WO2023024187A1 - Preparation method for yag-based transparent ceramic having large-scale thin sheet composite structure - Google Patents
Preparation method for yag-based transparent ceramic having large-scale thin sheet composite structureDownload PDFInfo
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Definitions
- the inventionbelongs to the technical field of preparation of advanced functional ceramics, and in particular relates to a preparation method of YAG-based transparent ceramics with a large-scale sheet composite structure.
- Thin-plate lasershave become a class of high-power solid-state lasers with broad development prospects due to their advantages such as small thermal lens effect, high output power, excellent beam quality, and high light-to-light conversion efficiency. They are widely used in key application fields such as industry, national defense, and medical treatment. .
- high-power laser outputthere are a large number of key technologies that need to be broken through in thin-sheet lasers.
- the thin-sheet laser gain medium with high doping concentrationhas always been an important factor restricting the development of high-power thin-sheet lasers.
- YAG transparent ceramicsAs an ideal laser gain medium, yttrium aluminum garnet (YAG) transparent ceramics have cubic structure, no birefringence effect, small high temperature creep, excellent optical properties and mechanical properties, etc., which can meet the application requirements of high-power laser output.
- YAG transparent ceramicsare mainly prepared by powder sintering. To achieve high transparency, it is necessary to fully eliminate the pores and impurity phases in the ceramics, be completely dense and have extremely thin grain boundaries, and have extremely stringent requirements for raw materials, equipment, molding and sintering processes.
- CN112500162Adiscloses a YAG transparent ceramic and its densification sintering method. The technical problem to be solved is to realize the preparation of high-quality ceramics without using sintering aids. However, this patent needs to be sintered under 196Mpa argon medium by hot isostatic pressing. out of transparent ceramics.
- CN111253153Adiscloses a method for preparing toughened large-size ultra-thin YAG transparent ceramic biscuits based on Isobam gel system. The technical problem solved is the difficult problem of preparing large-scale transparent ceramics, but the preparation of transparent ceramics with complex shapes and composite structures cannot be realized. , unable to meet the application requirements of high-power thin-sheet laser gain medium.
- the present inventionprovides a preparation method of large-scale sheet composite structure YAG-based transparent ceramics.
- the technical scheme adopted in the present inventionis as follows: a method for preparing a YAG-based transparent ceramic with a large-scale sheet composite structure, comprising the following steps:
- step (2)Add a YAG-based raw material powder obtained in step (1) into a roller mill tank, add dispersant B, and water as a solvent to adjust the solid content of the slurry to 60-65wt.%, ball mill for 4-8 hours, and rotate at a speed of 180 ⁇ 220r/min; add plasticizer, ball mill for 2 ⁇ 4 hours, the speed is 140 ⁇ 180r/min; add binder, ball mill for 24 ⁇ 30 hours, the speed is 80 ⁇ 120r/min; add water resistant agent, ball mill for 1 ⁇ 4h , with a rotating speed of 80-120r/min; filtering the obtained slurry, vacuum defoaming, and tape casting to obtain a water-based tape-cast YAG-based ceramic green body;
- step (3)Add another YAG-based raw material powder obtained in step (1) into a roller mill tank, add dispersant C, pH regulator, monomer acrylamide, crosslinking agent, add water as a solvent, and adjust the slurry
- the solid contentis 56-62vol.%, ball milling for 6-12 hours, and the ball milling speed is 120-150r/min; filter the obtained slurry, vacuum defoam, add catalyst ammonium persulfate, and then prepare the obtained slurry in step (2) Tape-cast molding on the YAG-based ceramic green body to obtain a composite structure YAG-based ceramic green body;
- step (3)Custom-cut the composite structure YAG-based ceramic green body obtained in step (3), put the green body into a constant temperature and humidity box, adjust the humidity to 80%, the temperature is 30 ° C, and dry for 6 to 12 hours; the adjusted humidity is 70%, the temperature is 30°C, dry for 48-96h; adjust the humidity to 60%, the temperature is 30°C, dry for 48-96h; adjust the humidity to 60%, the temperature is 40°C, dry for 24-48h; drying;
- step (4)Put the YAG-based ceramic green body obtained in step (4) into a muffle furnace for debinding treatment, then place it in a vacuum sintering furnace for sintering, and finally place it in a muffle furnace for annealing to obtain a composite structure YAG-based transparent ceramics.
- the dispersant Ais polyetherimide (PEI), the amount of dispersant A added accounts for 0.01-0.05wt.% of the total mass of the ceramic powder, and the sintering aid is orthosilicic acid Ethyl ester (TEOS) and magnesium oxide (MgO), the addition of ethyl orthosilicate is 0.03-0.08wt.% of the total mass of the ceramic powder, and the addition of magnesium oxide is 0.01-0.05wt of the total mass of the raw material powder .%.
- PEIpolyetherimide
- TEOSorthosilicic acid Ethyl ester
- MgOmagnesium oxide
- ethyl orthosilicateis 0.03-0.08wt.% of the total mass of the ceramic powder
- magnesium oxideis 0.01-0.05wt of the total mass of the raw material powder .%.
- step (1)the rotational speed of the ball mill is 160-190 r/min, and the milling time is 10-20 hours.
- step (1)the calcination temperature is 600-1000° C., and the calcination time is 3-10 hours.
- the dispersant Bis polyacrylic acid (PAA), and the amount of the dispersant B accounts for 0.1 to 0.5wt.% of the total mass of the YAG-based raw material powder;
- the plasticizeris polyethylene glycol (PEG), the addition of plasticizer accounts for 3.0 ⁇ 6.0wt.% of the total mass of YAG-based raw material powder; 3.0-6.0wt.% of the total mass of the YAG-based raw material powder;
- the water-resistant agentis acetic acid, and the amount of the water-resistant agent accounts for 0.1-2.0wt.% of the total mass of the YAG-based raw material powder.
- the dispersant Cis ammonium citrate
- the amount of the dispersant Cis 0.1-0.6wt.% of the total mass of the YAG-based powder
- the pH regulatoris ammonia water or tetramethyl hydroxide Ammonium
- the cross-linking agentis any one of ethylene dimethacrylate (EDMA), diethylene glycol diacrylate (DEGDA) or N,N'-methylenebisacrylamide (MBAM), cross-linking
- EDMAethylene dimethacrylate
- DEGDAdiethylene glycol diacrylate
- MBAMN,N'-methylenebisacrylamide
- step (4)the drying temperature is 55° C., and the drying time is 24-48 hours.
- step (5)the specific process of debinding is as follows: at room temperature, the temperature is raised to 800° C. at a rate of 0.5-2° C./min, and the temperature is kept for 24-72 hours.
