CN112500141A - Method for preparing porous quartz ceramic by photocuring molding - Google Patents

Method for preparing porous quartz ceramic by photocuring molding Download PDF

Info

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
Authority
CN
China
Prior art keywords
photocuring
molding
quartz ceramic
porous quartz
preparing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202011297236.8A
Other languages
Chinese (zh)
Inventor
郑海
唐明亮
朱海奎
王海华
王一峰
汪洋
胡增涵
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Donghai Advanced Silicon Based Materials Institute Nanjing University Of Technology
Original Assignee
Donghai Advanced Silicon Based Materials Institute Nanjing University Of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Donghai Advanced Silicon Based Materials Institute Nanjing University Of Technology filed Critical Donghai Advanced Silicon Based Materials Institute Nanjing University Of Technology
Priority to CN202011297236.8A priority Critical patent/CN112500141A/en
Publication of CN112500141A publication Critical patent/CN112500141A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/14Shaped 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE 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
    • B33Y10/00Processes of additive manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE 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
    • B33Y70/00Materials specially adapted for additive manufacturing
    • B33Y70/10Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/06Porous 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
    • C04B38/063Preparing or treating the raw materials individually or as batches
    • C04B38/0635Compounding ingredients
    • C04B38/0645Burnable, meltable, sublimable materials
    • C04B38/067Macromolecular compounds
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects 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
    • C04B2235/6562Heating rate
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects 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
    • C04B2235/6567Treatment 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

Method for preparing porous quartz ceramic by photocuring molding
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.
CN202011297236.8A 2020-11-18 2020-11-18 Method for preparing porous quartz ceramic by photocuring molding Pending CN112500141A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011297236.8A CN112500141A (en) 2020-11-18 2020-11-18 Method for preparing porous quartz ceramic by photocuring molding

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011297236.8A CN112500141A (en) 2020-11-18 2020-11-18 Method for preparing porous quartz ceramic by photocuring molding

Publications (1)

Publication Number Publication Date
CN112500141A true CN112500141A (en) 2021-03-16

Family

ID=74956960

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011297236.8A Pending CN112500141A (en) 2020-11-18 2020-11-18 Method for preparing porous quartz ceramic by photocuring molding

Country Status (1)

Country Link
CN (1) CN112500141A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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
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

Patent Citations (7)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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

Similar Documents

Publication Publication Date Title
CN108706978B (en) Method for preparing silicon carbide ceramic matrix composite by combining spray granulation with 3DP and CVI
CN108455978B (en) Surface-toughened alumina fiber rigid heat-insulating tile multilayer composite material, coating composition, preparation method and application thereof
CN106278335B (en) A kind of manufacturing method of fiber alignment toughening ceramic based composites turbo blade
CN112500141A (en) Method for preparing porous quartz ceramic by photocuring molding
CN112047727B (en) Preparation method of 3D printing alumina ceramic material
CN103691330B (en) A kind of preparation technology of porous stainless steel membrane
CN110732672A (en) gradient metal-based porous material and preparation method and application thereof
CN108516730A (en) A kind of composition, preparation and its application for spraying 3D printing based on binder
CN112778020A (en) High-temperature porous ceramic and preparation method thereof
CN101302117B (en) Preparation of ordered big hole porous ceramic film material
CN110294636A (en) A kind of lightweight heat-proof metallurgy of nickel waste residue foamed ceramics and preparation method thereof
CN114213107A (en) 3D printing forming method based on ceramic material
Yang et al. Layered extrusion forming of complex ceramic structures using starch as removable support
CN110204318B (en) Method for enhancing strength of alumina porous material based on powder bed melting
CN115724663A (en) full-3D printing silicon carbide ceramic optical component and preparation method thereof
CN111253172B (en) Method for preparing porous ceramic material
CN116354729B (en) SiC ceramic part and preparation method and application thereof
CN107696233B (en) A kind of ceramics 3D printing equipment
CN113548896A (en) Method for manufacturing ceramic composite material and product thereof
CN112851385A (en) Continuous alumina fiber reinforced ceramic matrix composite with adjustable dielectric property and preparation method thereof
CN111302785A (en) High-performance microwave dielectric ceramic and photocuring manufacturing method thereof
CN114478054B (en) Porous ceramic and preparation method thereof
CN115521158A (en) Preparation method of high-air-permeability ceramic fiber filter tube
CN111943690B (en) Mullite mixed powder, preparation method thereof and application thereof in 3D printing
CN111646804B (en) Preparation method of hollow tube micro-lattice structure ceramic material

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination