CN113149651A - High-energy ball milling and SPS sintering CaLa2S4Preparation method of infrared transparent ceramic - Google Patents
High-energy ball milling and SPS sintering CaLa2S4Preparation method of infrared transparent ceramic Download PDFInfo
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- 238000005245 sintering Methods 0.000 title claims abstract description 58
- 239000000919 ceramic Substances 0.000 title claims abstract description 57
- 238000000713 high-energy ball milling Methods 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title description 29
- 239000000843 powder Substances 0.000 claims abstract description 43
- 238000002360 preparation method Methods 0.000 claims abstract description 28
- 229910017586 La2S3 Inorganic materials 0.000 claims abstract description 20
- 239000011261 inert gas Substances 0.000 claims abstract description 18
- 238000002834 transmittance Methods 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 13
- 239000010439 graphite Substances 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000005498 polishing Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical group CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 36
- 239000002245 particle Substances 0.000 claims description 11
- 238000000498 ball milling Methods 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 3
- 238000002490 spark plasma sintering Methods 0.000 abstract description 14
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 5
- 238000000465 moulding Methods 0.000 abstract description 2
- 239000012298 atmosphere Substances 0.000 description 7
- 238000001035 drying Methods 0.000 description 6
- 244000137852 Petrea volubilis Species 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 229910003460 diamond Inorganic materials 0.000 description 5
- 239000010432 diamond Substances 0.000 description 5
- 238000007731 hot pressing Methods 0.000 description 5
- 239000008188 pellet Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 238000001513 hot isostatic pressing Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
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- 238000005987 sulfurization reaction Methods 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
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- 238000001272 pressureless sintering Methods 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 238000004073 vulcanization Methods 0.000 description 2
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 240000002329 Inga feuillei Species 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000005387 chalcogenide glass Substances 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
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- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 description 1
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- 238000003331 infrared imaging Methods 0.000 description 1
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- 229910000341 lead(IV) sulfide Inorganic materials 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
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Abstract
The invention relates to the technical field of new material preparation, in particular to high-energy ball milling and Spark Plasma Sintering (SPS) sintering CaLa2S4The preparation method of the infrared transparent ceramic comprises the following steps: (1) under the protection of inert gas, adding CaS and La2S3Mixing the powder according to a certain proportion, and performing high-energy ball milling to obtain CaLa2S4Powder; (2) the obtained CaLa2S4The powder is wrapped by graphite paper and then is sintered by discharge plasma in a vacuum state; (3) after sintering, the obtained block CaLa2S4Polishing the ceramic to obtain CaLa2S4An infrared transparent ceramic. The inventionThe preparation method utilizes high-energy ball milling and spark plasma sintering to realize ceramic molding, and prepares the CaLa with high hardness, high transmittance and high corrosion resistance2S4An infrared transparent ceramic.
Description
Technical Field
The invention relates to the technical field of new material preparation, in particular to high-energy ball milling and SPS sintering CaLa2S4A preparation method of infrared transparent ceramics.
Background
With the establishment of 'sky-sky integration and attack-defense combination' strategic targets in China, infrared optical systems such as infrared imaging and infrared guidance are increasingly important in modern battlefields, especially in military fields such as night information reconnaissance, air attack, air defense combat and the like, and windows and fairings are key components for ensuring whether the systems can work normally or not. Because high speed flight devices are subjected to harsh environmental conditions during flight, the window and fairing materials selected are transparent in the desired infrared region, and are also required to have high mechanical strength, high temperature and thermal shock resistance, resistance to wind, sand, rain and chemical corrosion, and to maximize the transmission of radiation from the target. The commonly used long-wave infrared materials mainly comprise single crystal Ge, polycrystal ZnS, ZnSe, GaAs, chalcogenide glass and the like, however, the materials have the defects of poor corrosion resistance, high thermal conductivity, low hardness and the like under severe environment, so that the development of the high-hardness sand-erosion-rain-erosion-resistant long-wave infrared optical material is urgently needed.
Recent studies have shown that γ -La2S3Has good transmittance in the 2.5-14 μm band and hardness (670 kg/mm)2) Is far higher than ZnSe and ZnS, and is an ideal window material for substituting ZnSe and ZnS in the next-generation long-wave infrared band. However, γ -La2S3Belongs to a high-temperature phase, and has poor phase stability when a melt is cooled, namely gamma-La2S3Has a body centered cubic Th3P4A structural configuration which can also be consideredIs a compound of La2S3And La3S4Solid solutions of the same. Due to gamma-La2S3High melting point (2100 ℃) and La at high temperature3+High affinity to O to obtain pure phase gamma-La2S3Powder and hot pressing preparation of gamma-La2S3Transparent polycrystalline materials still have many key problems which are difficult to solve, and are easy to convert into beta-La especially at high temperature2S3Is an important problem for restricting the preparation of the material.
