CN109264679A - A kind of AlN raw powder's production technology - Google Patents
A kind of AlN raw powder's production technology Download PDFInfo
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- CN109264679A CN109264679A CN201811269766.4A CN201811269766A CN109264679A CN 109264679 A CN109264679 A CN 109264679A CN 201811269766 A CN201811269766 A CN 201811269766A CN 109264679 A CN109264679 A CN 109264679A
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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
- C01B21/072—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 aluminium
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a kind of AlN raw powder's production technologies, this method is first 1:1~1:35 according to Al:N molar ratio, silicon source and nitrogen source, which are dissolved completely in solvent, mixes it uniformly, then solvent evaporated, obtained solid mixture 500~1000 DEG C of 1~9h of roasting in calcination atmosphere, then in air atmosphere 200~750 DEG C of 1~5h of decarburization to get arrive high-purity AlN powder；Wherein source of aluminium is aluminium chlorohydrate, aluctyl, aluminum glycinate, aluminum stearate etc., the nitrogen source is guanidine hydrochloride, guanidine acetate, chitosan, 1,10- Phen etc., the solvent is deionized water, methanol, ethyl alcohol, ethyl acetate, acetone, ether, benzene, any one in toluene, and the calcination atmosphere is nitrogen, ammonia, argon gas, one or two kinds of in helium.Compared with traditional AlN preparation method, the method for the present invention has many advantages, such as that reactant range is wide, environmental friendly, easy to operate, product purity is high, low in cost.
Description
Technical field
The invention belongs to technical field of material, and in particular to a method of prepare AlN powder.
Background technique
Aluminium nitride (AlN) is iii-v covalent compound, belongs to the diamond-like nitrogen of hexagonal crystal system wurtzite structure crystal form
Compound.Its room temperature intensity height (is Al2O35 times or more), thermal expansion coefficient is small, can increase substantially plastics and silicon rubber
Thermal conductivity is good heat shock resistance material；The ability of resist melt metal attack is strong, is founding pure iron, aluminum or aluminum alloy ideal
Crucible material；With excellent electrical insulating property, resistivity is up to 426 Ω cm, and dielectric properties are good, is large-scale integrated electricity
Road, semiconductor module circuit and high power device ideal heat sink material and encapsulating material；With good injection moulding performance,
Good with semiconductor silicon matching for composite material, interface compatibility is good, can be improved composite material mechanical performance and thermally conductive Jie
Electrical property.In recent years, the extensive concern of researcher and industry is received.
The primary synthetic methods of aluminium nitride have: 1) Al2O3Carbothermic method；2) self-propagating high-temperature method；3) water causes solid phase hair
Ying Fa；4) sol-gel method；5) chemical vapour deposition technique；6) Pechini method of key containing AlN；7) aluminium powder direct nitridation method.Its
In, Al2O3Carbothermic method is most widely used in the industrial production at present, and the comparison for studying it progress is goed deep into.In the method
Prepare and be commonly incorporated into calcium oxide, calcirm-fluoride, yttrium oxide etc. in aluminium nitride powder as catalyst, wherein plus calcirm-fluoride more effectively drop
Low-activation energy improves reaction rate.The aluminium nitride powder purity is high of this method preparation, forming and sintering character are good, but synthesize
Temperature is high, and the reaction time is long, and powder granularity is larger.
Komeya et al. (Synthesis of spherical AlN particles by gas-reduction-
Nitridation method, Journal of the European Ceramic Society, 2002,22,521-526) report
A kind of method of synthesizing spherical AlN particle in road, in tube furnace, with spherical Al2O3Particle is raw material, with NH3And propane
(C3H8) gaseous mixture be reactant gas, carried out at 1200~1500 DEG C reduction nitration reaction synthesized spherical AlN particle, and
And the form of AlN powder can be controlled by the form of specified feedstock.But the NH that this method uses3/C3H8Mixed gas cost
Compared with high, danger coefficient is big, it is gases used burn into reaction temperature easily carried out to equipment reach 1500 DEG C so that energy consumption of reaction is high, at
This is big, is unfavorable for industrialized production.Fukushima et al. (Kinetics of microwave synthesis of AlN by
carbothermal-reduction-nitridation at low temperature,The American Ceramic
Society, 2018, DOI:10.1111/jace.15903) microwave assisting method is utilized, with Al2O3: C molar ratio is the mixing of 1:10
Object is raw material, N2In atmosphere, submicron order AlN particle is successfully synthesized at a temperature of 1200 DEG C.This method although avoid using
The NH of higher cost3Gas, the introducing of microwave assisting method is so that reaction temperature reduces, but this method is due to the auxiliary bring of wave
Radiation is unfavorable for the health of the producer.
