CN106007791A - Porous ceramic and preparation method thereof - Google Patents

Porous ceramic and preparation method thereof Download PDF

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Publication number
CN106007791A
CN106007791A CN201610339747.9A CN201610339747A CN106007791A CN 106007791 A CN106007791 A CN 106007791A CN 201610339747 A CN201610339747 A CN 201610339747A CN 106007791 A CN106007791 A CN 106007791A
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porous ceramics
preparation
foaming
aqueous slurries
sintering
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周延春
王晓飞
向会敏
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China Academy of Launch Vehicle Technology CALT
Aerospace Research Institute of Materials and Processing Technology
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China Academy of Launch Vehicle Technology CALT
Aerospace Research Institute of Materials and Processing Technology
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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
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/10—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by using foaming agents or by using mechanical means, e.g. adding preformed foam
    • 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
    • C04B35/44—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 aluminates
    • 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
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C04B35/634—Polymers
    • C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63428—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds of ethylenically unsaturated dicarboxylic acid anhydride polymers, e.g. maleic anhydride copolymers
    • 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
    • C04B38/007—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore distribution, e.g. inhomogeneous distribution of pores
    • C04B38/0074—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore distribution, e.g. inhomogeneous distribution of pores expressed as porosity percentage
    • 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
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Abstract

The invention relates to Yb3Al5O12 porous ceramic and a preparation method thereof and belongs to the field of high-temperature porous heat-insulating ceramic materials. The preparation method includes: using Yb3Al5O12 ceramic powder, water, isobutylene-maleic anhydride copolymer and foamer (C12H25OSO3H N(C2H4OH)3 as raw materials; mixing and stirring the Yb3Al5O12 ceramic powder high in solid content, the water and the isobutylene-maleic anhydride copolymer accounting for 0.2-0.8wt% of the Yb3Al5O12 ceramic powder to form stable slurry; adding the foamer (C12H25OSO3H N(C2H4OH)3 of 0.05-2 vol%; strongly mechanically stirring the slurry containing the foamer for foaming; injecting into a metal or plastic die; curing and cross-linking at certain temperature to obtain a high-strength Yb3Al5O12 ceramic blank; sintering the blank at 1400-1700 DEG C without pressure to the Yb3Al5O12 porous ceramic.

