CN109650896A - The synthetic method of LiAlON transparent ceramic powder - Google Patents
The synthetic method of LiAlON transparent ceramic powder Download PDFInfo
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Abstract
The invention belongs to ceramic material synthesis and preparation technical fields, and in particular to a kind of synthetic method of LiAlON transparent ceramic powder.It is with nanometer C powder, nanometer γ-Al2O3Powder and self-designed L iAl5O8Powder is raw material, after certain proportion mixing and ball milling, drying process, is placed in α-Al2O3Or in BN crucible, another rise is placed into high temperature sintering furnace, is passed through flowing nitrogen, is warming up to 1550 DEG C~1700 DEG C with the rate of 5 DEG C~10 DEG C/min and is kept the temperature 1h~4h progress carbothermal reduction-nitridation reaction, after natural cooling, obtains LiAlON transparent ceramic powder.The method of the present invention cost of material is low, and the LiAlON powder granule degree obtained thin (average grain diameter is not higher than 800nm), purity is high (being higher than 99.5wt%), is adapted to production crystalline ceramics.
Description
Technical field
The invention belongs to ceramic material synthesis and preparation technical fields, and in particular to a kind of LiAlON transparent ceramic powder
Synthetic method, particularly relate to a kind of carbothermal reduction-nitridation of LiAlON powder that can be used to make LiAlON crystalline ceramics
Synthetic method,.
Background technique
AlON is the 1950s by Yamaguchi of Japan et al. discovery, it is a kind of stable by N element
Cubic spinel structure material.1979, the McCauley in the U.S. et al. used AlN, α-Al2O3For raw material, pass through reaction
Sintering process prepares first piece of optically transparent AlON ceramics.Surmet company is studies have shown that it has isotropic light
Learn performance, and mechanics, dielectric properties and sapphire are close, thus infrared window, optical dome, in terms of, tool
Have broad application prospects.However, AlON is in thermodynamic instability state, thus synthesis temperature at 1640 ± 10 DEG C or less
It is higher, usually at 1700 DEG C~1800 DEG C or more.The study found that doping Mg2+ or Li+ can be in phase in AlON phase forming process
To new single-phase MgAlON or LiAlON is formed at lower temperature, there is the optics similar with AlON, mechanical property.About
The report of this respect mainly has below with reference to document, such as: H.X.Willems et al. (J.Eur.Ceram.Soc., 10
(1992), 327-337), X.Liu et al. (J.Am.Ceram.Soc., 97 (2014), 63-66), D.Clay et al. (J.Eur.
Ceram.Soc.,26(2006),1351–1362).Wherein, D.Clay et al. is using LiAl5O8 and AlN, α-Al2O3 raw material body
It is reaction sintering method, the LiAlON crystalline ceramics of preparation has the mechanical property close with AlON.Recently, Rongshi
Zhang et al. (J.Eur. Ceram.Soc., 2018) prepares high transparency LiAlON crystalline ceramics for the first time, and optics penetrates
Performance (straight line transmittance) and MgAlON, AlON are close, and mechanical strength, hardness performance are better than MgAlON, thus have potential
Application value.
Currently, in the preparation about LiAlON crystalline ceramics, the method for use mainly has: (1) reaction sintering, i.e., will
Compound containing Li and AlN, α-Al2O3Mixing realizes transparent pottery by reaction-sintered (subsequent can hot isostatic pressing be further processed)
Porcelain preparation.(2) two-step method first synthesizes LiAlON powder, then the method being sintered.For example, R.A.Cutler et al.
(Ceramic Engineering and Science Proceedings, 2007) is the study found that choose a variety of containing Li's
Compound (such as Li2O、LiAlO2、LiAl5O8、LiAl11O17), it can (1550 DEG C~1650 DEG C) realizations at a lower temperature
The synthesis of LiAlON or completely conversion, AlN, α-Al without adding the compound containing Li2O3System, then it is generally necessary to 1750 DEG C
Or above temperature could obtain pure phase AlON.2011, Wuhan University of Technology Wanghao et al. (CN
Pat.201110125526.9 and CN Pat.201110194521.1) by compound, AlN and α-Al containing Li2O3Material system
Mixing, is placed in crystal vessel, and the high current provided by plasma discharging body device quickly heats, and 1400 DEG C~1800 DEG C
The synthesis of LiAlON powder can be achieved, and prepared LiAlON crystalline ceramics with the powder.
On the whole, two methods respectively have advantage and disadvantage.Reaction sintering needs remaining second phase in strict control final product
And the porosity, processing step is simple, but technical difficulty is larger；Two-step method is on condition that synthesize the thin LiAlON of high-purity, granularity
Powder needs to reduce stomata, the slightly aobvious complexity of processing step as far as possible in follow-up sintering process, but technical difficulty is relatively lower.
