The divisional application of the patent of " a method of preparing gallium nitride nano crystal using double screw extruder ".
Technical field
The invention belongs to inorganic compound semiconductor Material Fields, more particularly to a kind of to prepare nitrogen using double screw extruder
Change the method for gallium nanocrystal.
Background technology
It is known as third generation semi-conducting material, Yu Chuan together with the semi-conducting materials such as gallium nitride and silicon carbide (SiC), diamond
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 foreground in terms of automobile and aircraft industry, medical treatment, military affairs and general lighting.
GaN material belongs to direct transition type semiconductor material with wide forbidden band, and wide direct band gap is 3.4eV, while being also one kind
Stabilizer pole, hard materials with high melting point has small electron saturation velocities height, dielectric coefficient, good heat conductivity and radioresistance strong
High excellent performance is spent, is the ideal for making light emitting diode (LED), laser diode (LD) and high temperature high power integrated circuit
Material.GaN also has strong atom key, high thermal conductivity, good chemical stability (hardly by any acid corrosion), high breakdown
Voltage and strong Radiation hardness etc., in synthesizing high temperature gas sensor material, high density data storage, high-rate laser printing, purple
The application aspects such as external detector, high-frequency microwave device and high density integrated circuit also have wide application potential.Therefore GaN materials
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.Currently,
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, GaO2H nanometer rods is thermally formed using microwave hydrothermal, then by GaO2H nanometer rods powders
It is put into tube furnace, faint yellow GaN nanocrystals is obtained by the reaction under high temperature with ammonia, its advantage is that raw material is relatively inexpensive, technique
It is easy to operate, but due to needing to use concentrated nitric acid in preparation process, safety coefficient is low, and predecessor nanometer rods are unfavorable for gallium nitride
The growth of crystal is difficult to obtain the gallium nitride of high-quality.
China Patent Publication No. CN1944268 discloses a kind of side preparing gallium nitride nano crystal 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 the cooling in 2 hours of citric acid heating stirring, be packed into ceramic tube after dry, 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 needing to use concentrated nitric acid in preparation process, safety coefficient is low, and the nanocrystal area prepared
It is small, the performance of gallium nitride is influenced, is unfavorable for mass producing.
But since crystal growth rate is low in the above method, the period is long, and the crystal shape generated is irregular, influences
Therefore the quality of gallium nitride nano crystal, the large-scale industrial production for being not easy universal gallium nitride nano crystal find 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.
Invention content
The present invention is in view of the above-mentioned problems, propose a kind of method preparing gallium nitride nano crystal 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
So that water soluble polymer is carbonized under hot conditions, forms the gallium salt coated by carbon network structure；Thermoplasticity is added by auxiliary material mouth
Glue is kneaded reaction and forms thin slice by squeezing, and gallium nitride crystalline substance is prepared as the template in gallium source and crystal growth using obtained thin slice
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 method of preparing gallium nitride nano crystal using double screw extruder, it is characterised in that：It is squeezed using twin-screw
It is that reactor prepares gallium nitride nano crystal to go out machine, is included the following steps：
(1) water soluble polymer and water are configured to the water soluble polymer aqueous solution of a concentration of 60~120g/L, it will be golden
Belong to gallium salt powder to be mixed to join in water soluble polymer aqueous solution, with the speed of 3000~5000rpm in homogenizer
It is stirred 10~20min and obtains mixed slurry；
(2) slurry obtained in step (1) is pumped into double screw extruder charge door, setting dispersion screwing element section is anti-
It is 100~150 DEG C to answer temperature, and slurry makes gallium salt be coated on the hydrogel of water soluble polymer formation by disperseing screwing element
In network structure；Then by shearing carbonization screwing element, it is 180~240 DEG C that this section of reaction temperature, which is arranged, in shearing and high temperature
Under the conditions of so that water soluble polymer is carbonized, form the gallium salt that is coated by carbon network structure；Thermoplastic cement is added by auxiliary material mouth, if
It is 250~300 DEG C to set reaction temperature, is kneaded 10~15min of reaction, then forms thin slice by squeezing；
(3) thin slice obtained in step (2) is placed in alundum (Al2O3) crucible, is put into the middle part flat-temperature zone of tube furnace,
Dry 15~30min under 180~250 DEG C of air atmosphere；
(4) it is passed through the argon gas that flow is 50sccm into tube furnace, the temperature of tube furnace is warming up to 900~1200 DEG C,
Control heating rate be 8~20 DEG C/min, stop lead to argon gas, be passed through flow be 50~100sccm ammonia reaction 120~
150min, the logical ammonia of stopping change argon gas into and are protected, be cooled to room temperature in argon atmosphere, obtain faint yellow gallium nitride nanometer
Crystal.
Water soluble polymer described in above-mentioned steps (1) is 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.
Thermoplastic cement described in above-mentioned steps (2) is 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.
Double screw extruder described in above-mentioned steps (2), screw slenderness ratio are 40~45:1；Screw rod is from feed end to end
End is once set as dispersion 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 preparing gallium nitride nano crystal using double screw extruder of the present invention, first dissolves 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
Disperse screwing element, so that gallium salt is coated in the hydrogel network structure of water soluble polymer formation, in shearing and hot conditions
Under so that water soluble polymer is carbonized, form the gallium salt that is coated by carbon network structure；Thermoplastic cement is added 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 into inside thin slice by carbon network structure, nitridation reaction occurs with the gallium salt of package in the network architecture, makes nitridation
Gallium nanocrystal homoepitaxial in thin slice template.There is carbon network structure by the mixture thin slice that twin-screw extrusion is formed,
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, reaction nanocrystal that is fast, and generating for the gallium nitride prepared using the present invention
With preferable pattern and complete crystalline structure.
A kind of method preparing gallium nitride nano crystal using double screw extruder of the present invention, protrudes compared with prior art
The characteristics of and beneficial effect be：
1, a kind of method preparing gallium nitride nano crystal using double screw extruder of the present invention, gallium salt is coated on water-soluble
Property the hydrogel network structure that is formed of macromolecule in, reacted using twin-screw extrusion, form the gallium salt that is coated by carbon network structure
Thin slice prepares gallium nitride using thin slice as gallium source and template, increases the surface area of reactant, keeps ammonia completely fast
With gallium source nitridation reaction occurs for speed, and thin slice provides template for the growth of gallium nitride, keeps crystal uniform on thin slice
Growth forms the nanocrystal that pattern is preferable, crystalline structure is regular.
2, the gallium nitride pattern of the invention prepared 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.
3, the method provided by the invention for preparing gallium nitride nano crystal, have preparation method it is reproducible, raw material at
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 implementation mode
The present invention is explained in detail below in conjunction with specific implementation mode, 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 of a concentration of 60g/L, gallium nitrate powder is mixed
Conjunction is added in polyacrylamide solution, and the dosage of polyacrylamide is the 12% of gallium nitrate dosage；In homogenizer
It is stirred 20min with the speed of 3000rpm and obtains mixed slurry；
(2) slurry obtained in step (1) is pumped into double screw extruder charge door, setting dispersion screwing element section is anti-
It is 100 DEG C to answer temperature, and slurry makes gallium salt be coated on the hydrogel network structure of polyacrylamide formation by disperseing screwing element
In；Then by shearing carbonization screwing element, it is 240 DEG C that this section of reaction temperature, which is arranged, 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 by auxiliary material mouth to use for water soluble polymer
4% thermoplastic polyurethane of amount, setting reaction temperature are 250 DEG C, are kneaded reaction 15min, then form thin slice by squeezing；
(3) thin slice obtained in step (2) is placed in alundum (Al2O3) crucible, is put into the middle part flat-temperature zone of tube furnace,
Dry 30min under 180 DEG C of air atmosphere；
(4) it is passed through the argon gas that flow is 50sccm into tube furnace, the temperature of tube furnace is warming up to 900 DEG C, control rises
Warm rate is 8 DEG C/min, and argon gas is led in stopping, being passed through the ammonia that flow is 100sccm and reacts 120min, stops logical ammonia and change argon into
Gas is protected, and is cooled to room temperature in argon atmosphere, and faint yellow gallium nitride nano crystal is obtained.
