CN109650896B - Synthesis method of LiAlON transparent ceramic powder - Google Patents

Synthesis method of LiAlON transparent ceramic powder Download PDF

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CN109650896B
CN109650896B CN201811516233.1A CN201811516233A CN109650896B CN 109650896 B CN109650896 B CN 109650896B CN 201811516233 A CN201811516233 A CN 201811516233A CN 109650896 B CN109650896 B CN 109650896B
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lialon
transparent ceramic
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王跃忠
田猛
张荣实
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Tianjin Jinhang Institute of Technical Physics
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Abstract

The invention belongs to the technical field of synthesis and preparation of ceramic materials, and particularly relates to a synthesis method of LiAlON transparent ceramic powder. It is prepared from nano C powder and nano gamma-Al2O3Powder and self-made LiAl5O8The powder is taken as a raw material, mixed in a certain proportion, ball-milled, dried and then placed in α -Al2O3Or placing the materials in a BN crucible together into a high-temperature sintering furnace, introducing flowing nitrogen, heating to 1550-1700 ℃ at the speed of 5-10 ℃/min, preserving the heat for 1-4 h for carrying out carbothermic reduction nitridation reaction, and naturally cooling to obtain the LiAlON transparent ceramic powder. The method has low cost of raw materials, and the obtained LiAlON powder has fine granularity (the average grain diameter is not more than 800nm) and high purity (more than 99.5wt percent), and is suitable for preparing transparent ceramics.

Description

Synthesis method of LiAlON transparent ceramic powder
Technical Field
The invention belongs to the technical field of synthesis and preparation of ceramic materials, and particularly relates to a synthesis method of LiAlON transparent ceramic powder, in particular to a carbon thermal reduction nitridation synthesis method of LiAlON powder which can be used for manufacturing LiAlON transparent ceramic.
Background
AlON was discovered in the 50 th 20 th century by Yamaguchi et Al, Japan, as a cubic spinel structure material stabilized by N element 1979, McCauley et Al, USA, which used AlN, α -Al2O3The first piece of the AlON ceramic with optical transparency is prepared by a reaction sintering method. The research of the company Surmet shows that the sapphire infrared absorption film has isotropic optical performance, and the mechanical and dielectric properties are close to those of sapphire, so that the sapphire infrared absorption film has wide application prospect in the aspects of infrared windows, optical head covers, transparent armor and the like. However, AlON is thermodynamically unstable at 1640 + -10 ℃ or lower, so that the synthesis temperature is high, usually 1700 ℃ to 1800 ℃ or higher. Research shows that during AlON phase formation, doping Mg2+ or Li + can form new single-phase MgAlON or LiAlON at relatively low temperature, and the single-phase MgAlON or LiAlON has similar optical and mechanical properties to AlON. The following references are mainly reported in this respect, for example: X.Willems et al (J.Eur.Ceram.Soc.,10 (1992)), 327-. Among them, D.Clay et alRecently, RongshiZhang et Al (J.Eur. Ceram.Soc., 2018) firstly prepare high-transparency LiAlON transparent ceramic, the optical transmittance (linear transmittance) of the high-transparency LiAlON transparent ceramic is close to that of MgAlON and AlON, and the mechanical strength and hardness of the high-transparency LiAlON transparent ceramic are superior to those of MgAlON and AlON, so that the high-transparency LiAlON transparent ceramic has potential application value.
Currently, as for the preparation of LiAlON transparent ceramics, (1) a reaction sintering method, i.e., a method of reacting a Li-containing compound with AlN, &lTtT transition = α "&gTt α &/T &gTt-Al2O3Mixing, and carrying out the transparent ceramic preparation through reaction sintering (subsequent hot isostatic pressing further treatment). (2) And a two-step method, namely a method for synthesizing LiAlON powder and then sintering. For example, R.A. cutler et al (Ceramic Engineering and Science Proceedings, 2007) studies found that various compounds containing Li (e.g., Li) were selected2O、LiAlO2、LiAl5O8、LiAl11O17) Can realize the synthesis or complete conversion of LiAlON at lower temperature (1550-1650 ℃), without adding AlN and α -Al containing Li compounds2O3The system generally needs a temperature of 1750 ℃ or more to obtain pure phase AlON.2011, Wang Hao et Al (CN Pat.201110125526.9 and CNPat.201110194521.1) of Wuhan university to mix Li-containing compound, AlN and α -Al2O3The raw material system is mixed and placed in a graphite container, the LiAlON powder can be synthesized at 1400-1800 ℃ by rapidly heating the raw material system by the large current provided by a discharge plasma device, and the LiAlON transparent ceramic is prepared by the LiAlON powder.