CRN method (i.e. C-N2-Al2O3Or MgO-C-N2-Al2O3Material system) and solid-phase synthesis (i.e. AlN-Al2O3Or
MgO-AlN-Al2O3Material system) there is extensive report in terms of AlON, MgAlON transparent ceramic powder synthesis.Wherein, carbon
Heat-treat C and N of the nitriding because selecting low cost2AlN is substituted, there is advantage at low cost, be relatively suitble to inexpensive mass
It produces (such as WO 02/06156), is the hot spot of current research.At present, the synthesis of LiAlON powder only has solid-phase synthesis
It is reported.
Summary of the invention
(1) technical problems to be solved
The technical problem to be solved by the present invention is how to propose that a kind of cost of material is low and can obtain high-purity, fine grained
The method of LiAlON powder is spent, and the powder synthesized is adapted to production LiAlON crystalline ceramics.
(2) technical solution
To solve prior art problem, the present invention provides a kind of synthetic method of LiAlON transparent ceramic powder, this method
The following steps are included:
Step 1: self-designed L iAl5O8Powder；
Step 2: a nanometer C powder, nanometer γ-Al are taken2O3Powder and the resulting self-designed L iAl of step 15O8Powder is raw material, mixing
Ball milling, drying process obtain powder A；
Step 3: taking powder A, is placed in α-Al2O3Or in BN crucible, another rise is placed into high temperature sintering furnace, is passed through stream
Dynamic nitrogen is warming up to 1550 DEG C~1700 DEG C with the rate of 5 DEG C~10 DEG C/min and keeps the temperature 1h~4h progress carbothermal reduction-nitridation
It reacts, after natural cooling, obtains LiAlON transparent ceramic powder.
Wherein, self-designed L iAl described in step 15O8The synthetic method of powder is such that with nanometer γ-Al2O3Powder with
Li2CO3Powder is raw material, after the ratio mixing and ball milling of certain mass ratio, drying process, is placed in α-Al2O3In crucible, further
It rises and places into Muffle furnace, 800 DEG C~1300 DEG C are warming up under air atmosphere and carries out calcining 1h~5h, after natural cooling, obtain
LiAl5O8Powder.
Wherein, the mass ratio is 87.33:12.67.
Wherein, nanometer C powder content described in step 2 is 3.0wt%~6.0wt%, nanometer γ-Al2O3Powder content is
65.0wt%~80.0wt%, self-designed L iAl5O8Powder content is 15.0 wt%~30.0wt%；The nanometer C powder is purity
Not less than the commercially available C powder that 97wt%, average grain diameter are not higher than 30nm.
Wherein, the nanometer γ-Al2O3Powder is that purity is commercially available not higher than 100nm's not less than 99.5wt%, average grain diameter
γ-Al2O3Powder.
Wherein, the Li2CO3Powder is that purity is not less than 99wt%, average particle size is not higher than the commercially available Li of 200 nm2CO3Powder.
Wherein, the mixing and ball milling, drying method are such that (purity is not less than with commercial anhydrous ethyl alcohol
It 99.5wt%) is decentralized medium, with commercially available high purity aluminium oxide ball (purity be not less than 99wt%) for ball-milling medium, ball and powder
Mass ratio is 5:1~10:1, and rotational speed of ball-mill is 80r~200r/min, and Ball-milling Time is 16h~for 24 hours；Then, through 50 DEG C~80
DEG C be dried removal decentralized medium after, then through 60 mesh be sieved.
Wherein, in the step 3, α-Al2O3Or BN crucible is commercial product, purity is not less than 97wt%.
Wherein, the flowing nitrogen refers to the High Purity Nitrogen air-flow of constant rate of speed.
Wherein, nitrogen gas purity is not less than 99.99vol%, and flow rate is 0.5L~2L/min.
(3) beneficial effect
The invention proposes a kind of new methods for obtaining LiAlON powder.The LiAlON synthesis method being previously reported
It is solid phase method (with AlN and Al2O3For raw material), and CRN method obtains LiAlON powder and has not been reported.Previously report
The LiAlON synthesis method in road, mainly patent (the CN Pat. of Wuhan University of Technology Wanghao et al.
201110125526.9 with CN Pat.201110194521.1) method.In contrast, main advantage or beneficial effect are:
1) cost of material is low.Since nano-aluminum nitride powder involves great expense, and technique is also immature.Therefore with use AlN to be former
The solid phase method of material is compared, using C, N2、Al2O3For the CRN method of raw material, have cost of material more cheap
Advantage；
2) powder sintering excellent effect can be used to make crystalline ceramics.The LiAlON powder of this method synthesis, through being sintered
Verifying, the straight line transmittance of product are higher than method (CN Pat.201110125526.9 and CN before this
Pat.201110194521.1).And then reflect the technological progress point of the method for the present invention.