- step (5)the specific parameters of the vacuum sintering are: the sintering temperature is 1780° C., the vacuum degree is 8 ⁇ 10 ⁇ 3 Pa, and the holding time is 8 hours.
- step (5)the specific parameters of the annealing are: the annealing temperature is 1200-1500° C., and the holding time is 10-24 hours.
- the present inventionhas the following beneficial effects:
- the composite structure YAG-based ceramic green body prepared by the present inventiondoes not need cold isostatic pressing or warm isostatic pressing, effectively avoids the phenomenon of delamination and cracking in the dual-system wet forming and drying process, and the relative density after debinding is between More than 52%, it can be directly used in the later stage of vacuum sintering to prepare YAG-based transparent ceramics with high optical quality.
- the present inventionadopts water-based casting molding and gel casting molding to prepare YAG-based transparent ceramics with a composite structure.
- the preparation processis green, environmentally friendly, energy-saving, high-efficiency, and non-toxic, and is suitable for industrial production of YAG-based transparent ceramics.
- the water-based casting process used in the present inventionprepares YAG-based transparent ceramics, effectively avoids the interface melting phenomenon existing in the traditional preparation process of composite structure sheet materials, and the long diffusion distance of the dual-system slurry, etc., can directly realize the phenomenon of greater than 1mm bisque preparation.
- Fig. 1is the physical figure of the composite structure Ce:YAG/Cr:YAG based transparent ceramic ceramic green body.
- Fig. 2is a physical picture of the composite structure Ce:YAG/Cr:YAG-based transparent ceramic after polishing.
- Fig. 3is the EPMA test diagram at the interface of the composite structure Ce:YAG/Cr:YAG-based transparent ceramic.
- Fig. 4is a cross-sectional SEM test image of a composite structure Ce:YAG/Cr:YAG-based transparent ceramic.
- Fig. 5is a physical picture of a composite structure Ce:YAG/Mn:YAG-based transparent ceramic.
- Al raw materialsare selected from commercially available high-purity (99.99% and above) nano-Al 2 O 3 powder; Y, Ce, and Cr raw materials are selected from commercially available high-purity (99.999% and above) nano-Y 2 O 3 , CeO 2 , Cr 2 O 3 powder; use commercially available high-purity (99.99% and above) magnesium oxide (MgO) and tetraethyl orthosilicate (TEOS) as co-sintering aids for YAG-based transparent ceramics; use polyacrylic acid (PAA ), polyvinyl alcohol (PVA) and polyethylene glycol (PEG) respectively as the dispersant, binder and plasticizer of the slurry composition in water-based tape casting; ammonium citrate, acrylamide, NN methylene Bisacrylamide is used as the dispersant, monomer and crosslinking agent of the gel casting slurry; the commercially available ultrapure water is used as the solvent in the casting slurry of the two systems;
- the ball milling timeis 8h, and the ball milling speed It is 140r/min; Gained slurry is filtered, vacuum defoaming, add 0.0125g catalyzer ammonium persulfate, gained slurry is carried out tape-cast molding on the Ce:YAG ceramic biscuit that step (3) prepares, obtain composite structure Ce :YAG/Cr:YAG based porcelain biscuit.
- Drying of the composite structure Ce:YAG/Cr:YAG-based ceramic green bodycustom-cut the composite structure Ce:YAG/Cr:YAG-based ceramic green body prepared in step (4), and put the green body into a constant temperature Humidity box, adjust the humidity to 80%, the temperature is 30°C, and the drying time is 8 hours; adjust the humidity to 70%, the temperature is 30°C, and the drying time is 48 hours; adjust the humidity to 60%, the temperature is 30°C, and the drying time is 48 hours; The humidity is adjusted to 60%, the temperature is 40°C, and the drying time is 24 hours; then the obtained green body is put into a blast drying oven, the temperature is 55°C, and the drying time is 24 hours;
- Annealing of composite structure Ce:YAG/Cr:YAG-based transparent ceramicsput the YAG-based transparent ceramics obtained in step (7) into a muffle furnace for annealing, the annealing temperature is 1400°C, and the holding time is 24h, the target can be obtained.
- the composite structure of the productis Ce:YAG/Cr:YAG based transparent ceramics.
- Fig. 1is a physical picture of a composite structure Ce:YAG/Cr:YAG-based transparent ceramic ceramic green body. It can be seen from the figure that the green body has good molding quality and no defects such as peeling and wrinkles on the surface.
- Figure 2is the physical picture of the composite structure Ce:YAG/Cr:YAG-based transparent ceramic after polishing. From the picture, the interface of the sample is clearly visible, and the sample has good optical quality.
- Fig. 3is the EPMA test diagram at the interface of the composite structure Ce:YAG/Cr:YAG-based transparent ceramic, from which it can be clearly seen that the diffusion distance of the sample is relatively small.
- Figure 4is the SEM test diagram of the cross-section of the composite structure Ce:YAG/Cr:YAG-based transparent ceramics. It can be seen from the figure that the microstructures of the YAG ceramic samples with different structures are different.
- Raw material selectionAl raw materials are selected from commercially available high-purity (99.99% and above) nano-Al 2 O 3 powder; Y, Ce, and Mn raw materials are selected from commercially available high-purity (99.999% and above) nano-Y 2 O 3 , CeO 2 , MnCO 3 powder; use commercially available high-purity (99.99% and above) magnesium oxide (MgO) and tetraethyl orthosilicate (TEOS) as co-sintering aids for YAG-based transparent ceramics; use polyacrylic acid (PAA), Polyvinyl alcohol (PVA) and polyethylene glycol (PEG) are respectively used as the dispersant, binder and plasticizer of the slurry composition in the water-based tape casting; ammonium citrate, acrylamide, NN methylenebispropylene The amides are respectively used as the dispersant, monomer and crosslinking agent of the gel casting slurry; the commercially available ultrapure water is selected as the solvent in the casting s
- Drying of the composite structure Ce:YAG/Mn:YAG-based ceramic green bodycustom-cut the composite structure Ce:YAG/Mn:YAG-based ceramic green body prepared in step (4), and put the green body into a constant temperature Humidity box, adjust the humidity to 80%, the temperature is 30°C, and the drying time is 8 hours; adjust the humidity to 70%, the temperature is 30°C, and the drying time is 48 hours; adjust the humidity to 60%, the temperature is 30°C, and the drying time is 48 hours; The humidity is adjusted to 60%, the temperature is 40°C, and the drying time is 24 hours; then the obtained green body is put into a blast drying oven, the temperature is 55°C, and the drying time is 24 hours;
- Annealing of Ce:YAG/Mn:YAG-based transparent ceramics with composite structureput the YAG-based transparent ceramics obtained in step (7) into a muffle furnace for annealing, the annealing temperature is 1400 ° C, and the holding time is 24 hours, and the target can be obtained.
- the composite structure of the productis Ce:YAG/Mn:YAG based transparent ceramics.
- Fig. 5is a physical picture of a composite structure Ce:YAG/Mn:YAG-based transparent ceramic ceramic, which is a red transparent ceramic.
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Abstract
Description
Translated fromChinese本发明属于先进功能陶瓷制备技术领域，具体涉及一种大尺寸薄片复合结构YAG基透明陶瓷的制备方法。The invention belongs to the technical field of preparation of advanced functional ceramics, and in particular relates to a preparation method of YAG-based transparent ceramics with a large-scale sheet composite structure.
1960年1月18日，美国加利福尼亚休斯实验室的西奥多·梅曼研制出了世界上第一台红宝石激光器。从此，激光技术取得了飞速的发展，被广泛应用于军事、医疗、通信等领域。目前，市场上主要有四大类激光器，分别是固体激光器、气体激光器、半导体激光器和染料激光器；其中，固体激光器以其峰值功率大、输出能量高、结构简单、体积小等优势引领激光技术发展。On January 18, 1960, Theodore Maiman of Hughes Laboratory in California developed the world's first ruby laser. Since then, laser technology has achieved rapid development and has been widely used in military, medical, communication and other fields. At present, there are four main types of lasers on the market, namely solid-state lasers, gas lasers, semiconductor lasers and dye lasers; among them, solid-state lasers lead the development of laser technology with their advantages such as high peak power, high output energy, simple structure, and small size. .
薄片激光器以其热透镜效应小、输出功率高、光束质量优异、光-光转化效率高等优点成为一类具有广阔发展前景的高功率固体激光器，被广泛应用于工业、国防、医疗等重点应用领域。但是，围绕高功率的激光输出，薄片激光器存在大量亟待突破的关键技术。其中，高掺杂浓度的薄片激光增益介质一直是制约高功率薄片激光器发展的重要因素。Thin-plate lasers have become a class of high-power solid-state lasers with broad development prospects due to their advantages such as small thermal lens effect, high output power, excellent beam quality, and high light-to-light conversion efficiency. They are widely used in key application fields such as industry, national defense, and medical treatment. . However, around high-power laser output, there are a large number of key technologies that need to be broken through in thin-sheet lasers. Among them, the thin-sheet laser gain medium with high doping concentration has always been an important factor restricting the development of high-power thin-sheet lasers.
作为理想激光增益介质，钇铝石榴石(YAG)透明陶瓷具有立方结构，无双折射效应，高温蠕变小，光学性质和力学性能优异等特点能够满足高功率激光输出的应用要求。目前，YAG透明陶瓷主要采用粉末烧结制备方法，要达到高透明度，需要充分排除陶瓷中的气孔和杂质相、完全致密且晶界极薄，对原料、设备、成型和烧结工艺有极其苛刻的要求，比如需要高纯、高分散性的纳米粉体原料、热等静压和真空烧结等，晶粒在长时间高温烧结过程中容易长大。CN112500162A公开了一种YAG透明陶瓷及其致密化烧结方法，解决的技术问题是无需采用烧结助剂实现高质量陶瓷的制备，但是，该专利需使用热等静压在196Mpa氩气介质下烧结制备出透明陶瓷。CN111253153A公开了一种基于Isobam凝胶体系制备增韧大尺寸超薄YAG透明陶瓷素坯的方法，解决的技术问题是大尺寸透明陶瓷制备难题，但是，无法实现复杂形状、复合结构透明陶瓷的制备，无法满足高功率薄片激光器增益介质的应用要求。As an ideal laser gain medium, yttrium aluminum garnet (YAG) transparent ceramics have cubic structure, no birefringence effect, small high temperature creep, excellent optical properties and mechanical properties, etc., which can meet the application requirements of high-power laser output. At present, YAG transparent ceramics are mainly prepared by powder sintering. To achieve high transparency, it is necessary to fully eliminate the pores and impurity phases in the ceramics, be completely dense and have extremely thin grain boundaries, and have extremely stringent requirements for raw materials, equipment, molding and sintering processes. , such as the need for high-purity, high-dispersion nano-powder raw materials, hot isostatic pressing and vacuum sintering, etc., the grains are easy to grow during long-term high-temperature sintering. CN112500162A discloses a YAG transparent ceramic and its densification sintering method. The technical problem to be solved is to realize the preparation of high-quality ceramics without using sintering aids. However, this patent needs to be sintered under 196Mpa argon medium by hot isostatic pressing. out of transparent ceramics. CN111253153A discloses a method for preparing toughened large-size ultra-thin YAG transparent ceramic biscuits based on Isobam gel system. The technical problem solved is the difficult problem of preparing large-scale transparent ceramics, but the preparation of transparent ceramics with complex shapes and composite structures cannot be realized. , unable to meet the application requirements of high-power thin-sheet laser gain medium.
发明内容Contents of the invention
为了解决复合结构陶瓷制备过程中存在的扩散界面长、界面结合强度差的问题，本发明提供一种大尺寸薄片复合结构YAG基透明陶瓷的制备方法。In order to solve the problems of long diffusion interface and poor interfacial bonding strength existing in the preparation process of composite structure ceramics, the present invention provides a preparation method of large-scale sheet composite structure YAG-based transparent ceramics.
