Yttrium aluminum garnet precursor photocuring slurry and method for preparing porous yttrium aluminum garnet ceramic by using same

By combining yttrium aluminum garnet precursor photocuring slurry with 3D printing, debinding, and sintering processes, the preparation problem of porous yttrium aluminum garnet ceramics was solved, achieving high-precision and high-purity production of complex structures, and improving molding efficiency and structural design flexibility.

CN121735645APending Publication Date: 2026-03-27ANHUI POLYTECHNIC UNIV
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-12-18
Publication Date
2026-03-27

AI Technical Summary

Technical Problem

Existing technologies make it difficult to prepare porous yttrium aluminum garnet ceramics using 3D printing, especially for forming complex shapes and producing high-purity products. Furthermore, traditional processes suffer from drawbacks such as high sintering temperatures and low mechanical properties.

Method used

Porous yttrium aluminum garnet ceramics were prepared by using a yttrium aluminum garnet precursor photocurable slurry, including alumina, yttrium oxide, photosensitive resin and dispersant, which was formed by 3D printing technology and combined with a 6-stage debinding process and a mild sintering process.

Benefits of technology

It has enabled high-precision molding and high-purity production of complex-shaped porous yttrium aluminum garnet ceramics, improving molding efficiency and structural design flexibility, and solving the molding problems of traditional processes.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses yttrium aluminum garnet precursor photocuring slurry and a method for preparing porous yttrium aluminum garnet ceramic by using the same. The yttrium aluminum garnet precursor photocuring slurry comprises the following raw materials: mixed ceramic powder consisting of aluminum oxide and yttrium oxide, photosensitive resin and a dispersing agent, wherein in the mixed ceramic powder, the mass percent of aluminum oxide is 42.9%, and the mass percent of yttrium oxide is 57.1%; the photosensitive resin comprises the following raw materials: a photosensitive monomer, an initiator and a plasticizer; the porous YAG ceramic with a complex structure can be prepared through printing, degreasing and sintering processes matched with the YAG precursor photocuring slurry, and the method is high in forming precision, good in surface quality, high in forming efficiency and extremely high in structural design flexibility.
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Description

Technical Field

[0001] This invention belongs to the field of ceramic materials technology, specifically relating to a photocurable yttrium aluminum garnet precursor slurry and a method for preparing porous yttrium aluminum garnet ceramics using it. Background Technology

[0002] Yttrium aluminum garnet (YAG, chemical formula Y3Al5O) 12 Garnet-type composite oxide ceramics possess excellent high-temperature stability, with a melting point of approximately 1950℃ and no phase transformation below 1200℃. They also exhibit good chemical inertness and reliable biocompatibility, with an in vitro cell survival rate >95% and no harmful ion leaching. Porous YAG ceramics, by introducing a controllable pore structure into their matrix, further endow the material with high specific surface area, low thermal conductivity, and fluid permeability, thereby expanding their application potential in fields such as catalyst supports, high-temperature insulation, biological tissue repair, and filtration separation.

[0003] Traditional porous YAG preparation processes, such as organic foam impregnation and pore-forming agent methods combined with solid-state sintering, can achieve a certain degree of porosity control, but still face drawbacks such as difficulty in forming complex-shaped components, high sintering temperatures, and low mechanical properties, limiting their application areas. For example, Chinese patent CN110002863 A discloses a method for preparing yttrium aluminum garnet porous ceramics. The specific steps are: using ultrafine YAG powder prepared by co-precipitation as raw material, adding sintering aids silica and calcium oxide, and a foaming agent glucose, ball milling and mixing uniformly with water or anhydrous ethanol as the ball milling medium, drying, and molding to obtain a ceramic blank, placing the ceramic blank in a vacuum tube furnace, first foaming and decarburizing, then sintering the ceramic, and finally cooling the sintered ceramic at room temperature to obtain YAG porous ceramics. Although this patent can prepare yttrium aluminum garnet porous ceramics, it cannot achieve the forming of complex-shaped yttrium aluminum garnet porous ceramic components.