In general, both methods have advantages and disadvantages. The reaction sintering method needs to strictly control the residual second phase and porosity in the final product, and has simple process steps but higher technical difficulty; the two-step method is premised on synthesizing LiAlON powder with high purity and fine granularity, air holes need to be reduced as much as possible in the subsequent sintering process, the process steps are slightly complicated, but the technical difficulty is relatively low. Carbothermic nitridation (i.e., C-N)2-Al2O3Or MgO-C-N2-Al2O3Raw material system) andsolid phase synthesis (i.e., AlN-Al)2O3Or MgO-AlN-Al2O3Raw material system) has been widely reported in the synthesis of AlON and MgAlON transparent ceramic powder. Wherein, the carbothermal reduction nitridation method adopts C and N with low cost2The AlN substitute has the advantage of low cost, is suitable for low-cost mass production (such as WO 02/06156), and is the hot spot of the current research. Currently, only a solid-phase synthesis method has been reported for synthesizing LiAlON powder.
Disclosure of Invention
Technical problem to be solved
The technical problem to be solved by the invention is as follows: how to provide a method which has low raw material cost and can obtain high-purity and fine-particle LiAlON powder, and the synthesized powder is suitable for manufacturing LiAlON transparent ceramics.
(II) technical scheme
In order to solve the problems of the prior art, the invention provides a method for synthesizing LiAlON transparent ceramic powder, which comprises the following steps:
the method comprises the following steps: self-made LiAl5O8Pulverizing;
step two: taking nano C powder and nano gamma-Al2O3Powder and self-made LiAl obtained in the first step5O8Mixing the powder serving as a raw material, ball-milling and drying to obtain powder A;
thirdly, taking the powder A and placing the powder A in α -Al2O3Or placing the materials in a BN crucible together into a high-temperature sintering furnace, introducing flowing nitrogen, heating to 1550-1700 ℃ at the speed of 5-10 ℃/min, preserving the heat for 1-4 h for carrying out carbothermic reduction nitridation reaction, and naturally cooling to obtain the LiAlON transparent ceramic powder.
Wherein, the self-made LiAl in the step one5O8The synthesis method of the powder is as follows: with nano gamma-Al2O3Powder with Li2CO3The powder is taken as a raw material, mixed, ball-milled and dried according to a certain mass ratio, and then placed in α -Al2O3Placing the crucible and the crucible into a muffle furnace, heating to 800-1300 ℃ in air atmosphere, calcining for 1-5 h,naturally cooling to obtain LiAl5O8And (3) pulverizing.
Wherein the mass ratio is 87.33: 12.67.
Wherein, the content of the nano C powder in the step two is 3.0 wt% -6.0 wt%, and the nano gamma-Al powder is2O365.0-80.0 wt% of powder, self-made LiAl5O8The powder content is 15.0 wt% -30.0 wt%; the nano C powder is commercially available C powder with the purity of not less than 97 wt% and the average particle size of not more than 30 nm.
Wherein the nano gamma-Al2O3The powder is commercially available gamma-Al with purity of not less than 99.5 wt% and average particle size of not more than 100nm2O3And (3) pulverizing.
Wherein, the Li2CO3The powder is commercially available Li with purity of not less than 99 wt% and average particle size of not more than 200nm2CO3And (3) pulverizing.
Wherein, the mixed ball milling and drying treatment method comprises the following steps: taking commercially available absolute ethyl alcohol (the purity is not less than 99.5 wt%) as a dispersion medium, taking commercially available high-purity alumina balls (the purity is not less than 99 wt%) as a ball milling medium, wherein the mass ratio of the balls to the powder is 5: 1-10: 1, the ball milling speed is 80-200 r/min, and the ball milling time is 16-24 h; then, after the dispersion medium is removed by drying treatment at 50-80 ℃, the mixture is sieved by a 60-mesh sieve.
Wherein, in the third step, α -Al2O3Or the BN crucible is a commercial product, and the purity is not lower than 97 wt%.
Wherein the flowing nitrogen gas is high-purity nitrogen gas flow with constant speed.
Wherein, the purity of the nitrogen is not less than 99.99 vol%, and the flow rate is 0.5L-2L/min.
(III) advantageous effects
The invention provides a novel method for obtaining LiAlON powder. The previously reported LiAlON powder synthesis methods are all solid-phase methods (using AlN and Al2O3As raw material), and no report is found on obtaining LiAlON powder by carbothermal reduction nitridation. The synthesis method of LiAlON powder reported previously is mainly the patent of Wang Hao of Wuhan university (CN Pat.201110125526.9 and CN Pa)t.201110194521.1). In contrast, the main advantages or benefits are:
1) the raw material cost is low. The nanometer AlN powder is expensive in manufacturing cost and the process is not mature. Thus, C, N was used in comparison with the solid phase method using AlN as a raw material2、Al2O3The carbon thermal reduction nitridation method which is used as a raw material has the advantage of lower raw material cost;
2) the powder has excellent sintering effect and can be used for preparing transparent ceramics. The LiAlON powder synthesized by the method is proved by sintering that the linear transmittance of the product is higher than that of the product synthesized by the previous method (CN Pat.201110125526.9 and CNPat.201110194521.1). Further reflecting the technical step of the method of the invention.