CaLa2S4As an alternative window material to ZnS, its superior mechanical properties, better corrosion resistance and longer transmission wavelength range (up to 14 μm) in the Long Wave Infrared (LWIR) window. CaLa2S4The transparent ceramic not only has the characteristic of transparency from visible light to long-wave infrared light, but also has the advantages of high hardness, high temperature resistance and sand erosion and rain erosion resistance, and has important application in the aspects of multiband imaging systems and new-generation missile fairings. CaLa2S4The research on the infrared transparent ceramics mainly focuses on CaLa2S4Preparation of both powder and transparent ceramics, CaLa2S4The method for preparing the powder mainly comprises a precursor sulfurization method, a nitrate codeposition method, an alkoxide sulfurization method, an evaporative thermal decomposition method, a solution combustion method, a mixed oxide method and the like. In 1981, White et al [ White W, et al SPIE 1981; 297,38-43]Reports that La (OH)3And CaCO3By H2Preparation of CaLa by S-sulfurization method2S4Powder, which takes 3-7 days and the particle size formed is large (5-20 μm). The spray pyrolysis method (solution evaporation thermal decomposition method) developed later can obtain particles with smaller size, and is favorable for improving the compactness. In 1992, Tsai et al [ Tsai M S, script Metallurgica et Materialia,1995,32:713-]A precursor sulfidation process is reported, with La (OH)3And CaCO3Dissolved in HNO3Then (NH) is added slowly4)2CO3Stirring, drying the precipitate to obtain precursor, and placing into a tube furnace for use with CS2Vulcanization gave a CaLaS powder (La/Ca 15). Li Huanwang et al, northwest university of industry [ CN108715550A]Invent ingA method for preparing CaLaS powder and infrared ceramic by using CS2For La (OH) CO3·n(H2O) powder vulcanization to obtain dry LaS2And (3) powder. In 2016, Wu et al university of Alfred [ Li Y, et al RSC Advances,2016,6,34935-]Nanoscale CaLa2S4 powder was synthesized by wet chemistry.
The preparation of the CaLa2S4 ceramic mainly comprises an atmosphere hot pressing sintering method, an atmosphere pressureless sintering and vacuum hot pressing sintering method, a hot isostatic pressing sintering method and an electric field auxiliary sintering method. Micron-sized CaLa obtained by adopting carbonate precipitation method through atmosphere hot pressing sintering method2S4Sintering the powder at 1000 ℃ and 120MPa for 6h to obtain translucent CaLa2S4A ceramic. The hot isostatic pressing sintering method adopts CaLa doped with a small amount of PbS2S4Powder is firstly prepared from H2Pressureless sintering is carried out for 4-8 h under the S atmosphere at 1350 ℃, and then hot isostatic pressing sintering is carried out for 1h under the argon atmosphere at the pressure of 200MPa to obtain black semitransparent CaLa2S4A ceramic. However, the CaLa reported above2S4The problems of easy oxidation, serious sulfur loss, long sintering time, difficult sintering and the like in the sintering process commonly exist in the ceramic sintering method, and the obtained CaLa2S4Sulfur oxide impurities formed by oxidation exist in the infrared ceramic phase, which leads to 8-14 μm infrared band SO3 2-And SO4 2-And further results in low infrared transmittance.
At present, CaLa2S4The preparation and research of the infrared transparent ceramics have the following problems: firstly, the purity of the powder is not high, and the particle size is not uniform; secondly, the sintering temperature is high and the oxidation is easy in the hot pressing process; thirdly, the infrared transmittance is low, which seriously affects the CaLa2S4Application of infrared transparent ceramic window material. Therefore, in comprehensive view, the CaLa with high stability, high density and high transmittance is developed2S4The new process method of the transparent ceramic has important significance.
Disclosure of Invention
The invention aims to provide a high-energy ball milling and SPS sintering CaLa2S4Preparation method of infrared transparent ceramicThe method has simple and convenient preparation process and easy adjustment, and the obtained infrared transparent ceramic has high transmittance and good stability.
The scheme adopted by the invention for realizing the purpose is as follows: high-energy ball milling and SPS sintering CaLa2S4The preparation method of the infrared transparent ceramic comprises the following steps:
(1) under the protection of inert gas, adding CaS and La2S3Mixing the powder according to a certain proportion, and performing high-energy ball milling to obtain CaLa2S4Powder;
(2) the obtained CaLa2S4The powder is wrapped by graphite paper and then is sintered by discharge plasma in a vacuum state;
(3) after sintering, the obtained hot pressed block CaLa2S4Polishing the ceramic to obtain CaLa2S4An infrared transparent ceramic.