Although there are the high requirements on the equipment, work in conclusion existing method and technology are successfully prepared for AlN powder
Skill process is not environmentally, preparation temperature is badly in need of inventing a kind of prepare compared with the deficiencies such as high, energy consumption is high, product granularity is big, purity is low
The method of AlN powder.
Summary of the invention
The purpose of the present invention is for synthesis temperature present in the synthesis of existing aluminium nitride is high, the reaction time is long, technique is multiple
Miscellaneous, the problems such as product granularity is big, purity is low, provides a kind of method for preparing high-purity AlN powder at a lower temperature.
It to achieve the goals above, will the present invention adopts the following technical scheme: being 1:1~1:35 according to Al:N molar ratio
Silicon source and nitrogen source are dissolved completely in solvent, then solvent evaporated, and obtained solid mixture is 500~1000 DEG C in calcination atmosphere
1~9h is roasted, then 200~750 DEG C of 1~5h of decarburization in air atmosphere, obtain high-purity AlN powder.
Above-mentioned silicon source is aluminium chlorohydrate, aluctyl, aluminum glycinate, aluminum foil stearate, aluminum nitrate, aluminium carbonate, isopropanol
It is aluminium, aluminum acetate, any one in basic aluminium acetate, preferably aluminium chlorohydrate, aluctyl, aluminum glycinate, any in aluminum foil stearate
It is a kind of.
Above-mentioned nitrogen source be guanidine hydrochloride, guanidine acetate, chitosan, 1,10- Phen, urea, melamine, ammonium nitrate,
Any one in ammonium chloride, preferably guanidine hydrochloride, guanidine acetate, chitosan, any one in 1,10- Phen.
Above-mentioned solvent is deionized water, methanol, ethyl alcohol, ethyl acetate, acetone, ether, benzene, any one in toluene,
It is preferred that any one in deionized water, methanol, ethyl alcohol.
In above-mentioned preparation method, the molar ratio of Al:N is 1:5~1:20 preferably in silicon source and nitrogen source.
In above-mentioned preparation method, the calcination atmosphere is nitrogen, ammonia, helium, any one in argon gas or two kinds.
In above-mentioned preparation method, obtained solid mixture 800~900 DEG C of 1~3h of roasting preferably in calcination atmosphere.
In above-mentioned preparation method, 550~700 DEG C of 3~5h of decarburization preferably in air atmosphere.
In above-mentioned preparation method, the particle size distribution range of gained AlN powder is in 5~20nm.
The raw materials used in the present invention is cheap and easy to get, and preparation method is simple, and reaction temperature is lower, environmental-friendly, and the AlN prepared
Powder purity is high, has industrial applications prospect.
Detailed description of the invention
Fig. 1 is the XRD diagram of AlN powder prepared by embodiment 1.
Specific embodiment
Invention is further described in detail with reference to the accompanying drawings and examples, but protection scope of the present invention not only limits
In these embodiments.
Aluminium chlorohydrate (chemical formula, AlCl3·6H2O), No. CAS: 7784-13-6.
Aluctyl (molecular formula, C9H15AlO9), No. CAS: 18917-91-4.
Aluminum foil stearate (molecular formula, C54H105AlO6), No. CAS: 637-12-7.
Aluminum glycinate (molecular formula, C2H6AlNO4), No. CAS: 13682-92-3.
Guanidine hydrochloride (molecular formula, CH6ClN3), No. CAS: 50-01-1.
Guanidine acetate (molecular formula, C3H7N3O2), No. CAS: 352-97-6.
1,10- Phen (molecular formula, C12H8N2), No. CAS: 66-71-7.
Chitosan (molecular formula, C6H11NO4X2), No. CAS: 9012-76-4.
Ethyl alcohol (molecular formula, C2H6O), No. CAS: 64-17-5.
Methanol (molecular formula, CH4O), No. CAS: 67-56-1.
Embodiment 1
It is 1:18 according to Al:N molar ratio, weighs 2.4143g (0.01mol) AlCl respectively3·6H2O and 5.7318g
(0.06mol) guanidine hydrochloride is completely dissolved in 15mL ethyl alcohol, is then evaporated ethyl alcohol at 80 DEG C, by obtained solid mixture in nitrogen
800 DEG C of roasting 2h in gas atmosphere, then 550 DEG C of decarburization 3h in air atmosphere, naturally cool to room temperature, obtain AlN powder.