为实现上述目的，本发明采用的技术方案如下：一种大尺寸薄片复合结构YAG基透明陶瓷的制备方法，包括以下步骤：In order to achieve the above object, the technical scheme adopted in the present invention is as follows: a method for preparing a YAG-based transparent ceramic with a large-scale sheet composite structure, comprising the following steps:
(1)按照化学式(Yx,RE1-x)3Al5O12或Y3(Alx,RE1-x)5O12，0.0005<x<0.3中各元素化学计量比分别称量Y2O3、RE2O3和Al2O3粉体作为陶瓷粉体，其中RE为稀土元素铈、镨、钕、钐、铕、铽、镝、钬、铒、铥或镱中的一种；将称量好的陶瓷粉体、分散剂A、烧结助剂、无水乙醇按一定比例混合后加入行星式球磨罐中，球磨得混合浆料；将所述混合浆料过滤干燥，过筛，然后将过筛后的粉体置于马弗炉中煅烧，得到两种不同的YAG基原料粉体；(1) According to the chemical formula (Yx , RE1-x )3 Al5 O12 or Y3 (Alx , RE1-x )5 O12 , the stoichiometric ratio of each element in 0.0005<x<0.3 is weighed separately for Y2 O3 , RE2 O3 and Al2 O3 powders are used as ceramic powders, where RE is one of the rare earth elements cerium, praseodymium, neodymium, samarium, europium, terbium, dysprosium, holmium, erbium, thulium or ytterbium ; Mix the weighed ceramic powder, dispersant A, sintering aid, and absolute ethanol in a certain proportion and then add them to the planetary ball mill tank, and ball mill to obtain a mixed slurry; filter and dry the mixed slurry, and sieve , and then place the sieved powder in a muffle furnace for calcination to obtain two different YAG-based raw material powders;
(2)将步骤(1)得到的一种YAG基原料粉体加入滚筒球磨罐中，加入分散剂B，水作为溶剂，调节浆料固含量60～65wt.％，球磨4～8h，转速为180～220r/min；加入增塑剂，球磨2～4h，转速为140～180r/min；加入粘结剂，球磨24～30h，转速为80～120r/min；加入耐水剂，球磨1～4h，转速为80～120r/min；将所得浆料进行过滤，真空除泡，流延成型，得到水基流延成型YAG基陶瓷素坯；(2) Add a YAG-based raw material powder obtained in step (1) into a roller mill tank, add dispersant B, and water as a solvent to adjust the solid content of the slurry to 60-65wt.%, ball mill for 4-8 hours, and rotate at a speed of 180～220r/min; add plasticizer, ball mill for 2～4 hours, the speed is 140～180r/min; add binder, ball mill for 24～30 hours, the speed is 80～120r/min; add water resistant agent, ball mill for 1～4h , with a rotating speed of 80-120r/min; filtering the obtained slurry, vacuum defoaming, and tape casting to obtain a water-based tape-cast YAG-based ceramic green body;
(3)将步骤(1)得到的另一种YAG基原料粉体加入滚筒球磨罐中，加入分散剂C、pH调节剂、单体丙烯酰胺、交联剂，加入水作为溶剂，调节浆料固含量为56～62vol.％，球磨6～12h，球磨转速为120～150r/min；将所得浆料过滤，真空除泡，加入催化剂过硫酸铵，然后将所得浆料在步骤(2)制备的YAG基陶瓷素坯上进行流延成型，得到复合结构YAG基陶瓷素坯；(3) Add another YAG-based raw material powder obtained in step (1) into a roller mill tank, add dispersant C, pH regulator, monomer acrylamide, crosslinking agent, add water as a solvent, and adjust the slurry The solid content is 56-62vol.%, ball milling for 6-12 hours, and the ball milling speed is 120-150r/min; filter the obtained slurry, vacuum defoam, add catalyst ammonium persulfate, and then prepare the obtained slurry in step (2) Tape-cast molding on the YAG-based ceramic green body to obtain a composite structure YAG-based ceramic green body;
(4)将步骤(3)得到的复合结构YAG基陶瓷素坯进行自定义裁剪，将素坯放入恒温恒湿箱，调节湿度80％，温度为30℃，干燥6～12h；调节湿度为70％，温度为30℃，干燥48～96h；调节湿度为60％，温度为30℃，干燥48～96h；调节湿度为60％，温度为40℃，干燥24～48h；然后将所得素坯烘干；(4) Custom-cut the composite structure YAG-based ceramic green body obtained in step (3), put the green body into a constant temperature and humidity box, adjust the humidity to 80%, the temperature is 30 ° C, and dry for 6 to 12 hours; the adjusted humidity is 70%, the temperature is 30°C, dry for 48-96h; adjust the humidity to 60%, the temperature is 30°C, dry for 48-96h; adjust the humidity to 60%, the temperature is 40°C, dry for 24-48h; drying;
(5)将步骤(4)得到的YAG基陶瓷素坯放入马弗炉中排胶处理后，再置于真空烧结炉中烧结，最后置于马弗炉退火，即得到复合结构YAG基透明陶瓷。(5) Put the YAG-based ceramic green body obtained in step (4) into a muffle furnace for debinding treatment, then place it in a vacuum sintering furnace for sintering, and finally place it in a muffle furnace for annealing to obtain a composite structure YAG-based transparent ceramics.
步骤(1)中，所述分散剂A为聚醚酰亚胺(PEI)，分散剂A的加入量占 陶瓷粉体总质量的0.01～0.05wt.％，所述烧结助剂为正硅酸乙酯(TEOS)和氧化镁(MgO)，正硅酸乙酯的加入量为陶瓷粉体总质量的0.03～0.08wt.％，氧化镁的加入量为原料粉体总质量的0.01～0.05wt.％。In step (1), the dispersant A is polyetherimide (PEI), the amount of dispersant A added accounts for 0.01-0.05wt.% of the total mass of the ceramic powder, and the sintering aid is orthosilicic acid Ethyl ester (TEOS) and magnesium oxide (MgO), the addition of ethyl orthosilicate is 0.03-0.08wt.% of the total mass of the ceramic powder, and the addition of magnesium oxide is 0.01-0.05wt of the total mass of the raw material powder .%.
步骤(1)中，所述球磨转速为160～190r/min，球磨时长为10～20h。In step (1), the rotational speed of the ball mill is 160-190 r/min, and the milling time is 10-20 hours.
步骤(1)中，所述煅烧温度为600～1000℃，煅烧时长为3～10h。In step (1), the calcination temperature is 600-1000° C., and the calcination time is 3-10 hours.
步骤(2)中，所述分散剂B为聚丙烯酸(PAA)，分散剂B的加入量占YAG基原料粉体总质量的0.1～0.5wt.％；所述增塑剂为聚乙二醇(PEG)，增塑剂的加入量占YAG基原料粉体总质量的3.0～6.0wt.％；所述粘结剂为聚乙烯醇(PVA)，粘结剂的加入量占YAG基原料粉体总质量的3.0～6.0wt.％；所述耐水剂为醋酸，耐水剂的加入量占YAG基原料粉体总质量的0.1～2.0wt.％。In step (2), the dispersant B is polyacrylic acid (PAA), and the amount of the dispersant B accounts for 0.1 to 0.5wt.% of the total mass of the YAG-based raw material powder; the plasticizer is polyethylene glycol (PEG), the addition of plasticizer accounts for 3.0～6.0wt.% of the total mass of YAG-based raw material powder; 3.0-6.0wt.% of the total mass of the YAG-based raw material powder; the water-resistant agent is acetic acid, and the amount of the water-resistant agent accounts for 0.1-2.0wt.% of the total mass of the YAG-based raw material powder.