To sum up, carbothermic method method proposed by the invention, cost of material is low, and the powder granule degree synthesized is thin (flat
Equal partial size can be used to make LiAlON crystalline ceramics not higher than 800nm), purity is high (being higher than 99.5wt%).Meanwhile also for
The preparation of LiAlON crystalline ceramics provides new method and technological means, has certain academic significance and practical value.
Detailed description of the invention
Fig. 1 is the LiAlON powder XRD spectrum that case 1 synthesizes.Test equipment is X-ray diffractometer (XRD, D/max-
2600 types, Rigaku, Japan).
Fig. 2 is LiAlON crystalline ceramics straight line transmittance obtained after powder sintering.Used measuring instrument is purple
Outside-visible spectrophotometer (UV-2550 type, Shimadzu, Japan).
Specific embodiment
To keep the purpose of the present invention, content and advantage clearer, with reference to the accompanying drawings and examples, to of the invention
Specific embodiment is described in further detail.
To solve prior art problem, the present invention provides a kind of synthetic method of LiAlON transparent ceramic powder, this method
The following steps are included:
Step 1: self-designed L iAl5O8Powder；
Step 2: a nanometer C powder, nanometer γ-Al are taken2O3Powder and the resulting self-designed L iAl of step 15O8Powder is raw material, mixing
Ball milling, drying process obtain powder A；
Step 3: taking powder A, is placed in α-Al2O3Or in BN crucible, another rise is placed into high temperature sintering furnace, is passed through stream
Dynamic nitrogen is warming up to 1550 DEG C~1700 DEG C with the rate of 5 DEG C~10 DEG C/min and keeps the temperature 1h~4h progress carbothermal reduction-nitridation
It reacts, after natural cooling, obtains LiAlON transparent ceramic powder.
Wherein, self-designed L iAl described in step 15O8The synthetic method of powder is such that with nanometer γ-Al2O3Powder with
Li2CO3Powder is raw material, after the ratio mixing and ball milling of certain mass ratio, drying process, is placed in α-Al2O3In crucible, further
It rises and places into Muffle furnace, 800 DEG C~1300 DEG C are warming up under air atmosphere and carries out calcining 1h~5h, after natural cooling, obtain
LiAl5O8Powder.
Wherein, the mass ratio is 87.33:12.67.
Wherein, nanometer C powder content described in step 2 is 3.0wt%~6.0wt%, nanometer γ-Al2O3Powder content is
65.0wt%~80.0wt%, self-designed L iAl5O8Powder content is 15.0 wt%~30.0wt%；The nanometer C powder is purity
Not less than the commercially available C powder that 97wt%, average grain diameter are not higher than 30nm.
Wherein, the nanometer γ-Al2O3Powder is that purity is commercially available not higher than 100nm's not less than 99.5wt%, average grain diameter
γ-Al2O3Powder.
Wherein, the Li2CO3Powder is that purity is not less than 99wt%, average particle size is not higher than the commercially available Li of 200 nm2CO3Powder.
Wherein, the mixing and ball milling, drying method are such that (purity is not less than with commercial anhydrous ethyl alcohol
It 99.5wt%) is decentralized medium, with commercially available high purity aluminium oxide ball (purity be not less than 99wt%) for ball-milling medium, ball and powder
Mass ratio is 5:1~10:1, and rotational speed of ball-mill is 80r~200r/min, and Ball-milling Time is 16h~for 24 hours；Then, through 50 DEG C~80
DEG C be dried removal decentralized medium after, then through 60 mesh be sieved.
Wherein, in the step 3, α-Al2O3Or BN crucible is commercial product, purity is not less than 97wt%.
Wherein, the flowing nitrogen refers to the High Purity Nitrogen air-flow of constant rate of speed.
Wherein, nitrogen gas purity is not less than 99.99vol%, and flow rate is 0.5L~2L/min.
More specifically, the method include that
1)LiAl5O8Powder preparation.With Li2CO3Powder, nanometer γ-Al2O3Powder is raw material, is 87.33 according to mass ratio:
After 12.67 ratio mixing and ball milling, drying process, it is placed in α-Al2O3In crucible, another rise places the air atmosphere into Muffle furnace
Under be warming up to 800 DEG C~1300 DEG C and carry out calcining 1h~5h, after natural cooling, obtain LiAl5O8Powder.
Further, the Li2CO3Powder is that purity is commercially available not higher than 200nm's not less than 99wt%, average particle size
Li2CO3Powder；Nanometer γ-the Al2O3Powder is that purity is commercially available not higher than 100nm's not less than 99.5wt%, average particle size
γ-Al2O3Powder, such as: French Baikowski Products CR125；
Further, the mixing and ball milling, drying method are such that (purity is not low with commercial anhydrous ethyl alcohol
In 99.5wt%) it is decentralized medium, with commercially available high purity aluminium oxide ball (purity is not less than 99wt%) for ball-milling medium, ball and powder
Mass ratio be 5:1~10:1, rotational speed of ball-mill is 80r~200r/min, and Ball-milling Time is 16h~for 24 hours.Then, through 50 DEG C~
After 80 DEG C of drying process removal decentralized media, then through the sieving of 60 mesh.