[0004] While 3D printing technology offers a new approach to manufacturing complex ceramic parts, existing technologies do not disclose how to use this technology to prepare porous yttrium aluminum garnet ceramics, nor do they establish a complete and reliable debinding and sintering process route for porous yttrium aluminum garnet ceramics. Summary of the Invention

[0005] To address the aforementioned technical problems, this invention provides a photocurable slurry for yttrium aluminum garnet precursors and its preparation method. The photocurable slurry for yttrium aluminum garnet precursors can be used to produce green yttrium aluminum garnet precursors of arbitrary shapes through laser 3D printing technology, thereby enabling the large-scale production of porous yttrium aluminum garnet ceramics.

[0006] The present invention also provides a method for preparing porous yttrium aluminum garnet ceramics using the yttrium aluminum garnet precursor photocurable slurry, which can achieve the production of high-purity porous yttrium aluminum garnet ceramics.

[0007] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0008] This invention provides a yttrium aluminum garnet precursor photocurable slurry, which comprises the following raw materials: a mixed ceramic powder composed of alumina and yttrium oxide, a photosensitive resin, and a dispersant;

[0009] In the mixed ceramic powder, the mass percentage of alumina is 42.9% and the mass percentage of yttrium oxide is 57.1%.

[0010] The photosensitive resin comprises the following raw materials: photosensitive monomer, initiator and plasticizer.

[0011] The alumina has a particle size of 0.2 μm-2 μm; the yttrium oxide has a particle size of 0.1 μm-1 μm.

[0012] The mass fraction of the mixed ceramic powder in the yttrium aluminum garnet precursor photocurable slurry is 70-85%.

[0013] The amount of the dispersant used is 1-4% of the mass of the mixed ceramic powder; the dispersant is BYK111.

[0014] The photosensitive monomer is composed of trimethylolpropane triacrylate and 1,6-hexanediol diacrylate in a mass ratio of 1:3-5.

[0015] In the photosensitive resin, the amounts of initiator and plasticizer are 0.5-2.0% and 20-30% of the mass of the photosensitive monomer, respectively.

[0016] The plasticizer is any one or more of polyethylene glycol 200 and polyethylene glycol 400.

[0017] The initiator is 2,4,6-trimethylbenzoyl-diphenylphosphine oxide.

[0018] The present invention also provides a method for preparing the yttrium aluminum garnet precursor photocurable slurry, the preparation method comprising the following steps:

[0019] (1) Mix alumina and yttrium oxide, add a dispersant, and use anhydrous ethanol and zirconium oxide grinding balls as wet grinding media to ball mill to obtain dispersant-modified mixed ceramic powder;

[0020] (2) Mix the photosensitive monomer, initiator and plasticizer evenly to obtain the photosensitive resin;

[0021] (3) Add dispersant-modified mixed ceramic powder to photosensitive resin, mix thoroughly and then perform vacuum degassing to obtain yttrium aluminum garnet precursor photocurable slurry.

[0022] In step (1), the ball milling time is 4-8 hours; the sum of the masses of alumina and yttrium oxide: zirconium oxide milling balls: anhydrous ethanol = 1:2:2.

[0023] This invention also provides a method for preparing porous yttrium aluminum garnet ceramics using the yttrium aluminum garnet precursor photocurable slurry described herein, the preparation method comprising the following steps:

[0024] 1) The yttrium aluminum garnet precursor photocurable slurry described in this invention is used for 3D printing to obtain a printed sample;

[0025] 2) The printed samples were degreased under the protection of an inert gas atmosphere;

[0026] 3) After degreasing, the printed sample is heated to 580-620℃ at a heating rate of 0.5-1.5℃ / min and held for 1.5-2h to remove carbon. Then, it is heated to 1550-1650℃ at a heating rate of 3-8℃ / min and held for 1-5h to sinter, thus obtaining porous yttrium aluminum garnet ceramic.

[0027] In step 1), the 3D printing conditions are: laser energy density 177-757 mJ / cm². 2 The layer thickness is 25-100μm, and the scanning rate is 2000-6000mm / s.

[0028] In step 2), the degreasing process employs a 6-stage degreasing process, specifically as follows:

[0029] First stage: Heat from 20℃ to 110℃ at a heating rate of 1℃ / min and hold for 1-4 hours;

[0030] Second stage: Heat from 110℃ to 200℃ at a heating rate of 1℃ / min and hold for 1-4 hours;

[0031] The third stage: heating from 200℃ to 350℃ at a heating rate of 1℃ / min and holding for 1-4 hours;

[0032] Fourth stage: Increase the temperature from 350℃ to 400℃ at a heating rate of 0.2℃ / min and hold for 1-4 hours;

[0033] Fifth stage: Increase the temperature from 400℃ to 460℃ at a heating rate of 0.2℃ / min and hold for 1-4 hours;

[0034] Section 6: Heat from 460℃ to 550℃ at a heating rate of 0.2℃ / min and hold for 1-4 hours.