In conclusion, the carbothermic method provided by the invention has low raw material cost, and the synthesized powder has fine granularity (the average grain diameter is not more than 800nm) and high purity (more than 99.5wt percent), and can be used for preparing LiAlON transparent ceramics. Meanwhile, a new method and a technical means are provided for the preparation of the LiAlON transparent ceramic, and certain academic significance and practical value are achieved.
Drawings
Fig. 1 is an XRD pattern of LiAlON powder synthesized in case 1. The test instrument was an X-ray diffractometer (XRD, model D/max-2600, Rigaku, Japan).
FIG. 2 shows the linear transmittance of the LiAlON transparent ceramic obtained after sintering the powder. The measuring instrument used was an ultraviolet-visible spectrophotometer (model UV-2550, Shimadzu, japan).
Detailed Description
In order to make the objects, contents, and advantages of the present invention clearer, the following detailed description of the embodiments of the present invention will be made in conjunction with the accompanying drawings and examples.
In order to solve the problems of the prior art, the invention provides a method for synthesizing LiAlON transparent ceramic powder, which comprises the following steps:
the method comprises the following steps: self-made LiAl5O8Pulverizing;
step two: taking nano C powder and nano gamma-Al2O3Powder and self-made LiAl obtained in the first step5O8Mixing the powder serving as a raw material, ball-milling and drying to obtain powder A;
thirdly, taking the powder A and placing the powder A in α -Al2O3Or placing the materials in a BN crucible together into a high-temperature sintering furnace, introducing flowing nitrogen, heating to 1550-1700 ℃ at the speed of 5-10 ℃/min, preserving the heat for 1-4 h for carrying out carbothermic reduction nitridation reaction, and naturally cooling to obtain the LiAlON transparent ceramic powder.
Wherein, the self-made LiAl in the step one5O8The synthesis method of the powder is as follows: with nano gamma-Al2O3Powder with Li2CO3The powder is taken as a raw material, mixed, ball-milled and dried according to a certain mass ratio, and then placed in α -Al2O3Putting the crucible and the crucible into a muffle furnace, heating the crucible to 800-1300 ℃ in air atmosphere, calcining the crucible for 1-5 h, and naturally cooling the crucible to obtain LiAl5O8And (3) pulverizing.
Wherein the mass ratio is 87.33: 12.67.
Wherein, the content of the nano C powder in the step two is 3.0 wt% -6.0 wt%, and the nano gamma-Al powder is2O365.0-80.0 wt% of powder, self-made LiAl5O8The powder content is 15.0 wt% -30.0 wt%; the nano C powder is commercially available C powder with the purity of not less than 97 wt% and the average particle size of not more than 30 nm.
Wherein the nano gamma-Al2O3The powder is commercially available gamma-Al with purity of not less than 99.5 wt% and average particle size of not more than 100nm2O3And (3) pulverizing.
Wherein, the Li2CO3The powder is commercially available Li with purity of not less than 99 wt% and average particle size of not more than 200nm2CO3And (3) pulverizing.
Wherein, the mixed ball milling and drying treatment method comprises the following steps: taking commercially available absolute ethyl alcohol (the purity is not less than 99.5 wt%) as a dispersion medium, taking commercially available high-purity alumina balls (the purity is not less than 99 wt%) as a ball milling medium, wherein the mass ratio of the balls to the powder is 5: 1-10: 1, the ball milling speed is 80-200 r/min, and the ball milling time is 16-24 h; then, after the dispersion medium is removed by drying treatment at 50-80 ℃, the mixture is sieved by a 60-mesh sieve.
Wherein, in the third step, α -Al2O3Or the BN crucible is a commercial product, and the purity is not lower than 97 wt%.
Wherein the flowing nitrogen gas is high-purity nitrogen gas flow with constant speed.
Wherein, the purity of the nitrogen is not less than 99.99 vol%, and the flow rate is 0.5L-2L/min.
More specifically, the present invention provides a method comprising:
1)LiAl5O8and (3) preparing powder. With Li2CO3Powder, nano gamma-Al2O3The powder is taken as a raw material, mixed, ball-milled and dried according to the mass ratio of 87.33:12.67, and then placed in α -Al2O3Putting the crucible and the crucible into a muffle furnace, heating the crucible to 800-1300 ℃ in air atmosphere, calcining the crucible for 1-5 h, and naturally cooling the crucible to obtain LiAl5O8And (3) pulverizing.