As seen from Figure 1, the XRD diffraction maximum of gained AlN powder is consistent with standard diffraction peak, shows the purity of prepared AlN
It is high.It using the size that Debye-Scherrer formula calculates AlN crystal is 9.4nm in the diffraction maximum position that 2 θ values are 33 °, i.e.,
Indicate the mean particle size in 33 ° of vertical direction crystal.
Embodiment 2
It is 1:24 according to Al:N molar ratio, weighs 2.4143g (0.01mol) AlCl respectively3·6H2O and 7.6424g
(0.08mol) guanidine hydrochloride is completely dissolved in 15mL methanol, is then evaporated methanol at 70 DEG C, by obtained solid mixture in nitrogen
800 DEG C of roasting 2.5h in atmosphere, then 550 DEG C of decarburization 1h in air atmosphere, naturally cool to room temperature, obtain crystalline size and are
The AlN powder of 8.6nm.
Embodiment 3
It is 1:15 according to Al:N molar ratio, weighs 2.4143g (0.01mol) AlCl respectively3·6H2O and 5.8555g
(0.05mol) guanidine acetate is completely dissolved in 15mL deionized water, is then evaporated deionized water at 100 DEG C, obtained solid is mixed
Close object 850 DEG C of roasting 1h, then 550 DEG C of decarburizations in air atmosphere in the mixed atmosphere that ammonia and helium volume ratio are 1:9
3h naturally cools to room temperature, obtains the AlN powder that crystalline size is 15.9nm.
Embodiment 4
It is 1:18 according to Al:N molar ratio, weighs 2.9419g (0.01mol) aluctyl and 5.7318g (0.06mol) respectively
Guanidine hydrochloride is completely dissolved in 15mL ethyl alcohol, is then evaporated ethyl alcohol at 80 DEG C, by obtained solid mixture 800 in nitrogen atmosphere
DEG C roasting 3h, then 650 DEG C of decarburization 2h in air atmosphere, naturally cool to room temperature, obtain crystalline size be 9.2nm AlN
Powder.
Embodiment 5
It is 1:27 according to Al:N molar ratio, weighs 2.9419g (0.01mol) aluctyl and 10.5399g respectively
(0.09mol) guanidine acetate is completely dissolved in 15mL methanol, is then evaporated methanol at 70 DEG C, by obtained solid mixture in ammonia
With 900 DEG C of roasting 2h in mixed atmosphere that helium volume ratio is 1:9, then 550 DEG C of decarburization 1h, natural cooling in air atmosphere
To room temperature, the AlN powder that crystalline size is 19.7nm is obtained.
Embodiment 6
It is 1:1 according to Al:N molar ratio, weighs 2.9419g (0.01mol) aluctyl and 1.6116g (0.01mol) respectively
Chitosan point is dissolved in 15mL deionized water, is then evaporated deionized water at 100 DEG C, by obtained solid mixture ammonia with
Nitrogen volume ratio is 850 DEG C of roasting 1h in the mixed atmosphere of 2:98, then 600 DEG C of decarburization 2h, natural cooling in air atmosphere
To room temperature, the AlN powder that crystalline size is 17.6nm is obtained.
Embodiment 7
It is 1:30 according to Al:N molar ratio, weighs 8.7740g (0.01mol) aluminum stearate and 9.5530g respectively
(0.10mol) guanidine hydrochloride is completely dissolved in 25mL deionized water, is then evaporated deionized water at 100 DEG C, obtained solid is mixed
Close object 900 DEG C of roasting 3h, then 600 DEG C of decarburizations in air atmosphere in the mixed atmosphere that ammonia and nitrogen volume ratio are 2:98
4h naturally cools to room temperature, obtains the AlN powder that crystalline size is 20.0nm.
Embodiment 8
It is 1:27 according to Al:N molar ratio, weighs 8.7740g (0.01mol) aluminum stearate and 10.5399g respectively
(0.09mol) guanidine acetate is completely dissolved in 30mL deionized water, is then evaporated deionized water at 100 DEG C, obtained solid is mixed
Close object 900 DEG C of roasting 3h, then 700 DEG C of decarburizations in air atmosphere in the mixed atmosphere that ammonia and nitrogen volume ratio are 2:98
4h naturally cools to room temperature, obtains the AlN powder that crystalline size is 10.0nm.
Embodiment 9
It is 1:18 according to Al:N molar ratio, weighs 3.4515g (0.01mol) aluminum glycinate and 5.7318g respectively
(0.06mol) guanidine hydrochloride is completely dissolved in 15mL ethyl alcohol, is then evaporated ethyl alcohol at 80 DEG C, by obtained solid mixture in nitrogen
800 DEG C of roasting 2h in atmosphere, then 600 DEG C of decarburization 2h in air atmosphere, naturally cool to room temperature, obtain crystalline size and are
The AlN powder of 7.6nm.