[0035] The yttrium aluminum garnet precursor photocurable slurry provided by this invention comprises the following raw materials: a mixed ceramic powder consisting of 42.9 wt% alumina and 57.1 wt% yttrium oxide, a photosensitive resin, and a dispersant. The mass ratio of alumina to yttrium oxide in the mixed ceramic powder precisely corresponds to YAG (Y3Al5O3). 12 The stoichiometric ratio ensures sufficient solid-phase reaction between alumina and yttrium oxide during sintering, preventing the formation of impurity phases due to excess of any one component and guaranteeing a high-purity YAG phase in the final product. The dispersant forms an adsorption layer on the surface of the ceramic powder particles, hindering particle agglomeration through steric hindrance or electrostatic repulsion, thus uniformly dispersing the ceramic powder in the photosensitive resin to form a homogeneous and stable slurry system.

[0036] Photosensitive resin includes the following raw materials: photosensitive monomer, initiator, and plasticizer. Among them, the photosensitive monomer has high reactivity and can undergo a rapid polymerization reaction under the action of the initiator through light irradiation, realizing the instant curing of the slurry and improving the molding efficiency of 3D printing. The plasticizer can reduce the glass transition temperature of the photosensitive monomer after polymerization, improve the flexibility of the cured green body, and optimize the thermal decomposition behavior of the green body, so that the organic phase in the slurry decomposes and volatilizes slowly during the degreasing process, reducing the volume change and internal stress accumulation during the degreasing process, reducing the risk of green body cracking and deformation, and ensuring the integrity of the green body.

[0037] This invention provides a method for preparing porous yttrium aluminum garnet ceramics using a photocurable slurry based on a yttrium aluminum garnet precursor. The process involves 3D printing, debinding, decarburization, and sintering. The debinding stage employs a six-stage process, utilizing temperature zoning, rate control, and heat buffering to achieve gentle decomposition, slow degassing, and stress-free removal of organic matter in the printed sample, significantly improving the stability of the fine structure formed by 3D printing. After debinding, the temperature is raised to 580-620℃ at a matching rate to remove any remaining carbides. Finally, sintering is performed at 1550-1650℃ for 1-5 hours at a rate of 3-8℃ / min, yielding high-purity porous yttrium aluminum garnet ceramics.

[0038] Compared with the prior art, the present invention has the following beneficial effects:

[0039] This invention solves the problem that traditional processes cannot form complex porous yttrium aluminum garnet ceramic structures, and develops a complete process route of printing-debinding-sintering. By mixing a mixed ceramic powder composed of alumina and yttrium oxide with a premixed liquid, a YAG precursor photocurable slurry with excellent printing and curing properties is prepared. It can be directly applied to photocurable molding technology, filling a gap in this field, and the YAG ceramics prepared from it have high purity.

[0040] This invention solves the problem of preparing porous YAG ceramics with complex structures by using a printing, debinding, and sintering process that is compatible with the YAG precursor photocurable slurry. The porous YAG ceramics prepared by 3D printing technology using the Yttrium aluminum garnet precursor photocurable slurry described in this invention have high forming precision, good surface quality, high forming efficiency, and extremely high structural design flexibility. It also provides a new approach for combining solid-state synthesis and 3D printing. Attached Figure Description

[0041] Figure 1 Images of porous YAG ceramics of different shapes prepared in Example 7;

[0042] Figure 2 The XRD pattern of the porous yttrium aluminum garnet ceramic prepared in Example 7;

[0043] Figure 3 SEM image of the porous yttrium aluminum garnet ceramic prepared in Example 7;

[0044] Figure 4 The image shows the XRD pattern of the porous yttrium aluminum garnet ceramic prepared in Comparative Example 2. Detailed Implementation

[0045] The present invention will now be described in detail with reference to the embodiments.

[0046] The alumina used in each embodiment and comparative example is α-Al2O3 powder, and the yttrium oxide used is yttrium oxide powder.

