CN109265177A - Method for preparing superfine ALON transparent ceramic powder - Google Patents
Method for preparing superfine ALON transparent ceramic powder Download PDFInfo
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- CN109265177A CN109265177A CN201811202377.XA CN201811202377A CN109265177A CN 109265177 A CN109265177 A CN 109265177A CN 201811202377 A CN201811202377 A CN 201811202377A CN 109265177 A CN109265177 A CN 109265177A
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- 239000000843 powder Substances 0.000 title claims abstract description 154
- 239000000919 ceramic Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 29
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 141
- 238000000498 ball milling Methods 0.000 claims abstract description 48
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 19
- 239000011812 mixed powder Substances 0.000 claims abstract description 9
- 238000007873 sieving Methods 0.000 claims abstract description 8
- 229910052582 BN Inorganic materials 0.000 claims abstract description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910017083 AlN Inorganic materials 0.000 claims description 32
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 31
- 229910052782 aluminium Inorganic materials 0.000 claims description 16
- 239000004411 aluminium Substances 0.000 claims description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 16
- 239000008187 granular material Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 13
- 238000003837 high-temperature calcination Methods 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 238000003701 mechanical milling Methods 0.000 claims description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 239000010937 tungsten Substances 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 229910052573 porcelain Inorganic materials 0.000 claims 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 abstract description 16
- 239000002994 raw material Substances 0.000 abstract description 14
- 238000001035 drying Methods 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000003746 solid phase reaction Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- 239000000203 mixture Substances 0.000 description 10
- 239000011222 crystalline ceramic Substances 0.000 description 8
- 229910002106 crystalline ceramic Inorganic materials 0.000 description 8
- 239000011164 primary particle Substances 0.000 description 7
- 238000010586 diagram Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 229960004756 ethanol Drugs 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229960000935 dehydrated alcohol Drugs 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000008240 homogeneous mixture Substances 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000009738 saturating Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B35/62615—High energy or reactive ball milling
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Abstract
The invention relates to a method for preparing superfine ALON transparent ceramic powder, belonging to the technical field of transparent ceramic powder preparation. The method takes nano alumina powder and coarse aluminum nitride powder which is easy to store as raw materials, firstly ball-milling the coarse aluminum nitride powder to be nano-scale, then adding the nano alumina powder for continuous ball milling, and fully and uniformly mixing the alumina powder and the aluminum nitride. And drying and sieving the mixed powder subjected to ball milling, placing the powder into an alumina or boron nitride ceramic crucible, and carrying out high-temperature solid-phase reaction in a flowing nitrogen environment to obtain the ALON transparent ceramic powder. And finally, ball-milling the ALON transparent ceramic powder by using high-purity alumina balls to obtain the nanoscale ultrafine ALON transparent ceramic powder.
Description
Technical field
The invention belongs to transparent ceramic powder preparation technical fields, and in particular to a kind of to prepare ultra-fine ALON crystalline ceramics powder
The preparation method of body.
Background technique
Aluminium oxynitride (ALON) crystalline ceramics be it is a kind of have it is optically isotropic it is visible-in infrared (0.4~5 μm) light
Transparent material is learned, which possesses higher optical transmittance (> 80%) in service band, and has more excellent mechanics
Performance, intensity and hardness are close with sapphire respectively up to 600MPa and 1.85GPa.In addition it also has good high temperature resistant
Property (2142 DEG C of fusing point) and thermal shock resistance.Thus the material has potential application value in military and civilian field, such as
ALON crystalline ceramics can be applied to transparent armor, special optical window and head-shield, dental orthodontic materials, high pressure sodium vapour lamp
Pipe, electronic equipment screen etc..ALON crystalline ceramics generally use typical ceramic technique be made, by ALON material powder pass through at
Type, high temperature dense sintering are prepared.Wherein high-purity, ultra-fine ALON transparent ceramic powder is to prepare high-performance ALON crystalline ceramics
Important prerequisite.