Embodiment 10
It is 1:10 according to Al:N molar ratio, weighs 3.4515g (0.01mol) aluminum glycinate and 9.0105g respectively
(0.05mol) 1,10- Phen is completely dissolved in 15mL methanol, is then evaporated methanol at 70 DEG C, obtained solid is mixed
Object 800 DEG C of roasting 3h, then 650 DEG C of decarburizations in air atmosphere in the mixed atmosphere that ammonia and nitrogen volume ratio are 2:98
3h naturally cools to room temperature, obtains the AlN powder that crystalline size is 10.3nm.
Claims (9)
1. a kind of AlN raw powder's production technology, it is characterised in that: according to Al:N molar ratio be 1:1~1:35, by silicon source and nitrogen source
It is dissolved completely in solvent, then solvent evaporated, obtained solid mixture 500~1000 DEG C of 1~9h of roasting in calcination atmosphere,
Then 200~750 DEG C of 1~5h of decarburization in air atmosphere obtain high-purity AlN powder；
Above-mentioned silicon source is aluminium chlorohydrate, aluctyl, aluminum glycinate, aluminum foil stearate, aluminum nitrate, aluminium carbonate, aluminium isopropoxide, vinegar
Any one in sour aluminium, basic aluminium acetate；
Above-mentioned nitrogen source is guanidine hydrochloride, guanidine acetate, chitosan, 1,10- Phen, urea, melamine, ammonium nitrate, chlorination
Any one in ammonium；
Above-mentioned calcination atmosphere is nitrogen, ammonia, helium, any one in argon gas or two kinds.
2. AlN raw powder's production technology according to claim 1, it is characterised in that: the silicon source be aluminium chlorohydrate,
Aluctyl, aluminum glycinate, any one in aluminum foil stearate.
3. AlN raw powder's production technology according to claim 1, it is characterised in that: the nitrogen source is guanidine hydrochloride, acetic acid
Guanidine, chitosan, any one in 1,10- Phen.
4. AlN raw powder's production technology according to claim 1, it is characterised in that: Al:N in source of aluminium and nitrogen source
Molar ratio 1:5~1:20.
5. AlN raw powder's production technology according to claim 1, it is characterised in that: the solvent is deionized water, first
Alcohol, ethyl alcohol, ethyl acetate, acetone, ether, benzene, any one in toluene.
6. AlN raw powder's production technology according to claim 5, it is characterised in that: the solvent is deionized water, first
Any one in alcohol, ethyl alcohol.
7. AlN raw powder's production technology according to claim 1, it is characterised in that: obtained solid mixture is in roasting gas
800~900 DEG C of 1~3h of roasting in atmosphere.
8. AlN raw powder's production technology according to claim 1, it is characterised in that: 550~700 DEG C in air atmosphere
3~5h of decarburization.
9. AlN raw powder's production technology described in any one according to claim 1~8, it is characterised in that: gained AlN powder
Particle size distribution range be 5~20nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110228817A (en) * | 2019-06-10 | 2019-09-13 | 陕西师范大学 | A method of preparing a nanometer cyanogen ammonification indium powder |
| CN110642304A (en) * | 2019-10-09 | 2020-01-03 | 上海师范大学 | Trimetal nitride material for super capacitor and preparation method thereof |
| CN111732084A (en) * | 2020-06-23 | 2020-10-02 | 济南大学 | Method for preparing porous aluminum nitride metamaterial by utilizing two-dimensional carbon nitride template growth |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110228817A (en) * | 2019-06-10 | 2019-09-13 | 陕西师范大学 | A method of preparing a nanometer cyanogen ammonification indium powder |
| CN110642304A (en) * | 2019-10-09 | 2020-01-03 | 上海师范大学 | Trimetal nitride material for super capacitor and preparation method thereof |
| CN110642304B (en) * | 2019-10-09 | 2021-12-31 | 上海师范大学 | Trimetal nitride material for super capacitor and preparation method thereof |
| CN111732084A (en) * | 2020-06-23 | 2020-10-02 | 济南大学 | Method for preparing porous aluminum nitride metamaterial by utilizing two-dimensional carbon nitride template growth |
| CN111732084B (en) * | 2020-06-23 | 2021-11-09 | 济南大学 | Method for preparing porous aluminum nitride supercapacitor material by utilizing two-dimensional carbon nitride template growth |
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