[0047] Example 1

[0048] A YAG precursor photocurable slurry is composed of the following raw materials: 21.46g alumina powder, 28.54g yttrium oxide powder, 0.5g BYK111 dispersant, 10.83g 1,6-hexanediol diacrylate, 2.95g bis(trimethylolpropane) triacrylate, 3.86g polyethylene glycol 200, and 0.14g 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, wherein the D50 of the alumina powder is 0.2μm and the D50 of the yttrium oxide powder is 1μm.

[0049] The preparation method of the YAG precursor photocurable slurry includes the following steps:

[0050] (1) Mix alumina powder and yttrium oxide powder, add dispersant, use anhydrous ethanol and zirconia grinding balls as wet grinding media, and ball mill for 4 hours to obtain dispersant-modified mixed ceramic powder; the mass ratio of the sum of alumina powder and yttrium oxide powder, zirconia grinding balls and anhydrous ethanol is 1:2:2.

[0051] 2) 1,6-hexanediol diacrylate, bis(trimethylolpropane) triacrylate, trimethylolpropane triacrylate and polyethylene glycol 200 were thoroughly mixed using a planetary homogenizer to obtain a photosensitive resin.

[0052] 3) The dispersant-modified mixed ceramic powder is added to the photosensitive resin, and after thorough mixing and degassing using a vacuum degassing mixer, YAG precursor photocurable slurry is obtained.

[0053] Example 2

[0054] A YAG precursor photocurable slurry is composed of the following raw materials: 21.46 g of alumina powder, 28.54 g of yttrium oxide powder, 2.0 g of BYK111 dispersant, 5.90 g of 1,6-hexanediol diacrylate, 1.61 g of bis(trimethylolpropane) triacrylate, 2.10 g of polyethylene glycol 200, and 0.08 g of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, wherein the D50 of the alumina powder is 2 μm and the D50 of the yttrium oxide powder is 0.1 μm.

[0055] The preparation method of the YAG precursor photocurable slurry is the same as in Example 1.

[0056] Example 3

[0057] A YAG precursor photocurable slurry is composed of the following raw materials: 21.46 g of alumina powder, 28.54 g of yttrium oxide powder, 1.0 g of BYK111 dispersant, 7.19 g of 1,6-hexanediol diacrylate, 0.96 g of bis(trimethylolpropane) triacrylate, 2.56 g of polyethylene glycol 200, and 0.09 g of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, wherein the D50 of the alumina powder is 1 μm and the D50 of the yttrium oxide powder is 0.1 μm.

[0058] The preparation method of the YAG precursor photocurable slurry is the same as in Example 1.

[0059] Example 4

[0060] A YAG precursor photocurable slurry is composed of the following raw materials: 21.46g alumina powder, 28.54g yttrium oxide powder, 1.5g BYK111 dispersant, 8.81g 1,6-hexanediol diacrylate, 2.40g bis(trimethylolpropane) triacrylate, 3.14g polyethylene glycol 200, and 0.11g 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, wherein the D50 of the alumina powder is 0.5μm and the D50 of the yttrium oxide powder is 0.1μm.

[0061] The preparation method of the YAG precursor photocurable slurry is the same as in Example 1.

[0062] Example 5

[0063] A method for preparing porous YAG ceramics using the YAG precursor photocurable slurry from Example 1 includes the following steps:

[0064] 1) 3D printing was performed on the YAG precursor photocurable slurry to obtain a printed sample; the 3D printing conditions were: laser energy density 177 mJ / cm². 2 The layer thickness is 25μm, and the scanning rate is 2000mm / s;

[0065] 2) The printed samples were degreased using a 6-stage degreasing process under argon protection; specifically:

[0066] First stage: Heat from 20℃ to 110℃ at a heating rate of 1℃ / min and hold for 1 hour;

[0067] Second stage: Heat from 110℃ to 200℃ at a heating rate of 1℃ / min and hold for 1 hour;

[0068] The third stage: the temperature is increased from 200℃ to 350℃ at a heating rate of 1℃ / min and held for 1 hour;

[0069] Fourth stage: Increase the temperature from 350℃ to 400℃ at a heating rate of 0.2℃ / min and hold for 1 hour;

[0070] Fifth stage: Heat from 400℃ to 460℃ at a heating rate of 0.2℃ / min and hold for 4 hours;

[0071] Sixth step: Heat from 460℃ to 550℃ at a heating rate of 0.2℃ / min and hold for 1 hour, then proceed directly with the decarbonization process.