2) raw material mixing and ball milling.With commercial anhydrous ethyl alcohol (purity is not less than 99.5wt%) for decentralized medium, with commercially available height
Pure zirconia aluminium ball (purity be not less than 99wt%) is ball-milling medium, and the mass ratio of ball and powder is 5:1~10:1.Raw material powder is added
Body (nanometer C powder, nanometer γ-Al2O3Powder and self-designed L iAl5O8Powder) after, setting rotational speed of ball-mill is 80r~200r/min, when ball milling
Between for 16h~for 24 hours, obtain slurry.
Further, the nanometer C powder content is 3.5wt%~6.5wt%, nanometer γ-Al2O3Powder content is
60.0wt%~80.0wt%, self-designed L iAl5O8Powder content is 10.0 wt%~20.0wt%；
Further, the nanometer C powder is the commercially available C that purity is not higher than 30nm not less than 97wt%, average grain diameter
Powder, such as: Cabot Co., Ltd, the U.S. product M700, M880；
Further, the nanometer γ-Al2O3Powder is that purity is not less than 99.5wt%, average particle size is not higher than 100nm
Commercially available γ-Al2O3Powder, such as: French Baikowski Products CR125, Japan's Taimei Chemical Products
TM-300。
3) dry and sieving.By slurry obtained by step 2) after 50 DEG C~80 DEG C drying process remove decentralized medium, then pass through
The sieving of 60 mesh, obtains mixed powder.
4) calcining synthesis.Mixed powder obtained by step 3) is placed in α-Al2O3Or in BN crucible, another rise is placed to graphite
In heating furnace, it is passed through flowing nitrogen, be warming up to 1550 DEG C~1700 DEG C with the rate of 5 DEG C~10 DEG C/min and keeps the temperature 1h~4h
Carbothermic reduction reaction is carried out, after natural cooling, obtains LiAlON transparent ceramic powder.
Further, the α-Al2O3Or BN crucible is commercial product, purity is not less than 97wt%；
Further, the flowing nitrogen refers to the High Purity Nitrogen air-flow of constant rate of speed.Wherein, nitrogen gas purity is not less than
99.99vol%, flow rate are 0.5L~2L/min.
Carry out the present invention is described in detail combined with specific embodiments below.
1, LiAlON powder synthesizes case
1) example 1
a)LiAl5O8Powder preparation.With Li2CO3Powder (purity 99.5wt%, 200 nm of average particle size), nanometer γ-Al2O3Powder
(purity 99.9wt%, average particle size 20nm) is raw material, ratio mixing and ball milling, drying according to mass ratio for 87.33:12.67
After processing, it is placed in α-Al2O3In crucible, another rise is placed into Muffle furnace, and 800 DEG C are warming up under air atmosphere and is calcined
3h after natural cooling, obtains LiAl5O8 powder, spare.
Further, the mixing and ball milling, drying method are such that be situated between with commercial anhydrous ethyl alcohol for dispersion
Matter, using commercially available high purity aluminium oxide ball as ball-milling medium, the mass ratio of ball and powder is 5:1, rotational speed of ball-mill 200r/min, ball milling
Time is 16h.Then, after 50 DEG C of drying process remove decentralized medium, then through the sieving of 60 mesh.
B) raw material mixing and ball milling.Using commercial anhydrous ethyl alcohol as decentralized medium, it is situated between by ball milling of commercially available high purity aluminium oxide ball
The mass ratio of matter, ball and powder is 5:1.Material powder (nanometer C powder, nanometer γ-Al is added2O3Powder and self-designed L iAl5O8Powder) after,
Setting rotational speed of ball-mill is 200r/min, and Ball-milling Time 16h obtains slurry, spare.
Further, the nanometer C powder content is 3.0wt%, nanometer γ-Al2O3Powder content is 67.0wt%, makes by oneself
LiAl5O8Powder content is 30.0wt%；
Further, the nanometer C powder purity 97.5%, average grain diameter 30nm；Nanometer γ-the Al2O3Powder is
Purity 99.9wt%, average particle size 20nm.
C) dry and sieving.By slurry obtained by step b) after 80 DEG C of drying process remove decentralized medium, then through 60 mesh mistakes
Sieve, obtains mixed powder, spare.
D) calcining synthesis.Mixed powder obtained by step c) is placed in α-Al2O3In crucible, another rise is placed to graphite heating
In furnace, it is passed through flowing nitrogen, be warming up to 1550 DEG C with the rate of 10 DEG C/min and keeps the temperature 4h progress carbothermal reduction-nitridation reaction,
After natural cooling, LiAlON transparent ceramic powder is obtained.