步骤(3)中，所述分散剂C为柠檬酸铵，分散剂C的加入量占YAG基粉体总质量的0.1～0.6wt.％，所述pH调节剂为氨水或四甲基氢氧化铵，所述交联剂为乙二甲基丙烯酸酯(EDMA)、二乙二醇二丙烯酸酯(DEGDA)或N,N’-亚甲基双丙烯酰胺(MBAM)中任一种，交联剂的加入量占YAG基原料粉体总质量的0.1～0.5wt.％，所述单体丙烯酰胺的加入量占YAG基原料粉体总质量的2～5wt.％。In step (3), the dispersant C is ammonium citrate, the amount of the dispersant C is 0.1-0.6wt.% of the total mass of the YAG-based powder, and the pH regulator is ammonia water or tetramethyl hydroxide Ammonium, the cross-linking agent is any one of ethylene dimethacrylate (EDMA), diethylene glycol diacrylate (DEGDA) or N,N'-methylenebisacrylamide (MBAM), cross-linking The added amount of the agent accounts for 0.1-0.5 wt.% of the total mass of the YAG-based raw material powder, and the added amount of the monomer acrylamide accounts for 2-5 wt.% of the total mass of the YAG-based raw material powder.
步骤(4)中，所述烘干的温度为55℃，干燥时长为24～48h。In step (4), the drying temperature is 55° C., and the drying time is 24-48 hours.
步骤(5)中，所述排胶的具体过程为：室温下以0.5～2℃/min的速率升温至800℃，保温24～72h。In step (5), the specific process of debinding is as follows: at room temperature, the temperature is raised to 800° C. at a rate of 0.5-2° C./min, and the temperature is kept for 24-72 hours.
步骤(5)中，所述真空烧结的具体参数为：烧结温度为1780℃，真空度为8×10-3Pa，保温时长为8h。In step (5), the specific parameters of the vacuum sintering are: the sintering temperature is 1780° C., the vacuum degree is 8×10−3 Pa, and the holding time is 8 hours.
步骤(5)中，所述退火的具体参数为：退火温度为1200～1500℃，保温时长10～24h。In step (5), the specific parameters of the annealing are: the annealing temperature is 1200-1500° C., and the holding time is 10-24 hours.
与现有技术相比，本发明具有如下有益效果：Compared with the prior art, the present invention has the following beneficial effects:
(1)本发明制备的复合结构YAG基陶瓷素坯无需冷等静压、温等静压，有效避免双体系湿法成型干燥过程中存在的分层、开裂现象，且排胶后相对密度在52％以上，可直接用于后期的真空烧结进行制备高光学质量的YAG基透明陶瓷。(1) The composite structure YAG-based ceramic green body prepared by the present invention does not need cold isostatic pressing or warm isostatic pressing, effectively avoids the phenomenon of delamination and cracking in the dual-system wet forming and drying process, and the relative density after debinding is between More than 52%, it can be directly used in the later stage of vacuum sintering to prepare YAG-based transparent ceramics with high optical quality.
(2)本发明采用水系流延成型、凝胶流延成型制备复合结构YAG基透明陶瓷，制备过程绿色环保、节能高效、无毒性，适合YAG基透明陶瓷工业化生产。(2) The present invention adopts water-based casting molding and gel casting molding to prepare YAG-based transparent ceramics with a composite structure. The preparation process is green, environmentally friendly, energy-saving, high-efficiency, and non-toxic, and is suitable for industrial production of YAG-based transparent ceramics.
(3)本发明采用的水基流延工艺制备YAG基透明陶瓷，有效避免传统制备复合结构薄片材料制备工艺中存在的界面溶融现象，双体系浆料的长扩散距离等现象，能够直接实现大于1mm的素坯制备。(3) The water-based casting process used in the present invention prepares YAG-based transparent ceramics, effectively avoids the interface melting phenomenon existing in the traditional preparation process of composite structure sheet materials, and the long diffusion distance of the dual-system slurry, etc., can directly realize the phenomenon of greater than 1mm bisque preparation.
图1为复合结构Ce:YAG/Cr:YAG基透明陶瓷陶瓷素坯的实物图。Fig. 1 is the physical figure of the composite structure Ce:YAG/Cr:YAG based transparent ceramic ceramic green body.
图2为复合结构Ce:YAG/Cr:YAG基透明陶瓷端面抛光后的实物图。Fig. 2 is a physical picture of the composite structure Ce:YAG/Cr:YAG-based transparent ceramic after polishing.
图3为复合结构Ce:YAG/Cr:YAG基透明陶瓷界面处的EPMA测试图。Fig. 3 is the EPMA test diagram at the interface of the composite structure Ce:YAG/Cr:YAG-based transparent ceramic.
图4为复合结构Ce:YAG/Cr:YAG基透明陶瓷断面SEM测试图。Fig. 4 is a cross-sectional SEM test image of a composite structure Ce:YAG/Cr:YAG-based transparent ceramic.
图5为复合结构Ce:YAG/Mn:YAG基透明陶瓷的实物图。Fig. 5 is a physical picture of a composite structure Ce:YAG/Mn:YAG-based transparent ceramic.
下面结合附图和具体实施例对本发明作进一步详细说明。The present invention will be described in further detail below in conjunction with the accompanying drawings and specific embodiments.
实施例1：制备复合结构Ce:YAG/Cr:YAG基透明陶瓷Example 1: Preparation of composite structure Ce:YAG/Cr:YAG-based transparent ceramics
(1)原料选取：Al原料选用市售高纯(99.99％及以上)纳米Al2O3粉体；Y、Ce、Cr原料选用市售高纯(99.999％及以上)纳米Y2O3、CeO2、Cr2O3粉体；选用市售高纯(99.99％及以上)氧化镁(MgO)和正硅酸乙酯(TEOS)作为YAG基透明陶瓷的共烧结助剂；选用聚丙烯酸(PAA)、聚乙烯醇(PVA)和聚乙二醇(PEG)分别作为水系流延成型中浆料组成的分散剂、粘结剂和增塑剂；选用柠檬酸铵、丙烯酰胺、N-N亚甲基双丙烯酰胺分别作为凝胶流延浆料组成的分散剂、单体和交联剂；选用市售超纯水为两种体系流延浆料中的溶剂；(1) Selection of raw materials: Al raw materials are selected from commercially available high-purity (99.99% and above) nano-Al2 O3 powder; Y, Ce, and Cr raw materials are selected from commercially available high-purity (99.999% and above) nano-Y2 O3 , CeO2 , Cr2 O3 powder; use commercially available high-purity (99.99% and above) magnesium oxide (MgO) and tetraethyl orthosilicate (TEOS) as co-sintering aids for YAG-based transparent ceramics; use polyacrylic acid (PAA ), polyvinyl alcohol (PVA) and polyethylene glycol (PEG) respectively as the dispersant, binder and plasticizer of the slurry composition in water-based tape casting; ammonium citrate, acrylamide, NN methylene Bisacrylamide is used as the dispersant, monomer and crosslinking agent of the gel casting slurry; the commercially available ultrapure water is used as the solvent in the casting slurry of the two systems;
(2)YAG基粉体制备：按照(Y0.999,Ce0.001)3Al5O12化学计量比配制125g Ce:YAG陶瓷粉体，分别加入0.04g PEI作为分散剂，加入0.625g TEOS和0.125g MgO作为烧结助剂，加入无水乙醇作为溶剂，采用行星式球磨，球磨转速为180r/min，球磨时长为15h。将所得陶瓷浆料过滤干燥，过筛，在800℃下煅烧3h，得到混合好的Ce:YAG原料粉体。按照Y3(Al0.999,Cr0.001)5O12化学计量比配制125g Cr:YAG陶瓷粉体，采用相同方法球磨混合，过滤、干燥、过筛、煅烧，得到混合好的Cr:YAG原料粉体。(2) Preparation of YAG-based powder: prepare 125g Ce:YAG ceramic powder according to (Y0.999 , Ce0.001 )3 Al5 O12 stoichiometric ratio, add 0.04g PEI as dispersant, add 0.625g TEOS and 0.125g MgO was used as a sintering aid, absolute ethanol was added as a solvent, and a planetary ball mill was used with a ball milling speed of 180r/min and a ball milling time of 15h. The obtained ceramic slurry was filtered and dried, sieved, and calcined at 800° C. for 3 hours to obtain a mixed Ce:YAG raw material powder. Prepare 125g of Cr:YAG ceramic powder according to the stoichiometric ratio of Y3 (Al0.999 ,Cr0.001 )5 O12 , ball mill and mix in the same way, filter, dry, sieve, and calcinate to obtain the mixed Cr:YAG raw material powder .