Description

A kind of porous ceramics and preparation method thereof
Technical field
The present invention relates to a kind of Yb3Al5O12Porous ceramics and preparation method thereof, belongs to the heat insulation pottery of high temperature porous Ceramic material field.
Background technology
High temperature porous thermal insulation ceramics has the advantages such as low-density, high porosity, Heat stability is good so that they Large area at hypersonic aircraft, scramjet engine is heat insulation, seal and be catalyzed and the field such as filtration It is with a wide range of applications.These are applied, not only requires high porosity but also require high intensity.Therefore, How to obtain high porosity, the novel via pottery of high intensity is urgent problem.Document 1 (J.Am. Ceram.Soc.89:1771 1789 (2006)) report and prepare porous ceramic film material by template, literary composition Offer 2 (J.Eur.Ceram.Soc.35:1751 1759 (2015)) to report with partially sintering legal system Standby porous ceramic film material, document 3 (Philos.Trans.Roy.Soc.A, 364:109 124 (2006)) Report and prepare porous ceramic film material with direct foaming, document 4 (Int.Mater.Rev.57: 115 131 (2012)) report with sacrifice template method prepare porous ceramic film material, document 5 (J.Eur. Ceram.Soc.19:2059 2066 (1999)) and document 6 (Scripta Mater.62 (2010) 602 605) report with note solidification forming-foaming prepare porous ceramic film material.Note solidification forming-foaming is Note solidification forming is combined with foaming technique, the method need use surface dispersant, flocculation aid, catalyst, The multiple additives such as foaming agent, cross-linking agent, these additives can produce a large amount of harmful gas during removing.
The voidage of pottery prepared by the method for partially sintering is low, and template needs to remove template also can produce pollution, Directly the intensity of pottery prepared by foaming is low, and note solidification forming-foaming is owing to employing substantial amounts of organic interpolation Agent, discharges a large amount of toxic gas in sintering process.
And pottery prepared by above-mentioned method mostly is aluminium oxide ceramics and silicon oxide ceramics, its poor high temperature stability, Be not suitable for hypersonic aircraft, scramjet engine large area heat-barrier material on apply.
Summary of the invention
The technology of the present invention solves problem: overcome the deficiencies in the prior art, proposes a kind of Yb3Al5O12Many Hole pottery and preparation method thereof.
The technical solution of the present invention is:
A kind of porous ceramics, the molecular formula of this porous ceramics is Yb3Al5O12, the porosity of this porous ceramics For 60%-80%.
The intensity of this porous ceramics is 5-20MPa.
The gas permeability of this porous ceramics is 2 × 10-11-8×10-11m2。
The preparation method of a kind of porous ceramics, it is characterised in that step is:
(1) by Yb3Al5O12Powder, cross-linking agent mix with water, obtain aqueous slurries；
(2) in the aqueous slurries that step (1) obtains, add foaming agent, carry out strength and foam, contained There is the slip of foaming agent；
(3) slip that step (2) obtains is poured into and mould is noted solidification forming:
(4) base substrate of note solidification forming in step (3) is carried out crosslinking curing process；
(5) base substrate after step (4) crosslinking curing is dried process；
(6) by the Yb after step (5) dried3Al5O12Ceramic body carries out pressureless sintering, obtains Yb3Al5O12Porous ceramics.
In described step (1), the Yb of addition3Al5O12The quality of powder is the aqueous slurries quality obtained 45%-55%；The quality of the cross-linking agent added is Yb3Al5O12The 0.2%-0.8% of powder quality；Hand over Connection agent is isobutene .-maleic anhydride copolymer, and the molecular weight of isobutene .-maleic anhydride copolymer is The ratio of 55000-65000, isobutene. and maleic anhydride is 1:1, Yb3Al5O12Powder average Particle diameter is 0.6 μm, is stirred the aqueous slurries obtained, and mixing time is 0.5-3.0 hour, stirring Speed is 60-120 rev/min, obtains Yb after stirring3Al5O12Good stability, Yb3Al5O12Granule dispersion is all Even aqueous slurries.
In described step (2), in described step (2), the molecular formula of foaming agent is (C12H25OSO3H·N(C2H4OH)3, the volume of the foaming agent added be step (1) obtain water base The 0.05%-2% of the volume of slip；The condition of strength foaming is: mixing speed 900-1200 rev/min, sends out 0.1-0.5 hour bubble time.
In described step (3), described mould is resin die or stainless steel mould, and injection molding temperature is 20-35 DEG C, injection molding environment is air.
In described step (4), crosslinking curing condition is: crosslinking curing temperature is 30-45 DEG C, during solidification Between be 4-10 hour, curing environment is air.
In described step (5), drying condition is: baking temperature 35-85 DEG C, and drying time, 5-20 was little Time, dry environment is air.
In described step (6), pressureless sintering condition is: sintering temperature is 1400-1700 DEG C, sintering Time is 1-4 hour, and sintering atmosphere is air.
Beneficial effect
(1) method of the present invention uses dispersant and the solidifying agent system of note of non-toxic water soluble；
(2) present invention uses note solidification forming-foaming to prepare novel Yb3Al5O12Porous ceramics, Yb3Al5O12 The particle size of powder is 0.6 μm, and the note solidification forming agent of use is isobutene .-maleic anhydride copolymer, sends out Infusion is (C12H25OSO3H·N(C2H4OH)3.The molecular weight of isobutene .-maleic anhydride copolymer is The ratio of 55000-65000, isobutene. and maleic anhydride is 1:1, is a kind of nontoxic, tasteless helping Solidifying agent.Activated-COO in this copolymer-HN4 +Group and-CONH2Group, generates after hydrolysis -COOH group, can occur spontaneous crosslinking in air at room temperature, therefore without catalyst to be added and Initiator.