Further, the α-Al2O3Crucible purity is 98wt%；The flowing nitrogen purity is
99.995vol%, flow rate 2L/min.
2) example 2
a)LiAl5O8Powder preparation.With Li2CO3Powder (purity 99.5wt%, average particle size 50nm), nanometer γ-Al2O3Powder
(purity 99.9wt%, average particle size 100nm) is raw material, according to the ratio mixing and ball milling that mass ratio is 87.33:12.67, is done
After dry processing, it is placed in α-Al2O3In crucible, another rise is placed into Muffle furnace, and 800 DEG C are warming up under air atmosphere and is calcined
5 h after natural cooling, obtain LiAl5O8Powder, it is spare.
Further, the mixing and ball milling, drying method are such that be situated between with commercial anhydrous ethyl alcohol for dispersion
Matter, using commercially available high purity aluminium oxide ball as ball-milling medium, the mass ratio of ball and powder is 10:1, rotational speed of ball-mill 80r/min, ball milling
Time is for 24 hours.Then, after 50 DEG C of drying process remove decentralized medium, then through the sieving of 60 mesh.
B) raw material mixing and ball milling.Using commercial anhydrous ethyl alcohol as decentralized medium, it is situated between by ball milling of commercially available high purity aluminium oxide ball
The mass ratio of matter, ball and powder is 10:1.Material powder (nanometer C powder, nanometer γ-Al is added2O3Powder and self-designed L iAl5O8Powder)
Afterwards, setting rotational speed of ball-mill is 80r/min, and Ball-milling Time is for 24 hours, to obtain slurry, spare.
Further, the nanometer C powder content is 3.0wt%, nanometer γ-Al2O3Powder content is 80.0wt%, makes by oneself
LiAl5O8Powder content is 17.0wt%；
Further, nanometer C powder purity 98.5wt%, the average grain diameter 13nm；Nanometer γ-the Al2O3Powder
For purity 99.9wt%, average particle size 100nm.
C) dry and sieving.By slurry obtained by step b) after 80 DEG C of drying process remove decentralized medium, then through 60 mesh mistakes
Sieve, obtains mixed powder, spare.
D) calcining synthesis.Mixed powder obtained by step c) is placed in BN crucible, another rise is placed to graphite heater furnace
In, it is passed through flowing nitrogen, 1600 DEG C is warming up to the rate of 6 DEG C/min and keeps the temperature 3h progress carbothermal reduction-nitridation reaction, it is natural
After cooling, LiAlON transparent ceramic powder is obtained.
Further, the BN crucible purity is 98wt%；The flowing nitrogen purity is 99.999vol%, stream
Dynamic rate is 0.5L/min.
3) example 3
a)LiAl5O8Powder preparation.With Li2CO3Powder (purity 99.9wt%, 200 nm of average particle size), nanometer γ-Al2O3Powder
(purity 99.95wt%, average particle size 50nm) is raw material, according to the ratio mixing and ball milling that mass ratio is 87.33:12.67, is done
After dry processing, it is placed in α-Al2O3In crucible, another rise is placed into Muffle furnace, and 1100 DEG C are warming up under air atmosphere and is forged
2h is burnt, after natural cooling, obtains LiAl5O8Powder, it is spare.
Further, the mixing and ball milling, drying method are such that be situated between with commercial anhydrous ethyl alcohol for dispersion
Matter, using commercially available high purity aluminium oxide ball as ball-milling medium, the mass ratio of ball and powder is 7:1, rotational speed of ball-mill 150r/min, ball milling
Time is 16h.Then, after 65 DEG C of drying process remove decentralized medium, then through the sieving of 60 mesh.
B) raw material mixing and ball milling.Using commercial anhydrous ethyl alcohol as decentralized medium, it is situated between by ball milling of commercially available high purity aluminium oxide ball
The mass ratio of matter, ball and powder is 7:1.Material powder (nanometer C powder, nanometer γ-Al is added2O3Powder and self-designed L iAl5O8Powder) after,
Setting rotational speed of ball-mill is 150r/min, and Ball-milling Time 16h obtains slurry, spare.
Further, the nanometer C powder content is 4.5wt%, nanometer γ-Al2O3Powder content is 75.5wt%, makes by oneself
LiAl5O8Powder content is 20.0wt%；
Further, nanometer C powder purity 98.5wt%, the average grain diameter 18nm；Nanometer γ-the Al2O3Powder
For purity 99.95wt%, average particle size 50nm.
C) dry and sieving.By slurry obtained by step b) after 70 DEG C of drying process remove decentralized medium, then through 60 mesh mistakes
Sieve, obtains mixed powder, spare.