There are mainly three types of the methods for preparing ALON crystalline ceramics powder at present, the first is with alumina powder and carbon dust for original
The carbothermic method of material, second is to use alumina powder and aluminium powder for the direct nitridation method of raw material, the third is to pass through oxidation
Aluminium powder and aluminum nitride powder directly react the solid reaction process of synthesis ALON powder.Synthesis temperature needed for first two method is higher, generally
Higher than 1700 DEG C, soaking time is also longer, typically larger than 2h.Powder granule is under high temperature long duration of action, and roughening is obvious, therefore
The obtained general partial size of ALON powder is larger, and activity is lower, is unfavorable for preparing high-performance ALON crystalline ceramics.United States Patent (USP)
US4481300 describes the method that carbon thermal reduction alumina powder prepares ALON powder, and this method is by alumina powder and quality percentage
Than the carbon dust mixing for 5.4%~7.1%, calcining obtains ALON powder, ALON powder particle size after ball milling under 1750 DEG C of high temperature
It is 0.5~5 μm.Chinese patent CN104446496A, which is disclosed, a kind of uses alumina powder and aluminium powder for the Direct-Nitridation system of raw material
The method of standby ALON powder, this method is uniformly to mix aluminium powder and alumina powder in organic solvent, then that mixture is dry,
Then sieving keeps the temperature 3h or more at 1600~1700 DEG C, ALON powder primary particle partial size obtained is greater than 10 μm, through ball milling
ALON powder diameter is less than 1 μm afterwards.Different from first two method, solid reaction process has alumina powder and aluminum nitride powder directly to react raw
It at ALON phase, is reacted without middle transition, this method prepares ALON powder with generated time is short, synthesis temperature is lower, is easy to control
The advantages such as system.Chinese patent CN101045632A disclose it is a kind of use alumina powder and aluminum nitride powder for raw material prepare ALON powder
Method, after a certain proportion of alumina powder and aluminum nitride powder are mixed, 0~60min is kept the temperature under 1600~1850 DEG C of high temperature,
The ALON powder that average grain diameter is 1~2 μm is made.
H.X.Willems et al. the phase structure of Al2O3-AlN system at high temperature is studied (Willems,
H.X.,Hendrix,M.M.R.M.,de With,G.&Metselaar,R.,Thermodynamics of Alon.II:Phase
Relations.J.Eur.Ceram.Soc., 10 (1992) 339-46.), they think when temperature is higher than 1640 DEG C, in Al2O3
It will be reacted with AlN and generate ALON phase, and Al2O3It will have a direct impact on the generation of ALON phase with AlN mixing uniformity.Generally
For, powder is thinner, can be more uniform after mixing, it selects the thinner raw material powder of partial size to be conducive to the generation of ALON powder, can effectively reduce
ALON powder synthesis temperature and shortening generated time, while the partial size of ALON powder can also be reduced.But fine grain aluminium nitride
Powder activity is high, facile hydrolysis, unsuitable long-term preservation.Coarse grained aluminum nitride powder can be used as raw material, pass through substep ball milling mixing
Mode solves the problems, such as mixing uniformity.
Summary of the invention
The present invention is intended to provide a kind of method for preparing ultra-fine ALON transparent ceramic powder, this method is with nano alumina powder
Body and the coarse granule aluminium nitride powder for being easy to save are raw material, are uniformly mixed aluminium oxide and aln raw material powder by substep ball milling
Close, then at a lower temperature, ALON powder is synthesized in the short period, the ALON powder primary particle partial size of acquisition is small, easily broken, warp
The ultra-fine ALON crystalline ceramics powder centralized particle diameter that is obtained after ball milling, median diameter≤400nm.
The technical solution adopted by the present invention is that: a method of preparing ultra-fine ALON transparent ceramic powder, including following step
It is rapid:
Step (1) carries out ball milling to coarse granule aluminium nitride powder using high purity aluminium oxide abrading-ball, obtains fine grained aluminium nitride
Powder, high purity aluminium oxide abrading-ball purity >=99.9%, coarse granule aluminium nitride purity >=99.5%；
Nano aluminium oxide powder is added in step (2) in the fine grained aluminium nitride powder, continues ball milling and obtains aluminium oxide
With the mixed powder of aluminium nitride, coarse granule alumina powder purity >=99.9%, aluminium nitride mole in the mixed powder
Content is 28%~40%；
Step (3) by the mixed powder of the aluminium oxide and aluminium nitride be sieved, then by after sieving aluminium oxide and nitridation
The mixed powder of aluminium is placed in crucible；
The crucible is put into high temperature furnace by step (4), and high-temperature calcination, high-temperature calcination temperature are carried out under flowing nitrogen environment
Degree is 1650 DEG C~1750 DEG C, and calcination time is 10~30min, obtains ALON transparent ceramic powder；
Step (5) carries out ball milling to the ALON transparent ceramic powder with high purity aluminium oxide abrading-ball, and it is saturating to obtain ultra-fine ALON
Bright ceramic powder.