Embodiment 2
(1) polyacrylic acid and water are configured to the polyacrylic acid aqueous solution of a concentration of 90g/L, gallium chloride powder is mixed and is added
Enter into polyacrylic acid aqueous solution, the dosage of polyacrylic acid is the 15% of gallium chloride dosage；With 3500rpm in homogenizer
Speed be stirred 15min and obtain mixed slurry；
(2) slurry obtained in step (1) is pumped into double screw extruder charge door, setting dispersion screwing element section is anti-
It is 120 DEG C to answer temperature, and slurry makes gallium salt be coated on the hydrogel network structure of polyacrylic acid formation by disperseing screwing element
In；Then by shearing carbonization screwing element, it is 200 DEG C that this section of reaction temperature, which is arranged, 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 that dosage, which is added, by auxiliary material mouth
5% thermoplastic acrylic, setting reaction temperature be 250 DEG C, be kneaded reaction 15min, then by squeeze form thin slice；
(3) thin slice obtained in step (2) is placed in alundum (Al2O3) crucible, is put into the middle part flat-temperature zone of tube furnace,
Dry 25min under 200 DEG C of air atmosphere；
(4) it is passed through the argon gas that flow is 50sccm into tube furnace, the temperature of tube furnace is warming up to 1000 DEG C, control rises
Warm rate is 10 DEG C/min, and argon gas is led in stopping, being passed through the ammonia that flow is 80sccm and reacts 120min, stops logical ammonia and change argon into
Gas is protected, and is cooled to room temperature in argon atmosphere, and faint yellow gallium nitride nano crystal is obtained.
Embodiment 3
(1) polyethylene glycol and water are configured to the Aqueous Solutions of Polyethylene Glycol of a concentration of 100g/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；In homogenizer with
The speed of 4000rpm is stirred 15min and obtains mixed slurry；
(2) slurry obtained in step (1) is pumped into double screw extruder charge door, setting dispersion screwing element section is anti-
It is 150 DEG C to answer temperature, and slurry makes gallium salt be coated on the hydrogel network structure of polyethylene glycol formation by disperseing screwing element
In；Then by shearing carbonization screwing element, it is 200 DEG C that this section of reaction temperature, which is arranged, 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 that dosage, which is added, by auxiliary material mouth
6% thermoplastic styrene butadiene rubber, setting reaction temperature be 280 DEG C, be kneaded reaction 12min, then by squeeze form thin slice；
(3) thin slice obtained in step (2) is placed in alundum (Al2O3) crucible, is put into the middle part flat-temperature zone of tube furnace,
Dry 20min under 230 DEG C of air atmosphere；
(4) it is passed through the argon gas that flow is 50sccm into tube furnace, the temperature of tube furnace is warming up to 1100 DEG C, control rises
Warm rate is 15 DEG C/min, and argon gas is led in stopping, being passed through the ammonia that flow is 60sccm and reacts 150min, stops logical ammonia and change argon into
Gas is protected, and is cooled to room temperature in argon atmosphere, and faint yellow gallium nitride nano crystal is obtained.
Embodiment 4
(1) hydroxymethyl cellulose and water are configured to the hydroxymethyl cellulose aqueous solution of a concentration of 120g/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；In height
10min is stirred with the speed of 4500rpm in fast blender and obtains mixed slurry；
(2) slurry obtained in step (1) is pumped into double screw extruder charge door, setting dispersion screwing element section is anti-
It is 150 DEG C to answer temperature, and slurry makes gallium salt be coated on the hydrogel network knot of hydroxymethyl cellulose formation by disperseing screwing element
In structure；Then by shearing carbonization screwing element, it is 180 DEG C that this section of reaction temperature, which is arranged, 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 that dosage, which is added, by auxiliary material mouth
7% thermoplastic cement of sub- dosage, setting reaction temperature are 300 DEG C, are kneaded reaction 10min, then form thin slice by squeezing；
(3) thin slice obtained in step (2) is placed in alundum (Al2O3) crucible, is put into the middle part flat-temperature zone of tube furnace,
Dry 15min under 250 DEG C of air atmosphere；
(4) it is passed through the argon gas that flow is 50sccm into tube furnace, the temperature of tube furnace is warming up to 1150 DEG C, control rises
Warm rate is 20 DEG C/min, and argon gas is led in stopping, being passed through the ammonia that flow is 50sccm and reacts 150min, stops logical ammonia and change argon into
Gas is protected, and is cooled to room temperature in argon atmosphere, and faint yellow gallium nitride nano crystal is obtained.