Preferably, in the step (1), CaS is 4N pure grade CaS, La2S3Is 4N pure grade La2S3The ratio of the amounts of La and Ca is (2.0-3.0): 1.
preferably, in the step (1), ZrO is used2And (3) carrying out high-energy ball milling on the small balls, wherein the ball milling medium is n-heptane, and the ball-to-material ratio is 10-20: 1.
Preferably, in the step (1), the high-energy ball milling time is 30-720min, and the rotation speed is 300-.
Preferably, in the step (1), CaLa2S4The particle size of the powder is 0.5-1.5 μm.
Preferably, in the step (2), the sintering conditions are as follows: and (3) carrying out heat preservation sintering for 10-30 min under the sintering pressure of 50-100 MPa and the pulse current of 300-500A.
Preferably, in the step (3), CaLa2S4The maximum transmittance of the infrared transparent ceramic in an infrared band with a wavelength of 8-14 mu m is more than or equal to 55 percent.
The invention has the following advantages and beneficial effects: the preparation method of the invention realizes ceramic molding by using high-energy ball milling and spark plasma sintering (SPS sintering), and prepares CaLa with high hardness, high transmittance and high corrosion resistance2S4An infrared transparent ceramic. Compared with the prior ceramic sintering technology, the method utilizes a high-energy ball milling method to mix CaS and La2S3The powder is mixed evenly and alloyed, and H with high toxicity and high danger is not involved in the experiment2S is used, and SPS sintering in vacuum is used in the sintering process, so that the problem of CaLa is effectively solved2S4The infrared transparent ceramics are easy to oxidize during sintering, the sintering time is long, and the sulfur in the sample is lost. Meanwhile, the technology has the advantages of simple process, convenience and rapidness in preparation and high efficiency, and is suitable for preparing CaLa in batches2S4The infrared transparent ceramic has wide application prospect.
Drawings
FIG. 1 is a particle size distribution of the powder prepared in example 1;
FIG. 2 shows CaLa prepared in example 12S4The micro-morphology of the ceramic.
Detailed Description
The following examples are provided to further illustrate the present invention for better understanding, but the present invention is not limited to the following examples.
Example 1
In this example, high energy ball milling + SPS sintering of CaLa2S4The preparation method of the infrared transparent ceramic comprises the following steps:
(1) under the protection of inert gas, 15g of ZrO was weighed2Pellets and 0.1875g CaS and 1.3125g La2S3Powder;
(2) under the protection of inert gas, ZrO weighed in the step (1)2Adding the small balls and the raw materials into a high-energy ball milling tank;
(3) adding 2.5ml of n-heptane into the high-energy ball-milling tank in the step (2) under the protection of inert gas and sealing;
(4) putting the high-energy ball milling tank in the step (3) into a high-energy ball mill for ball milling for 360min, wherein the rotating speed of the ball mill is 600 rpm;
(5) opening the high-energy ball milling tank in the step (4), taking out the sample, washing the sample for multiple times by using n-heptane, and then putting the sample at 80 ℃ and the vacuum degree of 10-3Pa, drying for 6 hours to obtain CaLa2S4Powder with an average particle size of 1 μm; as shown in FIG. 1, the CaLa prepared in this example2S4Distribution diagram of particle size of powder.
(6) The CaLa obtained in the step (5) is used2S4The powder is wrapped by graphite paper and put into a graphite mould, the mould is placed in a vacuum chamber for vacuumizing, then a pulse power supply is turned on, and the electrode pressure head is utilized for carrying out discharge plasma sintering. Sintering at 100MPa of sintering pressure and 500A of pulse current for 30min in a heat preservation manner;
(7) then removing the voltage, naturally cooling the vacuum pressure to room temperature, and removing the vacuum pressure;
(8) taking out the sample from the mold to obtain a hot-pressed block body CaLa2S4Polishing the ceramic by using diamond sand paper to obtain CaLa with the highest transmittance of more than or equal to 55 percent in 8-14 mu m long-wave infrared band2S4An infrared transparent ceramic.
As shown in FIG. 2, CaLa prepared for this example2S4Microscopic topography of infrared transparent ceramics.