Further, said Li2CO3The powder is commercially available Li with purity of not less than 99 wt% and average particle size of not more than 200nm2CO3Pulverizing; the nano gamma-Al2O3The powder is commercially available gamma-Al with purity not less than 99.5 wt% and average particle size not greater than 100nm2O3Powders, such as: product CR125 from Baikowski, France;
further, the mixed ball milling and drying treatment method comprises the following steps: the method comprises the steps of taking commercially available absolute ethyl alcohol (the purity is not lower than 99.5 wt%) as a dispersion medium, taking commercially available high-purity alumina balls (the purity is not lower than 99 wt%) as a ball milling medium, wherein the mass ratio of the balls to powder is 5: 1-10: 1, the ball milling speed is 80-200 r/min, and the ball milling time is 16-24 h. Then, after the dispersion medium is removed by drying treatment at 50-80 ℃, the mixture is sieved by a 60-mesh sieve.
2) Mixing the raw materials and ball-milling. The method comprises the steps of taking commercially available absolute ethyl alcohol (the purity is not lower than 99.5 wt%) as a dispersion medium, taking commercially available high-purity alumina balls (the purity is not lower than 99 wt%) as a ball milling medium, and enabling the mass ratio of the balls to powder to be 5: 1-10: 1. Adding raw material powder (nanometer C powder, nanometer gamma-Al powder)2O3Powder and self-made LiAl5O8Powder) and setting the ball milling rotation speed to be 80 r-200 r/min and the ball milling time to be 16 h-24 h to obtain slurry.
Further, the content of the nano C powder is 3.5 to 6.5 weight percent, and the nano gamma-Al powder is2O360.0-80.0 wt% of powder, self-made LiAl5O8The powder content is 10.0 wt% -20.0 wt%;
further, the nano-C powder is a commercial C powder with purity not lower than 97 wt% and average particle size not higher than 30nm, such as: products M700, M880 from cabot americana;
further, the nano gamma-Al2O3The powder is commercially available gamma-Al with purity not less than 99.5 wt% and average particle size not greater than 100nm2O3Powders, such as: product CR125 from Baikowski, France, product TM-300 from Taimei Chemical, Japan.
3) Drying and sieving. Drying the slurry obtained in the step 2) at 50-80 ℃ to remove a dispersion medium, and sieving the slurry by a 60-mesh sieve to obtain mixed powder.
4) Calcining and synthesizing, namely placing the mixed powder obtained in the step 3) into α -Al2O3Or placing the materials in a BN crucible together into a graphite heating furnace, introducing flowing nitrogen, heating to 1550-1700 ℃ at the speed of 5-10 ℃/min, preserving the heat for 1-4 h for carbothermic reduction reaction, and naturally cooling to obtain the LiAlON transparent ceramic powder.
Further, the α -Al2O3Or the BN crucible is a commercial product, and the purity is not lower than 97 wt%;
further, the flowing nitrogen gas refers to a high-purity nitrogen gas flow with a constant rate. Wherein, the purity of the nitrogen is not less than 99.99 vol%, and the flow rate is 0.5L-2L/min.
The present invention will be described in detail with reference to specific examples.
1.LiAlON powder synthesis case
1) Example 1
a)LiAl5O8And (3) preparing powder. With Li2CO3Powder (purity 99.5 wt%, average particle size 200 nm), nano gamma-Al2O3Taking powder (with purity of 99.9 wt% and average particle size of 20nm) as raw material, mixing, ball-milling and drying according to the mass ratio of 87.33:12.67, and placing in α -Al2O3And putting the crucible and the crucible into a muffle furnace, heating to 800 ℃ in air atmosphere, calcining for 3h, and naturally cooling to obtain LiAl5O8 powder for later use.
Further, the mixed ball milling and drying treatment method comprises the following steps: the method is characterized in that commercially available absolute ethyl alcohol is used as a dispersion medium, commercially available high-purity alumina balls are used as a ball milling medium, the mass ratio of the balls to powder is 5:1, the ball milling speed is 200r/min, and the ball milling time is 16 h. Then, after removing the dispersion medium by drying treatment at 50 ℃, the dispersion medium is sieved by a 60-mesh sieve.
b) Mixing the raw materials and ball-milling. The method is characterized in that commercially available absolute ethyl alcohol is used as a dispersion medium, commercially available high-purity alumina balls are used as a ball milling medium, and the mass ratio of the balls to the powder is 5: 1. Adding raw material powder (nanometer C powder, nanometer gamma-Al powder)2O3Powder and self-made LiAl5O8Powder), setting the ball milling rotation speed at 200r/min and the ball milling time at 16h to obtain slurry for later use.
Further, the content of the nano C powder is 3.0 wt%, and the nano gamma-Al powder is nano gamma-Al2O3The powder content is 67.0 wt%, and the self-made LiAl5O8The powder content was 30.0 wt%;
further, the purity of the nano C powder is 97.5%, and the average particle size is 30 nm; the nano gamma-Al2O3The powder had a purity of 99.9 wt% and an average particle size of 20 nm.
c) Drying and sieving. Drying the slurry obtained in the step b) at 80 ℃ to remove a dispersion medium, and sieving the slurry with a 60-mesh sieve to obtain mixed powder for later use.
d) Calcining synthesis, namely placing the mixed powder obtained in the step c) into α -Al2O3And putting the crucible and the graphite heating furnace together, introducing flowing nitrogen, heating to 1550 ℃ at the speed of 10 ℃/min, preserving heat for 4 hours, carrying out carbothermic reduction nitridation reaction, and naturally cooling to obtain the LiAlON transparent ceramic powder.