D) calcining synthesis.Mixed powder obtained by step c) is placed in α-Al2O3In crucible, another rise is placed to graphite heating
In furnace, it is passed through flowing nitrogen, be warming up to 1650 DEG C with the rate of 7 DEG C/min and keeps the temperature 2h progress carbothermal reduction-nitridation reaction, from
So after cooling, LiAlON transparent ceramic powder is obtained.
Further, the α-Al2O3Crucible purity is 99wt%；The flowing nitrogen purity is
99.995vol%, flow rate 0.7L/min.
4) example 4
a)LiAl5O8Powder preparation.With Li2CO3Powder (purity 99.9wt%, 100 nm of average particle size), γ-Al2O3 nanosized powder
(purity 99.95wt%, average particle size 100nm) is raw material, according to the ratio mixing and ball milling that mass ratio is 87.33:12.67, is done
After dry processing, it is placed in α-Al2O3In crucible, another rise is placed into Muffle furnace, and 1100 DEG C are warming up under air atmosphere and is forged
4h is burnt, after natural cooling, obtains LiAl5O8Powder, it is spare.
Further, the mixing and ball milling, drying method are such that be situated between with commercial anhydrous ethyl alcohol for dispersion
Matter, using commercially available high purity aluminium oxide ball as ball-milling medium, the mass ratio of ball and powder is 8:1, rotational speed of ball-mill 200r/min, ball milling
Time is 18h.Then, after 65 DEG C of drying process remove decentralized medium, then through the sieving of 60 mesh.
B) raw material mixing and ball milling.Using commercial anhydrous ethyl alcohol as decentralized medium, it is situated between by ball milling of commercially available high purity aluminium oxide ball
The mass ratio of matter, ball and powder is 8:1.Material powder (nanometer C powder, nanometer γ-Al is added2O3Powder and self-designed L iAl5O8Powder) after,
Setting rotational speed of ball-mill is 200r/min, and Ball-milling Time 18h obtains slurry, spare.
Further, the nanometer C powder content is 4.5wt%, nanometer γ-Al2O3Powder content is 65.5wt%, makes by oneself
LiAl5O8Powder content is 30.0wt%；
Further, nanometer C powder purity 99wt%, the average grain diameter 10nm；Nanometer γ-the Al2O3Powder is
Purity 99.95wt%, average particle size 100nm.
C) dry and sieving.By slurry obtained by step b) after 70 DEG C of drying process remove decentralized medium, then through 60 mesh mistakes
Sieve, obtains mixed powder, spare.
D) calcining synthesis.Mixed powder obtained by step c) is placed in BN crucible, another rise is placed to graphite heater furnace
In, it is passed through flowing nitrogen, 1650 DEG C is warming up to the rate of 9 DEG C/min and keeps the temperature 3h progress carbothermal reduction-nitridation reaction, it is natural
After cooling, LiAlON transparent ceramic powder is obtained
Further, the α-Al2O3Crucible purity is 99wt%；The flowing nitrogen purity is
99.999vol%, flow rate 1.5L/min.
5) example 5
a)LiAl5O8Powder preparation.With Li2CO3Powder (purity 99.9wt%, 150 nm of average particle size), nanometer γ-Al2O3Powder
(purity 99.99wt%, average particle size 70nm) is raw material, according to the ratio mixing and ball milling that mass ratio is 87.33:12.67, is done
After dry processing, it is placed in α-Al2O3In crucible, another rise is placed into Muffle furnace, and 1300 DEG C are warming up under air atmosphere and is forged
4h is burnt, after natural cooling, obtains LiAl5O8Powder, it is spare.
Further, the mixing and ball milling, drying method are such that be situated between with commercial anhydrous ethyl alcohol for dispersion
Matter, using commercially available high purity aluminium oxide ball as ball-milling medium, the mass ratio of ball and powder is 6:1, rotational speed of ball-mill 120r/min, ball milling
Time is 20h.Then, after 80 DEG C of drying process remove decentralized medium, then through the sieving of 60 mesh.
B) raw material mixing and ball milling.Using commercial anhydrous ethyl alcohol as decentralized medium, it is situated between by ball milling of commercially available high purity aluminium oxide ball
The mass ratio of matter, ball and powder is 6:1.Material powder (nanometer C powder, nanometer γ-Al is added2O3Powder and self-designed L iAl5O8Powder) after,
Setting rotational speed of ball-mill is 120r/min, and Ball-milling Time 20h obtains slurry, spare.
Further, the nanometer C powder content is 6.0wt%, nanometer γ-Al2O3Powder content is 74.0wt%, makes by oneself
LiAl5O8Powder content is 20.0wt%；
Further, nanometer C powder purity 97.5wt%, the average grain diameter 16nm；Nanometer γ-the Al2O3Powder
For purity 99.99wt%, average particle size 70nm.