[0072] 3) The degreased printed sample was heated to 600℃ at a heating rate of 1℃ / min and held for 2 hours to remove carbon. Then, it was heated to 1550℃ at a heating rate of 5℃ / min and held for 1 hour for sintering. Then, it was cooled in the furnace to obtain porous YAG ceramic, which completely maintained the structure of the 3D printed sample. XRD test showed that it was entirely YAG phase.

[0073] Example 6

[0074] A method for preparing porous YAG ceramics using the YAG precursor photocurable slurry from Example 2 includes the following steps:

[0075] 1) 3D printing was performed on the YAG precursor photocurable slurry to obtain a printed sample; the 3D printing conditions were: laser energy density 757 mJ / cm². 2 The layer thickness is 100μm, and the scanning rate is 6000mm / s;

[0076] 2) The printed samples were degreased using a 6-stage degreasing process under argon protection; specifically:

[0077] First stage: Heat from 20℃ to 110℃ at a heating rate of 1℃ / min and hold for 1 hour;

[0078] Second stage: Heat from 110℃ to 200℃ at a heating rate of 1℃ / min and hold for 1 hour;

[0079] The third stage: the temperature is increased from 200℃ to 350℃ at a heating rate of 1℃ / min and held for 1 hour;

[0080] Fourth stage: Increase the temperature from 350℃ to 400℃ at a heating rate of 0.2℃ / min and hold for 1 hour;

[0081] Fifth stage: Heat from 400℃ to 460℃ at a heating rate of 0.2℃ / min and hold for 4 hours;

[0082] Sixth step: Heat from 460℃ to 550℃ at a heating rate of 0.2℃ / min and hold for 1 hour, then proceed directly with the decarbonization process.

[0083] 3) The degreased printed sample was heated to 600℃ at a heating rate of 1℃ / min and held for 2 hours to remove carbon. Then, it was heated to 1600℃ at a heating rate of 5℃ / min and held for 5 hours for sintering. Then, it was cooled in the furnace to obtain porous YAG ceramic, which completely maintained the structure of the 3D printed sample. XRD test showed that it was entirely YAG phase.

[0084] Example 7

[0085] A method for preparing porous YAG ceramics using the YAG precursor photocurable slurry from Example 3 includes the following steps:

[0086] 1) 3D printing was performed on the YAG precursor photocurable slurry to obtain a printed sample; the 3D printing conditions were: laser energy density 399 mJ / cm². 2 The layer thickness was 50 μm, and the scanning rate was 4000 mm / s;

[0087] 2) The printed samples were degreased using a 6-stage degreasing process under argon protection; specifically:

[0088] First stage: Heat from 20℃ to 110℃ at a heating rate of 1℃ / min and hold for 1 hour;

[0089] Second stage: Heat from 110℃ to 200℃ at a heating rate of 1℃ / min and hold for 1 hour;

[0090] The third stage: the temperature is increased from 200℃ to 350℃ at a heating rate of 1℃ / min and held for 1 hour;

[0091] Fourth stage: Increase the temperature from 350℃ to 400℃ at a heating rate of 0.2℃ / min and hold for 1 hour;

[0092] Fifth stage: Heat from 400℃ to 460℃ at a heating rate of 0.2℃ / min and hold for 4 hours;

[0093] Sixth step: Heat from 460℃ to 550℃ at a heating rate of 0.2℃ / min and hold for 1 hour, then proceed directly with the decarbonization process.

[0094] 3) The degreased printed sample was heated to 600℃ at a heating rate of 1℃ / min and held for 2 hours to remove carbon. Then, it was heated to 1600℃ at a heating rate of 5℃ / min and held for 2 hours for sintering. Then, it was cooled in the furnace to obtain porous YAG ceramic, which completely maintained the structure of the 3D printed sample.

[0095] Images of porous YAG ceramics of different shapes prepared in this embodiment are shown below. Figure 1 As shown.

[0096] The XRD diffraction pattern of the porous YAG ceramic prepared in this embodiment is as follows: Figure 2 As shown in the figure, the sintered part is entirely composed of the YAG phase after high-temperature sintering.