Embodiment 5
(1) polyethylene glycol and water are configured to the Aqueous Solutions of Polyethylene Glycol of a concentration of 120g/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；In homogenizer with
The speed of 5000rpm is stirred 10min and obtains mixed slurry；
(2) slurry obtained in step (1) is pumped into double screw extruder charge door, setting dispersion screwing element section is anti-
It is 150 DEG C to answer temperature, and slurry makes gallium salt be coated on the hydrogel network structure of polyethylene glycol formation by disperseing screwing element
In；Then by shearing carbonization screwing element, it is 200 DEG C that this section of reaction temperature, which is arranged, 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 as the 8% of polyethylene glycol dosage by auxiliary material mouth
Thermoplastic polyurethane, setting reaction temperature be 300 DEG C, be kneaded reaction 10min, then by squeeze form thin slice；
(3) thin slice obtained in step (2) is placed in alundum (Al2O3) crucible, is put into the middle part flat-temperature zone of tube furnace,
Dry 20min under 250 DEG C of air atmosphere；
(4) it is passed through the argon gas that flow is 50sccm into tube furnace, the temperature of tube furnace is warming up to 1200 DEG C, control rises
Warm rate is 20 DEG C/min, and argon gas is led in stopping, being passed through the ammonia that flow is 80sccm and reacts 120min, stops logical ammonia and change argon into
Gas is protected, and is cooled to room temperature in argon atmosphere, and faint yellow gallium nitride nano crystal is obtained.
Claims (3)
1. a kind of double screw extruder, which is characterized in that the screw slenderness ratio is 40~45:1；Screw rod is by feed end terminad
It is primary to be set as dispersion screwing element, shearing carbonization screwing element, compression screwing element, reverse-flight elements, wherein compressing
Sheet die is set between screwing element and reverse-flight elements.
2. application of the double screw extruder as described in claim 1 on preparing the gallium nitride thin slice with carbon network structure.
3. application side of the double screw extruder as described in claim 1 on preparing the gallium nitride thin slice with carbon network structure
Method, which is characterized in that including will be pumped into double screw extruder charge door containing the slurry that metal is sowed, setting dispersion screwing element
Section reaction temperature is 100~150 DEG C, and slurry makes gallium salt be coated on the water of water soluble polymer formation by disperseing screwing element
In gel network structure；Then by shearing be carbonized screwing element, be arranged this section of reaction temperature be 180~240 DEG C, shearing and
So that water soluble polymer is carbonized under hot conditions, forms the gallium salt coated by carbon network structure；Thermoplasticity is added by auxiliary material mouth
Glue, setting reaction temperature are 250~300 DEG C, are kneaded 10~15min of reaction, then form thin slice by squeezing.
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| CN201810069573.8A CN108357070B (en) | 2015-12-24 | 2015-12-24 | Double-screw extruder and application thereof |
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| CN201510978684.7A CN105502313B (en) | 2015-12-24 | 2015-12-24 | A kind of method that gallium nitride nano crystal is prepared using double screw extruder |
| CN201810069573.8A CN108357070B (en) | 2015-12-24 | 2015-12-24 | Double-screw extruder and application thereof |
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| US20110256693A1 (en) * | 2009-10-09 | 2011-10-20 | Soraa, Inc. | Method for Synthesis of High Quality Large Area Bulk Gallium Based Crystals |
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| CN100410179C (en) * | 2006-10-25 | 2008-08-13 | 国家纳米技术与工程研究院 | Method for preparing gallium nitride nano crystal using sol-gel method |
| KR101693071B1 (en) * | 2010-06-08 | 2017-01-04 | 덴카 주식회사 | Aluminium nitride substrate for circuit board and production method thereof |
| CN104629276B (en) * | 2013-11-12 | 2017-01-11 | 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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| US5409366A (en) * | 1991-06-26 | 1995-04-25 | Stork Protecon B.V. | Apparatus for processing extrudable materials |
| US20030124050A1 (en) * | 2002-01-03 | 2003-07-03 | Tapesh Yadav | Post-processed nanoscale powders and method for such post-processing |
| US20110256693A1 (en) * | 2009-10-09 | 2011-10-20 | Soraa, Inc. | Method for Synthesis of High Quality Large Area Bulk Gallium Based Crystals |
| CN102001170A (en) * | 2010-03-12 | 2011-04-06 | 北京化工大学 | High molecular material balanced extruder and axial force balancing method thereof |
| CN104009229A (en) * | 2014-05-21 | 2014-08-27 | 成都新柯力化工科技有限公司 | Lithium iron phosphate with controllable morphology and preparation method of lithium iron phosphate |
| 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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| CN108357070B (en) | 2021-09-10 |
| CN105502313B (en) | 2018-06-05 |
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