(3)水系流延浆料制备：将步骤(2)制备的Ce:YAG原料粉体加入滚筒球磨罐中，加入0.375g PAA作为分散剂，水作为溶剂，调节浆料固含量60wt.％，进行球磨，时长为4h，转速为200r/min；加入增塑剂6.25g PEG，进行球磨，时 长为4h，转速为160r/min；加入粘结剂6.25g PVA，球磨时长为24h，转速为110r/min；加入耐水剂0.625g醋酸，球磨为3h，转速为100r/min；将所得浆料进行过滤，真空除泡，流延成型，得到水基流延成型Ce:YAG基陶瓷素坯。(3) Preparation of water-based casting slurry: add the Ce:YAG raw material powder prepared in step (2) into a roller mill tank, add 0.375g PAA as a dispersant, and use water as a solvent to adjust the solid content of the slurry to 60wt.%. Carry out ball milling for 4 hours at a speed of 200r/min; add 6.25g of plasticizer PEG for ball milling for 4 hours at a speed of 160r/min; add binder 6.25g of PVA for 24 hours of ball milling at a speed of 110r /min; add 0.625g of acetic acid water-resistant agent, ball mill for 3 hours, and rotate at 100r/min; filter the obtained slurry, vacuum defoam, and tape-cast to obtain a water-based tape-cast Ce:YAG-based ceramic green body.
(4)水基凝胶流延成型浆料制备：将步骤(2)制备的Cr:YAG原料粉体加入滚筒球磨罐中，加入0.375g柠檬酸铵作为分散剂，加入氨水调节pH值到11，加入3.75g单体丙烯酰胺，加入0.125g交联剂N,N亚甲基双丙烯酰胺，加入水作为溶剂，调节浆料固含量为56vol.％，进行球磨，球磨时长为8h，球磨转速为140r/min；将所得浆料过滤，真空除泡，加入0.0125g催化剂过硫酸铵，将所得浆料在步骤(3)制备的Ce:YAG陶瓷素坯上进行流延成型，得到复合结构Ce:YAG/Cr:YAG基瓷素坯。(4) Preparation of water-based gel tape casting slurry: Add the Cr:YAG raw material powder prepared in step (2) into the roller mill tank, add 0.375g ammonium citrate as a dispersant, add ammonia water to adjust the pH value to 11 , add 3.75g of monomeric acrylamide, add 0.125g of cross-linking agent N, N methylene bisacrylamide, add water as a solvent, adjust the solid content of the slurry to 56vol.%, and perform ball milling. The ball milling time is 8h, and the ball milling speed It is 140r/min; Gained slurry is filtered, vacuum defoaming, add 0.0125g catalyzer ammonium persulfate, gained slurry is carried out tape-cast molding on the Ce:YAG ceramic biscuit that step (3) prepares, obtain composite structure Ce :YAG/Cr:YAG based porcelain biscuit.
(5)复合结构Ce:YAG/Cr:YAG基陶瓷素坯干燥：将步骤(4)制备的复合结构Ce:YAG/Cr:YAG基陶瓷素坯进行自定义裁剪，将素坯放入恒温恒湿箱，调节湿度80％，温度为30℃，干燥时长为8h；调节湿度为70％，温度为30℃，干燥时长为48h；调节湿度为60％，温度为30℃，干燥时长为48h；调节湿度为60％，温度为40℃，干燥时长为24h；然后将所得素坯加入鼓风式干燥箱，温度为55℃，干燥时长为24h；(5) Drying of the composite structure Ce:YAG/Cr:YAG-based ceramic green body: custom-cut the composite structure Ce:YAG/Cr:YAG-based ceramic green body prepared in step (4), and put the green body into a constant temperature Humidity box, adjust the humidity to 80%, the temperature is 30°C, and the drying time is 8 hours; adjust the humidity to 70%, the temperature is 30°C, and the drying time is 48 hours; adjust the humidity to 60%, the temperature is 30°C, and the drying time is 48 hours; The humidity is adjusted to 60%, the temperature is 40°C, and the drying time is 24 hours; then the obtained green body is put into a blast drying oven, the temperature is 55°C, and the drying time is 24 hours;
(6)复合结构Ce:YAG/Cr:YAG基陶瓷素坯排胶：将步骤(4)得到的Ce:YAG/Cr:YAG基陶瓷素坯放入马弗炉中排胶，排胶升温速率为0.5℃/min，温度为800℃，时长36h。(6) Composite structure Ce:YAG/Cr:YAG-based ceramic green body debinding: put the Ce:YAG/Cr:YAG-based ceramic green body obtained in step (4) into a muffle furnace for debinding, and the debinding heating rate The temperature is 0.5°C/min, the temperature is 800°C, and the time is 36h.
(7)复合结构Ce:YAG/Cr:YAG基陶瓷烧结：将步骤(6)得到的YAG基陶瓷素坯放入真空烧结炉中烧结，烧结温度为1780℃，真空度为8×10-3Pa，保温时长为8h，得到复合结构CeYAG/Cr:YAG基透明陶瓷。(7) Sintering of composite structure Ce:YAG/Cr:YAG-based ceramics: put the YAG-based ceramic green body obtained in step (6) into a vacuum sintering furnace for sintering, the sintering temperature is 1780°C, and the vacuum degree is 8×10-3 Pa, the holding time is 8h, and the composite structure CeYAG/Cr:YAG-based transparent ceramics is obtained.