Example 2
In this example, high energy ball milling + SPS sintering of CaLa2S4The preparation method of the infrared transparent ceramic comprises the following steps:
(1) under the protection of inert gas, 30g of ZrO was weighed2Pellets and 0.2425g CaS and 1.2575g La2S3Powder;
(2) under the protection of inert gas, ZrO weighed in the step (1)2Adding the small balls and the raw materials into a high-energy ball milling tank;
(3) adding 2.5ml of n-heptane into the high-energy ball-milling tank in the step (2) under the protection of inert gas and sealing;
(4) putting the high-energy ball milling tank in the step (3) into a high-energy ball mill for ball milling for 30min, wherein the rotating speed of the ball mill is 800 rpm;
(5) opening the high-energy ball milling tank in the step (4), taking out the sample, washing the sample for multiple times by using n-heptane, and then putting the sample at 60 ℃ and the vacuum degree of 10-3Drying under Pa for 8 hours to obtain CaLa2S4Powder with an average particle size of 1.5 μm;
(6) the CaLa obtained in the step (5) is used2S4The powder is wrapped by graphite paper and put into a graphite mould, the mould is placed in a vacuum chamber for vacuumizing, then a pulse power supply is turned on, and the electrode pressure head is utilized for carrying out discharge plasma sintering. Sintering at 100MPa sintering pressure and 350A pulse current for 20 min;
(7) then removing the voltage, naturally cooling the vacuum pressure to room temperature, and removing the vacuum pressure;
(8) taking out the sample from the mold to obtain a hot-pressed block body CaLa2S4Polishing the ceramic by using diamond sand paper to obtain CaLa with the highest transmittance of more than or equal to 45 percent in 8-14 mu m long-wave infrared band2S4An infrared transparent ceramic.
Example 3
In this example, high energy ball milling + SPS sintering of CaLa2S4The preparation method of the infrared transparent ceramic comprises the following steps:
step 1: CaLa2S4And (3) preparing the powder by high-energy ball milling.
(1) 22.5g of ZrO were weighed out under inert gas atmosphere2Pellets and 0.1709g CaS and 1.3291g La2S3Powder;
(2) under the protection of inert gas, ZrO weighed in the step (1)2Adding the small balls and the raw materials into a high-energy ball milling tank;
(3) adding 2.5ml of n-heptane into the high-energy ball-milling tank in the step (2) under the protection of inert gas and sealing;
(4) putting the high-energy ball milling tank in the step (3) into a high-energy ball mill for ball milling for 720min, wherein the rotating speed of the ball mill is 700 rpm;
(5) opening the high-energy ball milling tank in the step (4), taking out the sample, washing the sample for multiple times by using n-heptane, and then putting the sample at 50 ℃ and the vacuum degree of 10-3Drying under Pa for 10 hours to obtain CaLa2S4Powder with average grain diameter of 0.5 μm;
(2) the CaLa obtained in the step (5) is used2S4Wrapping the powder with graphite paper and putting the wrapped powder into a graphite moldAnd placing the mould in a vacuum chamber for vacuumizing, then opening a pulse power supply, and performing discharge plasma sintering by using an electrode pressure head. Sintering at 50MPa and 300A pulse current for 30 min;
(7) then removing the voltage, naturally cooling the vacuum pressure to room temperature, and removing the vacuum pressure;
(8) taking out the sample from the mold to obtain a hot-pressed block body CaLa2S4Polishing the ceramic by using diamond sand paper to obtain CaLa with the highest transmittance of more than or equal to 47.1 percent in a long-wave infrared band of 8-14 mu m2S4An infrared transparent ceramic.
Example 4
In this example, high energy ball milling + SPS sintering of CaLa2S4The preparation method of the infrared transparent ceramic comprises the following steps:
(1) 22.5g of ZrO were weighed out under inert gas atmosphere2Pellets and 0.1570g CaS and 1.3430g La2S3Powder;
(2) under the protection of inert gas, ZrO weighed in the step (1)2Adding the small balls and the raw materials into a high-energy ball milling tank;
(3) adding 2.5ml of n-heptane into the high-energy ball-milling tank in the step (2) under the protection of inert gas and sealing;
(4) putting the high-energy ball milling tank in the step (3) into a high-energy ball mill for ball milling for 120min, wherein the rotating speed of the ball mill is 300 rpm;
(5) opening the high-energy ball milling tank in the step (4), taking out the sample, washing the sample for multiple times by using n-heptane, and then putting the sample at 80 ℃ and the vacuum degree of 10-3Drying under Pa for 12 hours to obtain CaLa2S4Powder with an average particle size of 1.3 μm;
(6) the CaLa obtained in the step (5) is used2S4The powder is wrapped by graphite paper and put into a graphite mould, the mould is placed in a vacuum chamber for vacuumizing, then a pulse power supply is turned on, and the electrode pressure head is utilized for carrying out discharge plasma sintering. Sintering at 70MPa and 325A pulse current for 15 min;
(7) then removing the voltage, naturally cooling the vacuum pressure to room temperature, and removing the vacuum pressure;
(8) taking out the sample from the mold to obtain a hot-pressed block body CaLa2S4Polishing the ceramic by using diamond sand paper to obtain CaLa with the highest transmittance of more than or equal to 46.4 percent in a long-wave infrared band of 8-14 mu m2S4An infrared transparent ceramic.