Wherein, step (1) high purity aluminium oxide abrading-ball alumina content >=99.9%, the coarse granule aluminium nitride powder
Middle nitridation aluminium content >=99.5%, coarse granule aluminium nitride powder median diameter >=3 μm, in the fine grained aluminium nitride powder
Position diameter≤600nm.The ball milling is to adopt the loading of the organic solvents such as aluminium nitride material and methanol, ethyl alcohol, acetone, dimethylbenzene by oxygen
In the ball grinder for changing the production of the materials such as aluminium, zirconium oxide, nylon, 12~48h of planetary ball mill ball milling is then used.
Wherein, step (2) the nano aluminium oxide powder median diameter≤500nm, the nano aluminium oxide adding manner,
By after 12~48h of coarse grained aluminum nitride powder ball milling in step (1), suspends planetary ball mill, aluminium oxide is added in ball grinder
Powder, starting planetary ball mill continue ball milling.
Wherein, described in step (3) sieving used in sieve be 80~300 mesh, the crucible material be aluminium oxide or
Person's boron nitride.
Wherein, step (4) high temperature furnace is the high-temperature electric resistance furnace using materials such as graphite, tungsten, zirconium diborides as heater,
In the flowing nitrogen environment, the type of flow of nitrogen is nitrogen from the top of the crucible or side or lower section towards the crucible
Direction flows uniformly through.The high-temperature calcination is heated to 1650~1750 DEG C with the heating rate of 10~50 DEG C/min, soaking time
For 10~30min, then furnace cooling is cooled to room temperature.The ALON transparent ceramic powder primary particle average grain diameter is less than 1 μ
m。
Wherein, the Ball-milling Time of step (5) described mechanical milling process≤for 24 hours, position in the ultra-fine ALON transparent ceramic powder
Partial size≤400nm.
Present invention has an advantage that
(1) present invention is using the coarse granule aluminum nitride powder for being easy to save as raw material, using two step ball milling methods, make aluminium oxide and
Aln raw material powder obtain uniformly, be sufficiently mixed.
(2) raw material obtain uniformly, be sufficiently mixed on the basis of, obtain at a lower temperature, in the short period pure
The ALON phase powder of phase, the primary particle average grain diameter of powder is easily broken less than 1 μm, and the ultra-fine ALON obtained after ball milling is saturating
Bright ceramic powder centralized particle diameter, median diameter≤400nm.
Detailed description of the invention
Fig. 1 is the ultra-fine ALON transparent ceramic powder SEM figure in the embodiment of the present invention 1 after ball milling；
Fig. 2 is the ultra-fine ALON transparent ceramic powder particle diameter distribution schematic diagram in the embodiment of the present invention 1 after ball milling；
Fig. 3 is to obtain ALON powder XRD diagram in the embodiment of the present invention 3；
Fig. 4 is that the ALON powder SEM after grinding in the embodiment of the present invention 3 schemes (low power)；
Fig. 5 is that the ALON powder SEM after grinding in the embodiment of the present invention 3 schemes (high power)；
Fig. 6 is the ultra-fine ALON transparent ceramic powder XRD diagram in the embodiment of the present invention 3 after ball milling；
Fig. 7 is the ultra-fine ALON transparent ceramic powder SEM figure in the embodiment of the present invention 3 after ball milling；
Fig. 8 is the ultra-fine ALON transparent ceramic powder particle diameter distribution schematic diagram in the embodiment of the present invention 3 after ball milling.
Specific embodiment
With reference to the accompanying drawing and specific embodiment further illustrates the present invention.