Further, the α -Al2O3The purity of the crucible is 98 wt%; the flowing nitrogen is pureThe degree was 99.995 vol%, and the flow rate was 2L/min.
2) Example 2
a)LiAl5O8And (3) preparing powder. With Li2CO3Powder (purity 99.5 wt%, average particle size 50nm), nano gamma-Al2O3Taking powder (with the purity of 99.9 wt% and the average particle size of 100nm) as a raw material, mixing, ball-milling and drying according to the mass ratio of 87.33:12.67, and placing the powder in α -Al2O3Putting the crucible and the crucible into a muffle furnace, heating to 800 ℃ in air atmosphere, calcining for 5 hours, and naturally cooling to obtain LiAl5O8And (5) pulverizing for later use.
Further, the mixed ball milling and drying treatment method comprises the following steps: the method is characterized in that commercially available absolute ethyl alcohol is used as a dispersion medium, commercially available high-purity alumina balls are used as a ball milling medium, the mass ratio of the balls to powder is 10:1, the ball milling speed is 80r/min, and the ball milling time is 24 hours. Then, after removing the dispersion medium by drying treatment at 50 ℃, the dispersion medium is sieved by a 60-mesh sieve.
b) Mixing the raw materials and ball-milling. The method is characterized in that commercially available absolute ethyl alcohol is used as a dispersion medium, commercially available high-purity alumina balls are used as a ball milling medium, and the mass ratio of the balls to the powder is 10: 1. Adding raw material powder (nanometer C powder, nanometer gamma-Al powder)2O3Powder and self-made LiAl5O8Powder), setting the ball milling speed to be 80r/min and the ball milling time to be 24h, and obtaining slurry for later use.
Further, the content of the nano C powder is 3.0 wt%, and the nano gamma-Al powder is nano gamma-Al2O380.0 wt% of powder, self-made LiAl5O8The powder content was 17.0 wt%;
further, the purity of the nano C powder is 98.5 wt%, and the average particle size is 13 nm; the nano gamma-Al2O3The powder had a purity of 99.9 wt% and an average particle size of 100 nm.
c) Drying and sieving. Drying the slurry obtained in the step b) at 80 ℃ to remove a dispersion medium, and sieving the slurry with a 60-mesh sieve to obtain mixed powder for later use.
d) And (4) calcining and synthesizing. Putting the mixed powder obtained in the step c) into a BN crucible, putting the mixed powder into a graphite heating furnace together, introducing flowing nitrogen, heating to 1600 ℃ at the speed of 6 ℃/min, preserving heat for 3 hours to carry out carbothermic reduction nitridation reaction, and naturally cooling to obtain the LiAlON transparent ceramic powder.
Further, the purity of the BN crucible is 98 wt%; the purity of the flowing nitrogen is 99.999 vol%, and the flowing speed is 0.5L/min.
3) Example 3
a)LiAl5O8And (3) preparing powder. With Li2CO3Powder (purity 99.9 wt%, average particle size 200 nm), nano gamma-Al2O3Taking powder (with purity of 99.95 wt% and average particle size of 50nm) as raw material, mixing, ball-milling and drying according to the mass ratio of 87.33:12.67, and placing in α -Al2O3Putting the crucible and the crucible into a muffle furnace, heating to 1100 ℃ in air atmosphere, calcining for 2h, and naturally cooling to obtain LiAl5O8And (5) pulverizing for later use.
Further, the mixed ball milling and drying treatment method comprises the following steps: the method is characterized in that commercially available absolute ethyl alcohol is used as a dispersion medium, commercially available high-purity alumina balls are used as a ball milling medium, the mass ratio of the balls to powder is 7:1, the ball milling speed is 150r/min, and the ball milling time is 16 h. Then, the dispersion medium was removed by drying at 65 ℃ and then sieved with a 60-mesh sieve.
b) Mixing the raw materials and ball-milling. The method is characterized in that commercially available absolute ethyl alcohol is used as a dispersion medium, commercially available high-purity alumina balls are used as a ball milling medium, and the mass ratio of the balls to the powder is 7: 1. Adding raw material powder (nanometer C powder, nanometer gamma-Al powder)2O3Powder and self-made LiAl5O8Powder), setting the ball milling rotation speed at 150r/min and the ball milling time at 16h to obtain slurry for later use.