C) dry and sieving.By slurry obtained by step b) after 50 DEG C of drying process remove decentralized medium, then through 60 mesh mistakes
Sieve, obtains mixed powder, spare.
D) calcining synthesis.Mixed powder obtained by step c) is placed in α-Al2O3In crucible, another rise is placed to graphite heating
In furnace, it is passed through flowing nitrogen, be warming up to 1700 DEG C with the rate of 8 DEG C/min and keeps the temperature 1h progress carbothermal reduction-nitridation reaction, from
So after cooling, LiAlON transparent ceramic powder is obtained.
Further, the α-Al2O3Crucible purity is 98wt%；The flowing nitrogen purity is
99.995vol%, flow rate 1.8L/min.
6) example 6
a)LiAl5O8Powder preparation.With Li2CO3Powder (purity 99.5wt%, average particle size 50nm), nanometer γ-Al2O3Powder
(purity 99.99wt%, average particle size 20nm) is raw material, according to the ratio mixing and ball milling that mass ratio is 87.33:12.67, is done
After dry processing, it is placed in α-Al2O3In crucible, another rise is placed into Muffle furnace, and 1300 DEG C are warming up under air atmosphere and is forged
1h is burnt, after natural cooling, obtains LiAl5O8Powder, it is spare.
Further, the mixing and ball milling, drying method are such that be situated between with commercial anhydrous ethyl alcohol for dispersion
Matter, using commercially available high purity aluminium oxide ball as ball-milling medium, the mass ratio of ball and powder is 10:1, rotational speed of ball-mill 90r/min, ball milling
Time is for 24 hours.Then, after 80 DEG C of drying process remove decentralized medium, then through the sieving of 60 mesh.
B) raw material mixing and ball milling.Using commercial anhydrous ethyl alcohol as decentralized medium, it is situated between by ball milling of commercially available high purity aluminium oxide ball
The mass ratio of matter, ball and powder is 10:1.Material powder (nanometer C powder, nanometer γ-Al is added2O3Powder and self-designed L iAl5O8Powder)
Afterwards, setting rotational speed of ball-mill is 90r/min, and Ball-milling Time is for 24 hours, to obtain slurry, spare.
Further, the nanometer C powder content is 6.0wt%, nanometer γ-Al2O3Powder content is 78.0wt%, makes by oneself
LiAl5O8Powder content is 16.0wt%；
Further, nanometer C powder purity 99wt%, the average grain diameter 27nm；Nanometer γ-the Al2O3Powder is
Purity 99.99wt%, average particle size 20nm.
C) dry and sieving.By slurry obtained by step b) after 50 DEG C of drying process remove decentralized medium, then through 60 mesh mistakes
Sieve, obtains mixed powder, spare.
D) calcining synthesis.Mixed powder obtained by step c) is placed in BN crucible, another rise is placed to graphite heater furnace
In, it is passed through flowing nitrogen, 1700 DEG C is warming up to the rate of 5 DEG C/min and keeps the temperature 4h progress carbothermal reduction-nitridation reaction, it is natural
After cooling, LiAlON transparent ceramic powder is obtained.
Further, the α-Al2O3Crucible purity is 99wt%；The flowing nitrogen purity is
99.999vol%, flow rate 0.9L/min.
2, case implementation result:
A) the LiAlON powder characteristic of CRN method synthesis
If 1~6 gained powder sample of examples detailed above is single-phase LiAlON powder (table 1), typical spectrum through XRD analysis
As shown in Figure 1, analyzing result (table 1) in conjunction with ICP-MS, it can determine that powder purity is higher than 99.5wt%；In addition, ICP-MS is surveyed
Test result (table 1) is confirmed containing Li element in powder, further proves to be strictly LiAlON, and major impurity constituent content
It is extremely low；Case study on implementation 1~6 covers parameter area described in the invention substantially, and gained LiAlON powder granule degree is thin (flat
Equal partial size is not higher than 800nm).
B) LiAlON powder is used to make the effect of LiAlON crystalline ceramics
Gained powder sample in examples detailed above 1~6 is taken, biscuit is pressed into, is placed in graphite heater furnace, with 5 DEG C/min's
Rate is warming up to 1850 DEG C of heat preservations for 24 hours, the sample sanding and polishing prepared to 2mm thickness, and gained sample straight line transmittance is not low
In 65%, 75% (Fig. 2) can reach.Gained sample straight line transmittance, higher than method (the CN Pat. being previously reported
201110194521.1).This shows that the LiAlON powder characteristic that the present invention obtains is excellent, is suitble to production crystalline ceramics.
In conclusion example proves, a kind of method that carbothermic method synthesis LiAlON powder may be implemented in the present invention,
Gained powder granule degree thin (average grain diameter is not higher than 800nm), purity is high (being not less than 99.5wt%), are suitble to prepare transparent pottery
Porcelain.