[0097] The SEM image of the porous YAG ceramic prepared in this embodiment is shown below. Figure 3 As shown in the figure, it has a microporous morphology.

[0098] Example 8

[0099] A method for preparing porous YAG ceramics using the YAG precursor photocurable slurry from Example 4 includes the following steps:

[0100] 1) 3D printing was performed on the YAG precursor photocurable slurry to obtain a printed sample; the 3D printing conditions were: laser energy density 566 mJ / cm². 2 The layer thickness was 70 μm, and the scanning rate was 4000 mm / s;

[0101] 2) The printed samples were degreased using a 6-stage degreasing process under argon protection; specifically:

[0102] First stage: Heat from 20℃ to 110℃ at a heating rate of 1℃ / min and hold for 1 hour;

[0103] Second stage: Heat from 110℃ to 200℃ at a heating rate of 1℃ / min and hold for 1 hour;

[0104] The third stage: the temperature is increased from 200℃ to 350℃ at a heating rate of 1℃ / min and held for 1 hour;

[0105] Fourth stage: Increase the temperature from 350℃ to 400℃ at a heating rate of 0.2℃ / min and hold for 1 hour;

[0106] Fifth stage: Heat from 400℃ to 460℃ at a heating rate of 0.2℃ / min and hold for 4 hours;

[0107] Sixth step: Heat from 460℃ to 550℃ at a heating rate of 0.2℃ / min and hold for 1 hour, then proceed directly with the decarbonization process.

[0108] 3) The degreased printed sample was heated to 600℃ at a heating rate of 1℃ / min and held for 2 hours to remove carbon. Then, it was heated to 1650℃ at a heating rate of 5℃ / min and held for 3 hours for sintering. Then, it was cooled in the furnace to obtain porous YAG ceramic, which completely maintained the structure of the 3D printed sample. XRD test showed that it was entirely YAG phase.

[0109] Comparative Example 1

[0110] A YAG precursor photocurable slurry is composed of the following raw materials: 21.46g alumina powder, 28.54g yttrium oxide powder, 1.0g BYK111 dispersant, 16.81g 1,6-hexanediol diacrylate, 4.58g bis(trimethylolpropane) triacrylate, 5.99g polyethylene glycol 200, and 0.21g 2,4,6-trimethylbenzoyl-diphenylphosphine oxide.

[0111] The preparation method of the YAG precursor photocurable slurry is the same as in Example 1.

[0112] The method for preparing porous YAG ceramics using the YAG precursor photocurable slurry in this comparative example is the same as in Example 7.

[0113] In this comparative example, the viscosity of the YAG precursor photocurable slurry was too low, resulting in slurry flow and poor interlayer bonding during printing. The preform deformed after degreasing. This is because the low solid content leads to greater shrinkage during degreasing, causing stress concentration and ultimately resulting in localized deformation.

[0114] Comparative Example 2

[0115] The rest is the same as in Example 7, except that step 3) is adjusted as follows:

[0116] The degreased printed sample was heated to 600℃ at a heating rate of 1℃ / min and held for 2 hours to remove carbon. Then, it was heated to 1500℃ at a heating rate of 5℃ / min and held for 2 hours for sintering.

[0117] In this comparative example, the XRD pattern of the sintered sample is as follows: Figure 4 As shown in the figure, in addition to the YAG phase, there are also some Y2O3 and Al2Y4O9 phases. Therefore, the sintering temperature is crucial for the formation of the complete YAG phase.

[0118] Comparative Example 3

[0119] The rest is the same as in Example 7, except that step 2) is adjusted to: degreasing the printed sample under the protection of argon gas, and the degreasing process is: heating to 550°C at 1°C / min and holding for 2 hours.

[0120] In this comparative example, the printed sample after degreasing showed defects in the blank. This was because the resin decomposed too quickly during the degreasing process, and a large amount of gas was generated that could not be discharged in time, resulting in cracks in the blank.

[0121] The above detailed description of a yttrium aluminum garnet precursor photocurable slurry and a method for preparing porous yttrium aluminum garnet ceramics using the above-described embodiments is illustrative rather than limiting. Several embodiments may be listed within the defined scope. Therefore, variations and modifications that do not depart from the overall concept of the present invention should be within the protection scope of the present invention.