Example 5
In this example, high energy ball milling + SPS sintering of CaLa2S4The preparation method of the infrared transparent ceramic comprises the following steps:
(1) 22.5g of ZrO were weighed out under inert gas atmosphere2Pellets and 0.1489g CaS and 1.3511g La2S3Powder;
(2) under the protection of inert gas, ZrO weighed in the step (1)2Adding the small balls and the raw materials into a high-energy ball milling tank;
(3) adding 2.5ml of n-heptane into the high-energy ball-milling tank in the step (2) under the protection of inert gas and sealing;
(4) putting the high-energy ball milling tank in the step (3) into a high-energy ball mill for ball milling for 360min, wherein the rotating speed of the ball mill is 450 rpm;
(5) opening the high-energy ball milling tank in the step (4), taking out the sample, washing the sample for multiple times by using n-heptane, and then putting the sample at 80 ℃ and the vacuum degree of 10-3Drying under Pa for 12 hours to obtain CaLa2S4Powder with an average particle size of 1 μm;
(6) the CaLa obtained in the step (5) is used2S4The powder is wrapped by graphite paper and put into a graphite mould, the mould is placed in a vacuum chamber for vacuumizing, then a pulse power supply is turned on, and the electrode pressure head is utilized for carrying out discharge plasma sintering. Sintering at 70MPa and 325A pulse current for 10 min;
(7) then removing the voltage, naturally cooling the vacuum pressure to room temperature, and removing the vacuum pressure;
(8) taking out the sample from the mold to obtain a hot-pressed block body CaLa2S4Polishing the ceramic by using diamond sand paper to obtain CaLa with the highest transmittance of more than or equal to 46.4 percent in a long-wave infrared band of 8-14 mu m2S4An infrared transparent ceramic.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (7)
1. High-energy ball milling and SPS sintering CaLa2S4The preparation method of the infrared transparent ceramic is characterized by comprising the following steps:
(1) under the protection of inert gas, adding CaS and La2S3Mixing the powder according to a certain proportion, and performing high-energy ball milling to obtain CaLa2S4Powder;
(2) the obtained CaLa2S4The powder is wrapped by graphite paper and then is sintered by discharge plasma in a vacuum state;
(8) after sintering, the obtained hot pressed block CaLa2S4Polishing the ceramic to obtain CaLa2S4An infrared transparent ceramic.
2. The high energy ball mill + SPS sintering CaLa of claim 12S4The preparation method of the infrared transparent ceramic is characterized by comprising the following steps: in the step (1), the CaS is 4N pure grade CaS, La2S3Is 4N pure grade La2S3The ratio of the amounts of La and Ca is (2.0-3.0): 1.
3. the high energy ball mill + SPS sintering CaLa of claim 12S4The preparation method of the infrared transparent ceramic is characterized by comprising the following steps: in the step (1), ZrO is used2And (3) carrying out high-energy ball milling on the small balls, wherein the ball milling medium is n-heptane, and the ball-to-material ratio is 10-20: 1.
4. The high energy ball mill + SPS sintering CaLa of claim 12S4The preparation method of the infrared transparent ceramic is characterized by comprising the following steps: in the step (1), is highThe ball milling time is 30-720min, and the rotation speed is 300-800 rpm.
5. The high energy ball mill + SPS sintering CaLa of claim 12S4The preparation method of the infrared transparent ceramic is characterized by comprising the following steps: in the step (1), CaLa2S4The average particle diameter of the powder is 0.5-1.5 μm.
6. The high energy ball mill + SPS sintering CaLa of claim 12S4The preparation method of the infrared transparent ceramic is characterized by comprising the following steps: in the step (2), the sintering conditions are as follows: and (3) carrying out heat preservation sintering for 10-30 min under the sintering pressure of 50-100 MPa and the pulse current of 300-500A.
7. The high energy ball mill + SPS sintering CaLa of claim 12S4The preparation method of the infrared transparent ceramic is characterized by comprising the following steps: in the step (3), CaLa2S4The maximum transmittance of the infrared transparent ceramic in an infrared band with a wavelength of 8-14 mu m is more than or equal to 55 percent.
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