Embodiment 1
With nano alumina powder (median diameter 300nm, purity >=99.99%) and aluminum nitride powder (8 μm of median diameter, it is pure
Degree >=99.7%) it is raw material.For 24 hours with planetary ball mill ball milling by aluminum nitride powder, dehydrated alcohol is ball-milling medium, and abrading-ball is high-purity
Aoxidize aluminium material.Then nano alumina powder continuation ball milling is added to obtain a homogeneous mixture for 24 hours, alumina powder and nitrogen in mixture
Change aluminium powder molar ratio is 72:28.Mixture after ball milling is placed on drying in blast drier, and for 24 hours, 80 DEG C of drying temperature dry
Mixture is crossed into 200 meshes after dry.Powder after sieving is put into alumina crucible, crucible is then placed in high temperature furnace
In, it is passed through flowing nitrogen, nitrogen flow 10L/min.Start high temperature furnace, rises to 1750 DEG C with 10 DEG C/min heating rate, heat preservation
Then 10min cools to room temperature with the furnace, obtain loose white block.White block is ground in aluminium oxide mortar, mistake
100 meshes obtain ALON powder, carry out XRD, SEM to obtained powder, laser particle size analyzer characterizes, the results showed that powder is
ALON phase does not find remaining aluminium oxide or aluminium nitride miscellaneous phase, and it is by diameter less than 1 μ that ALON powder average grain diameter, which is about 30 μm,
Discrete particles made of slightly sintering is accumulated between the primary particle of m.Then ALON is (anhydrous for 24 hours with planetary ball mill ball milling
Ethyl alcohol is ball-milling medium, and high purity aluminium oxide ball is abrading-ball) ultra-fine ALON transparent ceramic powder is obtained, powder is still ALON phase, table
Bright aluminium oxide and aluminium nitride react completely, do not have " half-cooked " phenomenon, and ultra-fine ALON transparent ceramic powder median diameter is about
360nm.Ultra-fine ALON transparent ceramic powder SEM figure in Fig. 1 embodiment of the present invention 1 after ball milling；In Fig. 2 embodiment of the present invention 1
Ultra-fine ALON transparent ceramic powder particle diameter distribution schematic diagram after ball milling.
Embodiment 2
With nano alumina powder (median diameter 500nm, purity >=99.99%) and aluminum nitride powder (10 μm of median diameter, it is pure
Degree >=99.7%) it is raw material.For 24 hours with planetary ball mill ball milling by aluminum nitride powder, dehydrated alcohol is ball-milling medium, and abrading-ball is high-purity
Aoxidize aluminium material.Then nano alumina powder continuation ball milling is added to obtain a homogeneous mixture for 24 hours, alumina powder and nitrogen in mixture
Change aluminium powder molar ratio is 72:28.Mixture after ball milling is placed on drying in blast drier, and for 24 hours, 80 DEG C of drying temperature dry
Mixture is sieved with 100 mesh sieve after dry.Powder after sieving is put into alumina crucible, crucible is then placed in high temperature furnace
In, it is passed through flowing nitrogen, nitrogen flow 10L/min.Start high temperature furnace, rises to 1700 DEG C with 10 DEG C/min heating rate, heat preservation
Then 10min cools to room temperature with the furnace, obtain loose white block.White block is ground in aluminium oxide mortar, mistake
100 meshes obtain ALON powder, carry out XRD, SEM to obtained powder, laser particle size analyzer characterizes, the results showed that powder is
ALON phase does not find remaining aluminium oxide or aluminium nitride miscellaneous phase, and it is by diameter less than 1 μ that ALON powder average grain diameter, which is about 25 μm,
Discrete particles made of slightly sintering is accumulated between the primary particle of m.Then ALON is (anhydrous for 24 hours with planetary ball mill ball milling
Ethyl alcohol is ball-milling medium, and high purity aluminium oxide ball is abrading-ball) ultra-fine ALON transparent ceramic powder is obtained, powder is still ALON phase, table
Bright aluminium oxide and aluminium nitride react completely, do not have " half-cooked " phenomenon, and ultra-fine ALON transparent ceramic powder median diameter is about
400nm。
Embodiment 3
With nano alumina powder (median diameter 200nm, purity >=99.99%) and aluminum nitride powder (5 μm of median diameter, it is pure
Degree >=99.7%) it is raw material.For 24 hours with planetary ball mill ball milling by aluminum nitride powder, dehydrated alcohol is ball-milling medium, and abrading-ball is high-purity
Aoxidize aluminium material.Then nano alumina powder continuation ball milling is added to obtain a homogeneous mixture for 24 hours, alumina powder and nitrogen in mixture
Change aluminium powder molar ratio is 72:28.Mixture after ball milling is placed on drying in blast drier, and for 24 hours, 80 DEG C of drying temperature dry