Further, the content of the nano C powder is 4.5 wt%, and the nano gamma-Al powder is nano gamma-Al2O375.5 wt% of powder, self-made LiAl5O8The powder content was 20.0 wt%;
further, the purity of the nano C powder is 98.5 wt%, and the average particle size is 18 nm; the nano gamma-Al2O3The powder had a purity of 99.95 wt% and an average particle size of 50 nm.
c) Drying and sieving. Drying the slurry obtained in the step b) at 70 ℃ to remove a dispersion medium, and sieving the slurry with a 60-mesh sieve to obtain mixed powder for later use.
d) Calcining synthesis, namely placing the mixed powder obtained in the step c) into α -Al2O3And putting the crucible and the graphite heating furnace together, introducing flowing nitrogen, heating to 1650 ℃ at the speed of 7 ℃/min, preserving the temperature for 2h to perform carbothermic reduction nitridation reaction, and naturally cooling to obtain the LiAlON transparent ceramic powder.
Further, the α -Al2O3The purity of the crucible is 99 wt%; the purity of the flowing nitrogen gas is 99.995 vol%, and the flowing speed is 0.7L/min.
4) Example 4
a)LiAl5O8And (3) preparing powder. With Li2CO3Mixing powder (with purity of 99.9 wt% and average particle size of 100nm) and nanometer gamma-Al 2O3 powder (with purity of 99.95 wt% and average particle size of 100nm) at a mass ratio of 87.33:12.67, ball-milling, drying, and placing in α -Al2O3Putting the crucible and the crucible into a muffle furnace, heating to 1100 ℃ in air atmosphere, calcining for 4 hours, and naturally cooling to obtain LiAl5O8And (5) pulverizing for later use.
Further, the mixed ball milling and drying treatment method comprises the following steps: the method is characterized in that commercially available absolute ethyl alcohol is used as a dispersion medium, commercially available high-purity alumina balls are used as a ball milling medium, the mass ratio of the balls to powder is 8:1, the ball milling speed is 200r/min, and the ball milling time is 18 h. Then, the dispersion medium was removed by drying at 65 ℃ and then sieved with a 60-mesh sieve.
b) Mixing the raw materials and ball-milling. The method is characterized in that commercially available absolute ethyl alcohol is used as a dispersion medium, commercially available high-purity alumina balls are used as a ball milling medium, and the mass ratio of the balls to the powder is 8: 1. Adding raw material powder (nanometer C powder, nanometer gamma-Al powder)2O3Powder and self-made LiAl5O8Powder) is added, the ball milling rotating speed is set to be 200r/min, the ball milling time is set to be 18h, and slurry is obtained for later use.
Further, the content of the nano C powder is 4.5 wt%, and the nano gamma-Al powder is nano gamma-Al2O3The powder content is 65.5 wt%, and the self-made LiAl5O8The powder content was 30.0 wt%;
further, the purity of the nano C powder is 99 wt%, and the average particle size is 10 nm; the nano gamma-Al2O3The powder had a purity of 99.95 wt% and an average particle size of 100 nm.
c) Drying and sieving. Drying the slurry obtained in the step b) at 70 ℃ to remove a dispersion medium, and sieving the slurry with a 60-mesh sieve to obtain mixed powder for later use.
d) And (4) calcining and synthesizing. Placing the mixed powder obtained in the step c) into a BN crucible, then placing the mixed powder into a graphite heating furnace together, introducing flowing nitrogen, heating to 1650 ℃ at the speed of 9 ℃/min, preserving the temperature for 3 hours to carry out carbothermic reduction nitridation reaction, and naturally cooling to obtain LiAlON transparent ceramic powder
Further, the α -Al2O3The purity of the crucible is 99 wt%; the purity of the flowing nitrogen is 99.999 vol%, and the flowing speed is 1.5L/min.
5) Example 5
a)LiAl5O8And (3) preparing powder. With Li2CO3Powder (purity 99.9 wt%, average particle size 150 nm), nano gamma-Al2O3Taking powder (with purity of 99.99 wt% and average particle size of 70nm) as raw material, mixing, ball-milling and drying according to the mass ratio of 87.33:12.67, and placing in α -Al2O3Putting the crucible and the crucible into a muffle furnace, heating to 1300 ℃ in air atmosphere, calcining for 4 hours, and naturally cooling to obtain LiAl5O8And (5) pulverizing for later use.
Further, the mixed ball milling and drying treatment method comprises the following steps: the method is characterized in that commercially available absolute ethyl alcohol is used as a dispersion medium, commercially available high-purity alumina balls are used as a ball milling medium, the mass ratio of the balls to powder is 6:1, the ball milling speed is 120r/min, and the ball milling time is 20 hours. Then, after removing the dispersion medium by drying treatment at 80 ℃, the dispersion medium is sieved by a 60-mesh sieve.
b) Mixing the raw materials and ball-milling. The method is characterized in that commercially available absolute ethyl alcohol is used as a dispersion medium, commercially available high-purity alumina balls are used as a ball milling medium, and the mass ratio of the balls to the powder is 6: 1. Adding raw material powder (nanometer C powder, nanometer gamma-Al powder)2O3Powder and self-made LiAl5O8Powder) is added, the ball milling rotating speed is set to be 120r/min, and the ball milling time is set to beAnd (5) obtaining slurry for later use after 20 hours.
