CN112500141A - Method for preparing porous quartz ceramic by photocuring molding - Google Patents
Method for preparing porous quartz ceramic by photocuring molding Download PDFInfo
- Publication number
- CN112500141A CN112500141A CN202011297236.8A CN202011297236A CN112500141A CN 112500141 A CN112500141 A CN 112500141A CN 202011297236 A CN202011297236 A CN 202011297236A CN 112500141 A CN112500141 A CN 112500141A
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- Prior art keywords
- photocuring
- molding
- quartz ceramic
- porous quartz
- preparing
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- 239000000919 ceramic Substances 0.000 title claims abstract description 46
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000010453 quartz Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000000016 photochemical curing Methods 0.000 title claims abstract description 17
- 238000000465 moulding Methods 0.000 title claims abstract description 14
- 235000015895 biscuits Nutrition 0.000 claims abstract description 13
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 239000002270 dispersing agent Substances 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 238000007599 discharging Methods 0.000 claims abstract description 8
- 239000004519 grease Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229920005989 resin Polymers 0.000 claims abstract description 6
- 239000011347 resin Substances 0.000 claims abstract description 6
- 238000005516 engineering process Methods 0.000 claims abstract description 5
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims abstract description 5
- 238000000498 ball milling Methods 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- 238000004140 cleaning Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims 1
- 239000011148 porous material Substances 0.000 abstract description 7
- 238000002844 melting Methods 0.000 abstract description 2
- 230000008018 melting Effects 0.000 abstract description 2
- 238000009827 uniform distribution Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 description 6
- 238000009413 insulation Methods 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
- C04B38/067—Macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
Abstract
The invention discloses a method for preparing porous quartz ceramic by photocuring molding, which comprises the following specific steps: melting nano quartz powder as a raw material, epoxy acrylate as a light-cured resin, polyethylene glycol 400 as a dispersing agent, wherein the solid content is 20-45 wt%, the dispersing agent is 0.5-1.2 wt%, and preparing light-cured molding slurry through planetary ball milling and vacuum defoaming; preparing a porous ceramic biscuit by adopting a photocuring 3D forming technology; after cleaning and drying the biscuit, firstly carrying out 400-plus-600 ℃ grease discharging, and then carrying out 1300-plus-1500 ℃ calcination to obtain the porous quartz ceramic. The porous quartz ceramic prepared by the photocuring 3D forming technology has uniform pore structure size, uniform distribution and controllable density.
Description
Technical Field
The invention relates to a preparation method of quartz ceramic, in particular to a preparation method of porous quartz ceramic.
Background
The quartz ceramic, also called quartz glass ceramic, has as low a thermal conductivity as glass, only 2.1W/(m · K), and the thermal conductivity remains substantially unchanged with temperature change, so the quartz ceramic has excellent heat insulation performance below 1200 ℃, and is often made into light porous heat insulation materials, such as quartz heat insulation tiles of aerospace vehicles, heat insulation of rocket engine nozzles and other parts, and the like.
The main preparation process of the porous ceramic comprises the following steps: organic foam impregnation process, foaming process, pore-forming agent adding process, extrusion forming process and the like. The organic impregnation process can prepare porous ceramics with high porosity, but the ceramic framework is fragile and has a plurality of defects. The porous ceramic prepared by the foaming process has the characteristics of high porosity and high strength, and the prepared closed-pore porous ceramic has advantages, but has higher requirements on raw materials. The process of adding the pore-forming agent can be applied to porous ceramics with complex shapes, but the pore size is difficult to control, and the process is not suitable for preparing the porous ceramics with high porosity. The extrusion forming process is applied to manufacturing long and thin porous ceramics, the size and the shape of pores can be accurately controlled, but the method is not suitable for preparing the porous ceramics with complicated pore diameters.
The method for preparing the porous quartz ceramic by photocuring 3D molding not only can regulate and control the porous structure and distribution, but also can control the density.
Disclosure of Invention
The invention aims to provide a preparation method of porous quartz ceramic, and solves the problem of controlling the pore structure and distribution of the porous quartz ceramic.