(8)复合结构Ce:YAG/Cr:YAG基透明陶瓷退火：将步骤(7)得到的YAG基透明陶瓷放入马弗炉中退火，退火温度为1400℃，保温时长24h，即可得到目标产品复合结构Ce:YAG/Cr:YAG基透明陶瓷。(8) Annealing of composite structure Ce:YAG/Cr:YAG-based transparent ceramics: put the YAG-based transparent ceramics obtained in step (7) into a muffle furnace for annealing, the annealing temperature is 1400°C, and the holding time is 24h, the target can be obtained. The composite structure of the product is Ce:YAG/Cr:YAG based transparent ceramics.
图1为复合结构Ce:YAG/Cr:YAG基透明陶瓷陶瓷素坯的实物图，从图中可以看出素坯成型质量良好、表面无起皮、褶皱等缺陷。Fig. 1 is a physical picture of a composite structure Ce:YAG/Cr:YAG-based transparent ceramic ceramic green body. It can be seen from the figure that the green body has good molding quality and no defects such as peeling and wrinkles on the surface.
图2为复合结构Ce:YAG/Cr:YAG基透明陶瓷端面抛光后的实物图，从图中出样品分界面清晰可见，样品具有良好的光学质量。Figure 2 is the physical picture of the composite structure Ce:YAG/Cr:YAG-based transparent ceramic after polishing. From the picture, the interface of the sample is clearly visible, and the sample has good optical quality.
图3为复合结构Ce:YAG/Cr:YAG基透明陶瓷界面处的EPMA测试图，从图中可以清晰的看出样品的扩散距离较小。Fig. 3 is the EPMA test diagram at the interface of the composite structure Ce:YAG/Cr:YAG-based transparent ceramic, from which it can be clearly seen that the diffusion distance of the sample is relatively small.
图4为复合结构Ce:YAG/Cr:YAG基透明陶瓷断面SEM测试图，从图中看出不同结构的YAG陶瓷样品的显微结构不同。Figure 4 is the SEM test diagram of the cross-section of the composite structure Ce:YAG/Cr:YAG-based transparent ceramics. It can be seen from the figure that the microstructures of the YAG ceramic samples with different structures are different.
实施例2：制备复合结构Ce:YAG/Mn:YAG基透明陶瓷Example 2: Preparation of composite structure Ce:YAG/Mn:YAG-based transparent ceramics
(1)原料选取：Al原料选用市售高纯(99.99％及以上)纳米Al2O3粉体；Y、Ce、Mn原料选用市售高纯(99.999％及以上)纳米Y2O3、CeO2、MnCO3粉体；选用市售高纯(99.99％及以上)氧化镁(MgO)和正硅酸乙酯(TEOS)作为YAG基透明陶瓷的共烧结助剂；选用聚丙烯酸(PAA)、聚乙烯醇(PVA)和聚乙二醇(PEG)分别作为水系流延成型中浆料组成的分散剂、粘结剂和增塑剂；选用柠檬酸铵、丙烯酰胺、N-N亚甲基双丙烯酰胺分别作为凝胶流延浆料组成的分散剂、单体和交联剂；选用市售超纯水为两种体系流延浆料中的溶剂；(1) Raw material selection: Al raw materials are selected from commercially available high-purity (99.99% and above) nano-Al2 O3 powder; Y, Ce, and Mn raw materials are selected from commercially available high-purity (99.999% and above) nano-Y2 O3 , CeO2 , MnCO3 powder; use commercially available high-purity (99.99% and above) magnesium oxide (MgO) and tetraethyl orthosilicate (TEOS) as co-sintering aids for YAG-based transparent ceramics; use polyacrylic acid (PAA), Polyvinyl alcohol (PVA) and polyethylene glycol (PEG) are respectively used as the dispersant, binder and plasticizer of the slurry composition in the water-based tape casting; ammonium citrate, acrylamide, NN methylenebispropylene The amides are respectively used as the dispersant, monomer and crosslinking agent of the gel casting slurry; the commercially available ultrapure water is selected as the solvent in the casting slurry of the two systems;
(2)YAG基粉体制备：按照(Y0.999,Ce0.001)3Al5O12化学计量比配制125g Ce:YAG陶瓷粉体，加入0.04g PEI作为分散剂，加入0.625g TEOS和0.125g MgO作为烧结助剂，加入无水乙醇作为溶剂，采用行星式球磨，球磨转速为180r/min，球磨时长为15h；将所得陶瓷浆料过滤干燥，过筛，在800℃下煅烧3h，得到混合好的Ce:YAG原料粉体。按照Y3(Al0.999,Mn0.001)5O12化学计量比配置125gMn:YAG陶瓷粉体，采用相同方法球磨混合，过滤、干燥、过筛、煅烧，得到混合好的Mn:YAG原料粉体；(2) Preparation of YAG-based powder: prepare 125g Ce:YAG ceramic powder according to (Y0.999 , Ce0.001 )3 Al5 O12 stoichiometric ratio, add 0.04g PEI as dispersant, add 0.625g TEOS and 0.125g MgO As a sintering aid, add absolute ethanol as a solvent, use planetary ball milling, the ball milling speed is 180r/min, and the ball milling time is 15h; the obtained ceramic slurry is filtered and dried, sieved, and calcined at 800°C for 3h to obtain a good mixture. Ce:YAG raw material powder. Configure 125g of Mn:YAG ceramic powder according to the stoichiometric ratio of Y3 (Al0.999 ,Mn0.001 )5 O12 , ball mill and mix in the same way, filter, dry, sieve, and calcinate to obtain the mixed Mn:YAG raw material powder;
(3)水系流延浆料制备：将步骤(2)制备的Ce:YAG原料粉体加入滚筒球磨罐中，加入0.375g PAA作为分散剂，水作为溶剂，调节浆料固含量60wt.％，进行球磨，时长为4h，转速为200r/min；加入增塑剂6.25g PEG，进行球磨，时长为4h，转速为160r/min；加入粘结剂6.25gPVA，球磨时长为24h，转速为110r/min；加入耐水剂0.625g醋酸，球磨为3h，转速为100r/min；将所得浆料进行过滤，真空除泡，流延成型，得到水基流延成型Ce:YAG基陶瓷素坯。(3) Preparation of water-based casting slurry: add the Ce:YAG raw material powder prepared in step (2) into a roller mill tank, add 0.375g PAA as a dispersant, and use water as a solvent to adjust the solid content of the slurry to 60wt.%. Carry out ball milling for 4 hours at a speed of 200r/min; add 6.25g of plasticizer PEG for ball milling for 4 hours at a speed of 160r/min; add binder 6.25g of PVA for 24 hours of ball milling at a speed of 110r/min min; add 0.625g of water resistant agent acetic acid, ball mill for 3 hours, and rotate at a speed of 100r/min; filter the obtained slurry, vacuum defoam, and tape cast to obtain a water-based tape-cast Ce:YAG-based ceramic green body.