Further, the content of the nano C powder is 6.0 wt%, and the nano gamma-Al powder is nano gamma-Al2O374.0 wt% of powder, self-made LiAl5O8The powder content was 20.0 wt%;
further, the purity of the nano C powder is 97.5 wt%, and the average particle size is 16 nm; the nano gamma-Al2O3The powder had a purity of 99.99 wt% and an average particle size of 70 nm.
c) Drying and sieving. Drying the slurry obtained in the step b) at 50 ℃ to remove a dispersion medium, and sieving the slurry with a 60-mesh sieve to obtain mixed powder for later use.
d) Calcining synthesis, namely placing the mixed powder obtained in the step c) into α -Al2O3And putting the crucible and the graphite heating furnace together, introducing flowing nitrogen, heating to 1700 ℃ at the speed of 8 ℃/min, preserving the temperature for 1h for carrying out carbothermic reduction nitridation reaction, and naturally cooling to obtain the LiAlON transparent ceramic powder.
Further, the α -Al2O3The purity of the crucible is 98 wt%; the purity of the flowing nitrogen gas is 99.995 vol%, and the flowing speed is 1.8L/min.
6) Example 6
a)LiAl5O8And (3) preparing powder. With Li2CO3Powder (purity 99.5 wt%, average particle size 50nm), nano gamma-Al2O3Taking powder (with purity of 99.99 wt% and average particle size of 20nm) as raw material, mixing, ball-milling and drying according to the mass ratio of 87.33:12.67, and placing in α -Al2O3Putting the crucible and the crucible into a muffle furnace, heating to 1300 ℃ in air atmosphere, calcining for 1h, and naturally cooling to obtain LiAl5O8And (5) pulverizing for later use.
Further, the mixed ball milling and drying treatment method comprises the following steps: the method is characterized in that commercially available absolute ethyl alcohol is used as a dispersion medium, commercially available high-purity alumina balls are used as a ball milling medium, the mass ratio of the balls to powder is 10:1, the ball milling speed is 90r/min, and the ball milling time is 24 hours. Then, after removing the dispersion medium by drying treatment at 80 ℃, the dispersion medium is sieved by a 60-mesh sieve.
b) Mixing of raw materialsAnd (5) ball milling. The method is characterized in that commercially available absolute ethyl alcohol is used as a dispersion medium, commercially available high-purity alumina balls are used as a ball milling medium, and the mass ratio of the balls to the powder is 10: 1. Adding raw material powder (nanometer C powder, nanometer gamma-Al powder)2O3Powder and self-made LiAl5O8Powder) is added, the ball milling rotating speed is set to be 90r/min, the ball milling time is set to be 24h, and slurry is obtained for later use.
Further, the content of the nano C powder is 6.0 wt%, and the nano gamma-Al powder is nano gamma-Al2O378.0 wt% of powder, self-made LiAl5O8The powder content was 16.0 wt%;
further, the purity of the nano C powder is 99 wt%, and the average particle size is 27 nm; the nano gamma-Al2O3The powder had a purity of 99.99 wt% and an average particle size of 20 nm.
c) Drying and sieving. Drying the slurry obtained in the step b) at 50 ℃ to remove a dispersion medium, and sieving the slurry with a 60-mesh sieve to obtain mixed powder for later use.
d) And (4) calcining and synthesizing. Putting the mixed powder obtained in the step c) into a BN crucible, putting the mixed powder into a graphite heating furnace together, introducing flowing nitrogen, heating to 1700 ℃ at the speed of 5 ℃/min, preserving heat for 4h for carrying out carbothermic reduction nitridation reaction, and naturally cooling to obtain the LiAlON transparent ceramic powder.
Further, the α -Al2O3The purity of the crucible is 99 wt%; the purity of the flowing nitrogen is 99.999 vol%, and the flowing speed is 0.9L/min.
2. The implementation effect of the case is as follows:
a) LiAlON powder performance synthesized by carbothermal reduction nitridation method
The powder samples obtained in the above examples 1-6 are single-phase LiAlON powder (Table 1) by XRD analysis, a typical spectrum is shown in figure 1, and the powder purity can be determined to be higher than 99.5 wt% by combining the ICP-MS analysis result (Table 1); in addition, the ICP-MS test result (Table 1) proves that the powder contains Li element, and further proves that the powder is actually LiAlON and the content of main impurity elements is extremely low; the embodiment examples 1-6 basically cover the parameter range described in the invention, and the obtained LiAlON powder has fine particle size (the average particle size is not higher than 800 nm).
b) Effect of LiAlON powder for producing LiAlON transparent ceramic
Taking the powder samples obtained in the examples 1-6, pressing into a biscuit, placing in a graphite heating furnace, heating to 1850 ℃ at the speed of 5 ℃/min, keeping the temperature for 24 hours, grinding and polishing the prepared sample to the thickness of 2mm, wherein the linear transmittance of the obtained sample is not less than 65 percent and can reach 75 percent at most (figure 2). The linear transmittance of the obtained sample is higher than that of the previously reported method (CN Pat.201110194521.1). The LiAlON powder obtained by the method has excellent performance and is suitable for manufacturing transparent ceramics.