The technical problem to be solved by the invention is realized by the following technical scheme, the invention relates to a method for preparing porous quartz ceramic by photocuring molding, which comprises the following steps:
(1) preparing forming slurry: preparing photocuring molding slurry by using fused nano quartz powder as a raw material, epoxy acrylate as photocuring resin and polyethylene glycol 400 as a dispersing agent through planetary ball milling and vacuum defoaming;
wherein: the raw material is fused nano quartz powder, the light-cured resin is epoxy acrylate, and the dispersing agent is polyethylene glycol 400; the solid content of the molding slurry is 20-40 wt%, and the dispersant content is 0.5-1.2 wt%;
(2) forming a ceramic biscuit: setting forming parameters by adopting a photocuring 3D forming technology to prepare a porous quartz ceramic biscuit;
(3) grease discharging and calcining: after being cleaned and dried, the porous quartz ceramic biscuit is firstly subjected to grease discharging at the temperature of 400-plus-one-year and then to calcination at the temperature of 1300-plus-one-year and 1500-year to obtain the porous quartz ceramic.
The invention has the beneficial effects that: the spherical fused nano quartz powder is adopted as a raw material, and the polyethylene glycol dispersant is matched, so that the prepared molding slurry has good fluidity, is convenient for photocuring 3D molding, and can not generate volume deformation caused by crystal transformation in the calcining process; compared with the existing main preparation process of the porous ceramic, the preparation method has the advantages of quick forming, high dimensional precision and the like, and the prepared porous quartz ceramic has uniform pore structure size and uniform distribution and can be regulated and controlled in density.
Detailed Description
Specific embodiments of the present invention will now be further described to facilitate further understanding of the present invention by those skilled in the art, and are not to be construed as limiting the claims thereto.
(1) Preparing forming slurry: melting nano quartz powder as a raw material, taking epoxy acrylate as a light-cured resin, carrying out planetary ball milling for 2 hours, and standing for 24 hours under the pressure of 0.1 kPa to remove bubbles of the slurry to obtain light-cured molding slurry, wherein the solid content of the molding slurry is 25 wt%, and the dispersant polyethylene glycol 4000.5 wt%;
(2) forming a porous quartz ceramic biscuit: adopting a photocuring 3D forming technology, wherein the forming technological parameters are exposure time of 20 s and layer thickness of 25 um, and preparing a porous quartz ceramic biscuit;
(3) grease discharging and calcining: washing a porous quartz ceramic biscuit by using absolute ethyl alcohol, then ultrasonically cleaning the porous quartz ceramic biscuit by using clear water for 10 min, and then drying the porous quartz ceramic biscuit for 30 min at 80 ℃; the grease discharging temperature is 400 ℃, the heating rate is 5 ℃/min, and the heat preservation time is 90 min; the calcining temperature is 1350 ℃, the heating rate is 2 ℃/min, the heat preservation time is 120 min, and finally the porous quartz ceramic is prepared.
Claims (7)
1. The method for preparing the porous quartz ceramic by photocuring molding comprises the following specific steps:
(1) preparing forming slurry: preparing photocuring molding slurry by using fused nano quartz powder as a raw material, epoxy acrylate as photocuring resin and polyethylene glycol 400 as a dispersing agent through planetary ball milling and vacuum defoaming;
(2) forming a ceramic biscuit: setting forming parameters by adopting a photocuring 3D forming technology to prepare a porous quartz ceramic biscuit;
(3) grease discharging and calcining: after cleaning and drying the biscuit, firstly carrying out 400-plus-one 600 ℃ grease discharging, and then carrying out 1300-plus-one 1500 ℃ calcination to obtain the porous quartz ceramic.
2. The photocuring-molding-prepared porous quartz ceramic according to claim 1, wherein: the raw material is fused nano quartz powder, the light-cured resin is epoxy acrylate, and the dispersing agent is polyethylene glycol 400.
3. The photocuring-molding-prepared porous quartz ceramic according to claim 1, wherein: the fused nano quartz powder is spherical, and the particle size D50 is 250-350 nm.
4. The photocuring-molding-prepared porous quartz ceramic according to claim 1, wherein: the solid content of the formed slurry is 20-40 wt%, and the dispersant content is 0.5-1.2 wt%.
5. The photocuring-molding-prepared porous quartz ceramic according to claim 1, wherein: the porous ceramic forming process is photocuring 3D forming, the exposure time is 20-40 s, and the layer thickness is 20-80 um.
6. The photocuring-molding-prepared porous quartz ceramic according to claim 1, wherein: the grease discharging temperature is 400-.