Claims

1. A photocurable slurry containing a yttrium aluminum garnet precursor, characterized in that, The yttrium aluminum garnet precursor photocurable slurry comprises the following raw materials: a mixed ceramic powder composed of alumina and yttrium oxide, photosensitive resin, and dispersant; In the mixed ceramic powder, the mass percentage of alumina is 42.9% and the mass percentage of yttrium oxide is 57.1%. The photosensitive resin comprises the following raw materials: photosensitive monomer, initiator and plasticizer.

2. The yttrium aluminum garnet precursor photocurable slurry according to claim 1, characterized in that, The mass fraction of the mixed ceramic powder in the yttrium aluminum garnet precursor photocurable slurry is 70-85%.

3. The yttrium aluminum garnet precursor photocurable slurry according to claim 1, characterized in that, The amount of the dispersant used is 1-4% of the mass of the mixed ceramic powder; the dispersant is BYK111.

4. The yttrium aluminum garnet precursor photocurable slurry according to claim 1, characterized in that, The photosensitive monomer is composed of trimethylolpropane triacrylate and 1,6-hexanediol diacrylate in a mass ratio of 1:3-5.

5. The yttrium aluminum garnet precursor photocurable slurry according to any one of claims 1-4, characterized in that, In the photosensitive resin, the amounts of initiator and plasticizer are 0.5-2.0% and 20-30% of the mass of the photosensitive monomer, respectively.

6. The yttrium aluminum garnet precursor photocurable slurry according to any one of claims 1-4, characterized in that, The plasticizer is any one or more of polyethylene glycol 200 and polyethylene glycol 400; the initiator is 2,4,6-trimethylbenzoyl-diphenylphosphine oxide.

7. The method for preparing the yttrium aluminum garnet precursor photocurable slurry according to any one of claims 1-6, characterized in that, The preparation method includes the following steps: (1) Mix alumina and yttrium oxide, add a dispersant, and use anhydrous ethanol and zirconium oxide grinding balls as wet grinding media to ball mill to obtain dispersant-modified mixed ceramic powder; (2) Mix the photosensitive monomer, initiator and plasticizer evenly to obtain the photosensitive resin; (3) Add dispersant-modified mixed ceramic powder to photosensitive resin, mix thoroughly and then perform vacuum degassing to obtain yttrium aluminum garnet precursor photocurable slurry.

8. A method for preparing porous yttrium aluminum garnet ceramics using a photocurable slurry containing a yttrium aluminum garnet precursor as described in any one of claims 1-6, characterized in that, The preparation method includes the following steps: 1) The yttrium aluminum garnet precursor photocurable slurry as described in any one of claims 1-6 is used for 3D printing to obtain a printed sample; 2) The printed samples were degreased under the protection of an inert gas atmosphere; 3) After degreasing, the printed sample is heated to 580-620℃ at a heating rate of 0.5-1.5℃ / min and held for 1.5-2h to remove carbon. Then, it is heated to 1550-1650℃ at a heating rate of 3-8℃ / min and held for 1-5h to sinter, thus obtaining porous yttrium aluminum garnet ceramic.

9. The method according to claim 8, characterized in that, In step 1), the 3D printing conditions are: laser energy density 177-757 mJ / cm². 2 The layer thickness is 25-100μm, and the scanning rate is 2000-6000mm / s.

10. The method according to claim 8, characterized in that, In step 2), the degreasing process employs a 6-stage degreasing process, specifically as follows: First stage: Heat from 20℃ to 110℃ at a heating rate of 1℃ / min and hold for 1-4 hours; Second stage: Heat from 110℃ to 200℃ at a heating rate of 1℃ / min and hold for 1-4 hours; The third stage: heating from 200℃ to 350℃ at a heating rate of 1℃ / min and holding for 1-4 hours; Fourth stage: Increase the temperature from 350℃ to 400℃ at a heating rate of 0.2℃ / min and hold for 1-4 hours; Fifth stage: Increase the temperature from 400℃ to 460℃ at a heating rate of 0.2℃ / min and hold for 1-4 hours; Section 6: Heat from 460℃ to 550℃ at a heating rate of 0.2℃ / min and hold for 1-4 hours.

Citation Information

Patent Citations

  • Preparation method of yttrium aluminum garnet porous ceramic

    CN110002863A