Mixture is crossed into 200 meshes after dry.Powder after sieving is put into alumina crucible, crucible is then placed in high temperature furnace
In, it is passed through flowing nitrogen, nitrogen flow 10L/min.Start high temperature furnace, rises to 1680 DEG C with 10 DEG C/min heating rate, heat preservation
Then 20min cools to room temperature with the furnace, obtain loose white block.White block is ground in aluminium oxide mortar, mistake
100 meshes obtain ALON powder, carry out XRD, SEM to obtained powder, laser particle size analyzer characterizes, the results showed that powder is
ALON phase does not find remaining aluminium oxide or aluminium nitride miscellaneous phase, and it is by diameter less than 1 μ that ALON powder average grain diameter, which is about 20 μm,
Discrete particles made of slightly sintering is accumulated between the primary particle of m.Then ALON is (anhydrous for 24 hours with planetary ball mill ball milling
Ethyl alcohol is ball-milling medium, and high purity aluminium oxide ball is abrading-ball) ultra-fine ALON transparent ceramic powder is obtained, powder is still ALON phase, table
Bright aluminium oxide and aluminium nitride react completely, do not have " half-cooked " phenomenon, and ultra-fine ALON transparent ceramic powder median diameter is about
320nm。
Claims (8)
1. a kind of method for preparing ultra-fine ALON transparent ceramic powder, which comprises the following steps:
Step (1) carries out ball milling to coarse granule aluminium nitride powder using high purity aluminium oxide abrading-ball, obtains fine grained aluminium nitride powder,
High purity aluminium oxide abrading-ball purity >=99.9%, coarse granule aluminium nitride purity >=99.5%；
Nano aluminium oxide powder is added in step (2) in the fine grained aluminium nitride powder, continues ball milling and obtains aluminium oxide and nitrogen
Change the mixed powder of aluminium, coarse granule alumina powder purity >=99.9%, aluminium nitride molar content in the mixed powder
It is 28%~40%；
The mixed powder of the aluminium oxide and aluminium nitride is sieved by step (3), then by the aluminium oxide and aluminium nitride after sieving
Mixed powder is placed in crucible；
The crucible is put into high temperature furnace by step (4), and high-temperature calcination is carried out under flowing nitrogen environment, and high-temperature calcination temperature is
1650 DEG C~1750 DEG C, calcination time is 10~30min, obtains ALON transparent ceramic powder；
Step (5) carries out ball milling to the ALON transparent ceramic powder with high purity aluminium oxide abrading-ball, obtains the transparent pottery of ultra-fine ALON
Porcelain powder.
2. the method according to claim 1 for preparing ultra-fine ALON transparent ceramic powder, it is characterised in that: step (1) institute
High purity aluminium oxide abrading-ball alumina content >=99.9% is stated, nitrogenizes aluminium content >=99.5% in the coarse granule aluminium nitride powder,
Coarse granule aluminium nitride powder median diameter >=3 μm, the fine grained aluminium nitride powder median diameter≤600nm.
3. the method according to claim 1 for preparing ultra-fine ALON transparent ceramic powder, it is characterised in that: step (2) institute
State nano aluminium oxide powder median diameter≤500nm.
4. the method according to claim 1 for preparing ultra-fine ALON transparent ceramic powder, it is characterised in that: step (3) institute
Stating crucible material is aluminium oxide or boron nitride.
5. the method according to claim 1 for preparing ultra-fine ALON transparent ceramic powder, it is characterised in that: step (4) institute
Stating high temperature furnace is the high-temperature electric resistance furnace using materials such as graphite, tungsten, zirconium diborides as heater.
6. the method according to claim 1 for preparing ultra-fine ALON transparent ceramic powder, it is characterised in that: step (4) institute
It states in flowing nitrogen environment, the type of flow of nitrogen is nitrogen from the top of the crucible or side or lower section towards the crucible side
To flowing uniformly through.
7. the method according to claim 1 for preparing ultra-fine ALON transparent ceramic powder, it is characterised in that: step (4) institute
High-temperature calcination is stated, is heated to 1650~1750 DEG C with the heating rate of 10~50 DEG C/min, soaking time is 10~30min.
8. the method according to claim 1 for preparing ultra-fine ALON transparent ceramic powder, it is characterised in that: step (5) institute
State the Ball-milling Time of mechanical milling process≤for 24 hours, the ultra-fine ALON transparent ceramic powder median≤400nm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114133252A (en) * | 2021-12-21 | 2022-03-04 | 厦门钜瓷科技有限公司 | AlON transparent ceramic shape-preserving infrared hood and preparation method thereof |
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