In conclusion, the examples prove that the method for synthesizing the LiAlON powder by the carbothermic method can be realized, the obtained powder has the advantages of fine granularity (the average grain diameter is not higher than 800nm) and high purity (not lower than 99.5 wt%), and is suitable for preparing transparent ceramics.
TABLE 1 LiAlON powder Performance test results
Figure BDA0001902037380000141
Figure BDA0001902037380000151
Fig. 1 is table 1, LiAlON powder performance test results. The information covered includes: the LiAlON powder obtained in cases 1-6 has purity, content of related elements and average particle size. In characterization test, we analyzed the phase and relative content by X-ray diffractometer (XRD, D/max-2600, Rigaku, Japan); an inductively coupled plasma mass spectrometer (ICP-MS, Agilent7700x, USA) is adopted to obtain the content of Li element and main metal impurities; the particle size of the powder particles was obtained by scanning electron microscopy (SEM, model S-4800, Hitach, Japan).
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.

Claims (9)

1. A synthesis method of LiAlON transparent ceramic powder is characterized by comprising the following steps:
the method comprises the following steps: self-made LiAl5O8Pulverizing;
step two: taking nano C powder and nano gamma-Al2O3Powder and self-made LiAl obtained in the first step5O8Mixing the powder serving as a raw material, ball-milling and drying to obtain powder A;
thirdly, taking the powder A and placing the powder A in α -Al2O3Or placing the materials in a BN crucible together into a high-temperature sintering furnace, introducing flowing nitrogen, heating to 1550-1700 ℃ at the speed of 5-10 ℃/min, preserving the heat for 1-4 h for carrying out carbothermic reduction nitridation reaction, and naturally cooling to obtain LiAlON transparent ceramic powder;
the content of the nano C powder in the second step is 3.0 to 6.0 weight percent, and the nano gamma-Al powder2O365.0-80.0 wt% of powder, self-made LiAl5O8The powder content is 15.0 wt% -30.0 wt%; the nano C powder is commercially available C powder with the purity of not less than 97 wt% and the average particle size of not more than 30 nm.
2. The method for synthesizing LiAlON transparent ceramic powder according to claim 1, wherein the self-made LiAl in step one5O8The synthesis method of the powder is as follows: with nano gamma-Al2O3Powder with Li2CO3The powder is taken as a raw material, mixed, ball-milled and dried according to a certain mass ratio, and then placed in α -Al2O3Putting the crucible and the crucible into a muffle furnace, heating the crucible to 800-1300 ℃ in air atmosphere, calcining the crucible for 1-5 h, and naturally cooling the crucible to obtain LiAl5O8And (3) pulverizing.
3. The method for synthesizing LiAlON transparent ceramic powder according to claim 2, wherein the mass ratio is 87.33: 12.67.
4. The method for synthesizing LiAlON transparent ceramic powder according to claim 1Characterized in that the nano gamma-Al2O3The powder is commercially available gamma-Al with purity of not less than 99.5 wt% and average particle size of not more than 100nm2O3And (3) pulverizing.
5. The method for synthesizing LiAlON transparent ceramic powder according to claim 2, wherein the Li is2CO3The powder is commercially available Li with purity of not less than 99 wt% and average particle size of not more than 200nm2CO3And (3) pulverizing.
6. The method for synthesizing LiAlON transparent ceramic powder according to claim 1, wherein the mixing ball milling and drying treatment method comprises the following steps: taking anhydrous ethanol with the purity not lower than 99.5 wt% on the market as a dispersion medium, taking high-purity alumina balls with the purity not lower than 99 wt% on the market as a ball milling medium, wherein the mass ratio of the balls to the powder is 5: 1-10: 1, the ball milling speed is 80 r-200 r/min, and the ball milling time is 16 h-24 h; then, after the dispersion medium is removed by drying treatment at 50-80 ℃, the mixture is sieved by a 60-mesh sieve.
7. The method for synthesizing LiAlON transparent ceramic powder according to claim 1, wherein α -Al is added in the third step2O3Or the BN crucible is a commercial product, and the purity is not lower than 97 wt%.
8. The method for synthesizing LiAlON transparent ceramic powder according to claim 1, wherein the flowing nitrogen gas is a high-purity nitrogen gas flow with a constant rate.
9. The method for synthesizing LiAlON transparent ceramic powder according to claim 8, wherein the purity of nitrogen is not less than 99.99 vol% and the flow rate is 0.5L-2L/min.
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