7. The photocuring-molding-prepared porous quartz ceramic according to claim 1, wherein: the calcination temperature is 1300-1500 ℃, the heating rate is 2-5 ℃/min, and the heat preservation time is 120-180 min.
Priority Applications (1)
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CN202011297236.8A CN112500141A (en) | 2020-11-18 | 2020-11-18 | Method for preparing porous quartz ceramic by photocuring molding |
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CN202011297236.8A CN112500141A (en) | 2020-11-18 | 2020-11-18 | Method for preparing porous quartz ceramic by photocuring molding |
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CN112500141A true CN112500141A (en) | 2021-03-16 |
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CN202011297236.8A Pending CN112500141A (en) | 2020-11-18 | 2020-11-18 | Method for preparing porous quartz ceramic by photocuring molding |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114349334A (en) * | 2022-01-24 | 2022-04-15 | 哈尔滨工业大学 | Photosensitive slurry for fused quartz photocuring molding and preparation method and curing molding method thereof |
CN116375459A (en) * | 2023-04-10 | 2023-07-04 | 唐山隆昌瓷业有限公司 | High-silicon functional porcelain and preparation method thereof |
Citations (7)
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CN103130525A (en) * | 2013-02-28 | 2013-06-05 | 西安交通大学 | Making method of high-toughness porous SiC ceramic complex part |
CN106431367A (en) * | 2016-09-07 | 2017-02-22 | 山东工业陶瓷研究设计院有限公司 | Photocurable fused silica slurry and preparing method and application thereof |
CN107032798A (en) * | 2017-05-31 | 2017-08-11 | 清华大学 | A kind of preparation method of the porous ceramic film material based on photocureable rapid shaping |
KR20170122100A (en) * | 2016-04-26 | 2017-11-03 | 고려대학교 산학협력단 | System for manufacturing three-dimensional porous scaffolds using photocurable slurry and method for manufacturing photocurable slurry |
CN107353036A (en) * | 2017-08-21 | 2017-11-17 | 广东工业大学 | A kind of porous silicon nitride ceramic based on increases material manufacturing technology, its preparation method and its application |
CN107500779A (en) * | 2017-08-21 | 2017-12-22 | 广东工业大学 | A kind of porous silicon-base structural ceramics and preparation method thereof |
US20180148378A1 (en) * | 2015-05-28 | 2018-05-31 | 3M Innovative Properties Company | Additive manufacturing process for producing ceramic articles using a sol containing nano-sized particles |
-
2020
- 2020-11-18 CN CN202011297236.8A patent/CN112500141A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103130525A (en) * | 2013-02-28 | 2013-06-05 | 西安交通大学 | Making method of high-toughness porous SiC ceramic complex part |
US20180148378A1 (en) * | 2015-05-28 | 2018-05-31 | 3M Innovative Properties Company | Additive manufacturing process for producing ceramic articles using a sol containing nano-sized particles |
KR20170122100A (en) * | 2016-04-26 | 2017-11-03 | 고려대학교 산학협력단 | System for manufacturing three-dimensional porous scaffolds using photocurable slurry and method for manufacturing photocurable slurry |
CN106431367A (en) * | 2016-09-07 | 2017-02-22 | 山东工业陶瓷研究设计院有限公司 | Photocurable fused silica slurry and preparing method and application thereof |
CN107032798A (en) * | 2017-05-31 | 2017-08-11 | 清华大学 | A kind of preparation method of the porous ceramic film material based on photocureable rapid shaping |
CN107353036A (en) * | 2017-08-21 | 2017-11-17 | 广东工业大学 | A kind of porous silicon nitride ceramic based on increases material manufacturing technology, its preparation method and its application |
CN107500779A (en) * | 2017-08-21 | 2017-12-22 | 广东工业大学 | A kind of porous silicon-base structural ceramics and preparation method thereof |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114349334A (en) * | 2022-01-24 | 2022-04-15 | 哈尔滨工业大学 | Photosensitive slurry for fused quartz photocuring molding and preparation method and curing molding method thereof |
CN116375459A (en) * | 2023-04-10 | 2023-07-04 | 唐山隆昌瓷业有限公司 | High-silicon functional porcelain and preparation method thereof |
CN116375459B (en) * | 2023-04-10 | 2024-05-03 | 唐山隆昌瓷业有限公司 | High-silicon functional porcelain and preparation method thereof |
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