(4)水基凝胶流延成型浆料制备：将步骤(2)制备的Mn:YAG原料粉体加入滚筒球磨罐中，加入0.375g柠檬酸铵作为分散剂，加入四甲基氢氧化铵调节pH值到11，加入3.75g单体丙烯酰胺，加入0.125g交联剂N,N亚甲基双丙烯酰胺，加入水作为溶剂，调节浆料固含量为56vol.％，进行球磨，球磨时长为 8h，球磨转速为140r/min；将所得浆料过滤，真空除泡，加入0.0125g催化剂过硫酸铵，将所得浆料在步骤(3)制备的Ce:YAG陶瓷素坯上进行流延成型，得到复合结构Ce:YAG/Mn:YAG基瓷素坯。(4) Preparation of water-based gel casting slurry: add the Mn:YAG raw material powder prepared in step (2) into the roller mill tank, add 0.375g ammonium citrate as a dispersant, and add tetramethylammonium hydroxide Adjust the pH value to 11, add 3.75g of monomer acrylamide, add 0.125g of crosslinking agent N,N methylenebisacrylamide, add water as a solvent, adjust the solid content of the slurry to 56vol.%, and perform ball milling for a long time 8h, the ball milling speed is 140r/min; the resulting slurry is filtered, vacuum defoamed, and 0.0125g of catalyst ammonium persulfate is added, and the resulting slurry is tape-casted on the Ce:YAG ceramic biscuit prepared in step (3) , to obtain a composite structure Ce:YAG/Mn:YAG based ceramic green body.
(5)复合结构Ce:YAG/Mn:YAG基陶瓷素坯干燥：将步骤(4)制备的复合结构Ce:YAG/Mn:YAG基陶瓷素坯进行自定义裁剪，将素坯放入恒温恒湿箱，调节湿度80％，温度为30℃，干燥时长为8h；调节湿度为70％，温度为30℃，干燥时长为48h；调节湿度为60％，温度为30℃，干燥时长为48h；调节湿度为60％，温度为40℃，干燥时长为24h；然后将所得素坯加入鼓风式干燥箱，温度为55℃，干燥时长为24h；(5) Drying of the composite structure Ce:YAG/Mn:YAG-based ceramic green body: custom-cut the composite structure Ce:YAG/Mn:YAG-based ceramic green body prepared in step (4), and put the green body into a constant temperature Humidity box, adjust the humidity to 80%, the temperature is 30°C, and the drying time is 8 hours; adjust the humidity to 70%, the temperature is 30°C, and the drying time is 48 hours; adjust the humidity to 60%, the temperature is 30°C, and the drying time is 48 hours; The humidity is adjusted to 60%, the temperature is 40°C, and the drying time is 24 hours; then the obtained green body is put into a blast drying oven, the temperature is 55°C, and the drying time is 24 hours;
(6)复合结构Ce:YAG/Mn:YAG基陶瓷素坯排胶：将步骤(4)得到的Ce:YAG/Mn:YAG基陶瓷素坯放入马弗炉中排胶，排胶升温速率为0.5℃/min，温度为800℃，时长36h。(6) Composite structure Ce:YAG/Mn:YAG-based ceramic green body debinding: put the Ce:YAG/Mn:YAG-based ceramic green body obtained in step (4) into a muffle furnace for debinding, and the debinding heating rate The temperature is 0.5°C/min, the temperature is 800°C, and the time is 36h.
(7)复合结构Ce:YAG/Mn:YAG基陶瓷烧结：将步骤(6)得到的YAG基陶瓷素坯放入真空烧结炉中烧结，烧结温度为1780℃，真空度为8×10-3Pa，保温时长为8h，得到复合结构Ce:YAG/Mn:YAG基透明陶瓷。(7) Sintering of composite structure Ce:YAG/Mn:YAG-based ceramics: put the YAG-based ceramic green body obtained in step (6) into a vacuum sintering furnace for sintering, the sintering temperature is 1780°C, and the vacuum degree is 8×10-3 Pa, the holding time is 8h, and the composite structure Ce:YAG/Mn:YAG-based transparent ceramics is obtained.
(8)复合结构Ce:YAG/Mn:YAG基透明陶瓷退火：将步骤(7)得到的YAG基透明陶瓷放入马弗炉中退火，退火温度为1400℃，保温时长24h，即可得到目标产品复合结构Ce:YAG/Mn:YAG基透明陶瓷。(8) Annealing of Ce:YAG/Mn:YAG-based transparent ceramics with composite structure: put the YAG-based transparent ceramics obtained in step (7) into a muffle furnace for annealing, the annealing temperature is 1400 ° C, and the holding time is 24 hours, and the target can be obtained. The composite structure of the product is Ce:YAG/Mn:YAG based transparent ceramics.
图5为复合结构Ce:YAG/Mn:YAG基透明陶瓷陶瓷实物图，为红色透明陶瓷。Fig. 5 is a physical picture of a composite structure Ce:YAG/Mn:YAG-based transparent ceramic ceramic, which is a red transparent ceramic.
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| US20040167010A1 (en)* | 2001-01-19 | 2004-08-26 | Tatsuhiro Sato | Transparent ceramics and method for producing the same |
| US20090108507A1 (en)* | 2007-09-14 | 2009-04-30 | The Penn State Research Foundation | Method for manufacture of transparent ceramics |
| CN104725052A (en)* | 2014-12-18 | 2015-06-24 | 徐州市江苏师范大学激光科技有限公司 | Preparation method of multilayer composite structured transparent ceramic |
| CN112174668A (en)* | 2020-10-17 | 2021-01-05 | 江苏师范大学 | Preparation method and application of transparent ceramic with multilayer composite structure |
| CN112851331A (en)* | 2021-02-08 | 2021-05-28 | 新沂市锡沂高新材料产业技术研究院有限公司 | Industrial production method of YAG-based transparent ceramic |
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| CN117229057A (en)* | 2023-09-14 | 2023-12-15 | 福州大学 | Simple and convenient LaGaO preparation 3 Method for preparing electrolyte sheet |
| CN117964357A (en)* | 2023-12-26 | 2024-05-03 | 江苏锡沂高新材料产业技术研究院有限公司 | A method for preparing YAG-based transparent ceramics by rotary evaporation and drying |
| CN118026691A (en)* | 2024-02-03 | 2024-05-14 | 江苏三责新材料科技股份有限公司 | Preparation method of pressureless sintered silicon carbide ceramic sheet |
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| CN113716951A (en) | 2021-11-30 |
| CN113716951B (en) | 2022-04-29 |
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