Table 1.LiAlON powder characteristic test result
Fig. 1 is table 1.LiAlON powder characteristic test result.The information covered includes: the LiAlON that case 1~6 obtains
Powder purity and coherent element content, average grain diameter.On characterization test, we use X-ray diffractometer (XRD, D/max-
2600 types, Rigaku, Japan) analyze object phase and relative amount；Using icp ms (ICP-MS,
Agilent 7700x, the U.S.) obtain Li element and principal metal impurities content；Using scanning electron microscope (SEM, S-
4800 types, Hitach, Japan) obtain powder granule particle size.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvement and deformations can also be made, these improve and become
Shape also should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of synthetic method of LiAlON transparent ceramic powder, which is characterized in that method includes the following steps:
Step 1: self-designed L iAl5O8Powder；
Step 2: a nanometer C powder, nanometer γ-Al are taken2O3Powder and the resulting self-designed L iAl of step 15O8Powder is raw material, mixing and ball milling,
It is dried, obtains powder A；
Step 3: taking powder A, is placed in α-Al2O3Or in BN crucible, another rise is placed into high temperature sintering furnace, is passed through flowing nitrogen
Gas is warming up to 1550 DEG C~1700 DEG C with the rate of 5 DEG C~10 DEG C/min and keeps the temperature 1h~4h progress carbothermal reduction-nitridation reaction,
After natural cooling, LiAlON transparent ceramic powder is obtained.
2. the synthetic method of LiAlON transparent ceramic powder as described in claim 1, which is characterized in that described in step 1 certainly
LiAl processed5O8The synthetic method of powder is such that with nanometer γ-Al2O3Powder and Li2CO3Powder is raw material, according to certain mass ratio
After ratio mixing and ball milling, drying process, it is placed in α-Al2O3In crucible, another rise is placed into Muffle furnace, is heated up under air atmosphere
Calcining 1h~5h is carried out to 800 DEG C~1300 DEG C, after natural cooling, obtains LiAl5O8Powder.
3. the synthetic method of LiAlON transparent ceramic powder as claimed in claim 2, which is characterized in that the mass ratio is
87.33:12.67。
4. the synthetic method of LiAlON transparent ceramic powder as described in claim 1, which is characterized in that received described in step 2
Rice C powder content is 3.0wt%~6.0wt%, nanometer γ-Al2O3Powder content is 65.0wt%~80.0wt%, self-designed L iAl5O8
Powder content is 15.0wt%~30.0wt%；The nanometer C powder is that purity is not less than 97wt%, average grain diameter is not higher than 30nm
Commercially available C powder.
5. the synthetic method of LiAlON transparent ceramic powder as claimed in claim 4, which is characterized in that the nanometer γ-
Al2O3Powder is the commercially available γ-Al that purity is not higher than 100nm not less than 99.5wt%, average grain diameter2O3Powder.
6. the synthetic method of LiAlON transparent ceramic powder as claimed in claim 4, which is characterized in that the Li2CO3Powder is
Purity is not higher than the commercially available Li of 200nm not less than 99wt%, average particle size2CO3Powder.
7. the synthetic method of LiAlON transparent ceramic powder according to claim 4, which is characterized in that the mixing ball
Mill, drying method are such that with commercial anhydrous ethyl alcohol (purity is not less than 99.5wt%) for decentralized medium, with commercially available height
Pure zirconia aluminium ball (purity be not less than 99wt%) is ball-milling medium, and the mass ratio of ball and powder is 5:1~10:1, and rotational speed of ball-mill is
80r~200r/min, Ball-milling Time are 16h~for 24 hours；Then, it after 50 DEG C~80 DEG C drying process remove decentralized medium, then passes through
The sieving of 60 mesh.
8. the synthetic method of LiAlON transparent ceramic powder according to claim 1, which is characterized in that the step 3
In, α-Al2O3Or BN crucible is commercial product, purity is not less than 97wt%.
9. the synthetic method of LiAlON transparent ceramic powder according to claim 1, which is characterized in that the flowing nitrogen
Gas refers to the High Purity Nitrogen air-flow of constant rate of speed.
10. the synthetic method of LiAlON transparent ceramic powder according to claim 9, which is characterized in that nitrogen gas purity is not
Lower than 99.99vol%, flow rate is 0.5L~2L/min.
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| CN111204786A (en) * | 2020-01-16 | 2020-05-29 | 中山大学 | LiAl recovered and prepared from waste lithium ion battery5O8Method (2) |
| CN112225568A (en) * | 2020-09-22 | 2021-01-15 | 天津津航技术物理研究所 | MgLiAlON transparent ceramic for infrared optical window and preparation method thereof |
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| WO2009044399A2 (en) * | 2007-10-02 | 2009-04-09 | Lior Miller | Water-based methods for producing high green density and transparent aluminum oxynitride (alon) |
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