(3) in the present invention, the addition of isobutene .-maleic anhydride copolymer only accounts for Yb3Al5O12Powder 0.2%-0.8wt%, the content of foaming agent accounts for 0.05% 2vol% of slip.
(4) by Yb3Al5O12Powder mixes with flocculation aid isobutene .-maleic anhydride copolymer and deionized water Close, after long agitation is uniform, adds the foaming agent of 0.05% 2vol% (C12H25OSO3H·N(C2H4OH)3.After mechanical agitation is bubbled, pour into and mould is heated to uniform temperature shape Becoming gel base substrate, drying and high temperature sintering prepare novel Yb3Al5O12Porous ceramics.
(5) raw material used by the method for the present invention is Yb3Al5O12Ceramic powders, water, isobutene .-along fourth Alkene two anhydride copolymer and foaming agent (C12H25OSO3H·N(C2H4OH)3.By the Yb of high solids content3Al5O12 Ceramic powders, water, account for Yb3Al5O12The isobutene. of ceramic powders 0.2%-0.8wt%-maleic anhydride copolymerization Thing mix and blend forms stable slip, is subsequently adding the foaming agent of 0.05 2vol% (C12H25OSO3H·N(C2H4OH)3.To the slip strength mechanical agitation foaming containing foaming agent, then note Enter in metal or mould of plastics, after the solidification crosslinking under uniform temperature, obtain the Yb of high intensity3Al5O12 Ceramic body, finally can obtain Yb in 1-4 hour 1400-1700 DEG C of pressureless sintering3Al5O12Porous is made pottery Porcelain.
(6) the novel Yb that the present invention provides3Al5O12Porous ceramics and preparation method thereof have technique simple, Feature practical, eco-friendly, need not add catalyst, initiator, reduction in technical process Agent, high temperature sintering aid, dispersant etc., isobutene. used-maleic anhydride copolymer is nontoxic, tasteless, Good water solubility, can cross-link by spontaneous cure, foaming agent in room temperature, air (C12H25OSO3H·N(C2H4OH)3Foaming effect good, consumption is low.
(7) Yb prepared by the present invention3Al5O12Porous ceramics technical process is simple, at water base Yb3Al5O12 Ceramic slurry has only to add isobutene .-maleic anhydride copolymer and foaming agent (C12H25OSO3H·N(C2H4OH)3, it is not necessary to catalyst, dispersant, initiator, reducing agent etc. are multiple The complicated ingredients such as additive and operation.
(8) isobutene .-maleic anhydride copolymer that the present invention uses is nontoxic, tasteless, isobutene .-maleic Two anhydride copolymers and foaming agent (C12H25OSO3H·N(C2H4OH)3Usage amount little, to human body fanout free region, Yb3Al5O12Preparation and the foaming of ceramic slurry can be carried out in room temperature, air.
(9) Yb that the present invention provides3Al5O12The sintering process of porous ceramics is simple, it is not necessary to pressure sintering With protective atmosphere control, pressureless sintering can obtain the Yb of high intensity, high porosity in atmosphere3Al5O12 Porous ceramics.
(10) present invention passes through lot of experiments to Yb3Al5O12Porous ceramics is preparation technology be optimized, Especially aqueous slurries prepare, foam, note solidification forming, solidify, be dried and high temperature pressure-free sintering technique bar Part is optimized, and further increases Yb3Al5O12The porosity of porous ceramics and intensity.
(11) Yb that the present invention provides3Al5O12The preparation method technique of porous ceramics is simple, need not height Pressure equipment, it is easily achieved, there is stronger practicality.
(12) the present invention relates to high temperature porous heat-barrier material field, a kind of novel Yb3Al5O12 Porous ceramics and preparation method thereof, the novel Yb of described one3Al5O12It is high, strong that porous ceramics has the porosity The feature that degree is high, gas permeability is high, described preparation method is a kind of Yb utilizing high-volume fractional3Al5O12 Ceramic slurry prepared by powder, isobutene .-maleic anhydride copolymer and surfactant, through note solidification forming, sends out Bubble, 1400-1700 DEG C of pressureless sintering of high temperature obtains high porosity (55-85%), high intensity in 1-4 hour (compressive strength 15-100MPa, bending strength 5-20MPa), high gas permeability (4.3 × 10-13Extremely 7.8×10-11m2) Yb3Al5O12Porous heat-insulating pottery.The superhigh temperature that the present invention provides is heat insulation Yb3Al5O12The preparation method of pottery has the advantages that technique is simple, practical, is noting solidification forming and is sending out Need not during bubble add catalyst, cross-linking agent, initiator, reducing agent, isobutene .-maleic used Two anhydride copolymers are nontoxic, tasteless, good water solubility, can spontaneous cure crosslinking in room temperature, air；In nothing Pressure sintering process need not add sintering aid.
Accompanying drawing explanation
Fig. 1 (a) is that foaming agent is to Yb3Al5O12The impact of ceramic slurry Z-current potential, line 1 is Yb3Al5O12 Ceramic powders and water carry out the stability curve figure of mixed aqueous slurries, and line 2 is Yb3Al5O12Pottery The stability curve figure of the mixed aqueous slurries of powder, water and cross-linking agent, line 3 is Yb3Al5O12Pottery Powder, water, cross-linking agent and foaming agent carry out the stability curve figure of mixed aqueous slurries；
Fig. 1 (b) is Yb3Al5O12The viscosity of ceramic slurry and the graph of relation of rotating speed；Line 1 is Yb3Al5O12Ceramic powders and water carry out the viscosity curve figure of mixed aqueous slurries, and line 2 is Yb3Al5O12The viscosity curve figure of the mixed aqueous slurries of ceramic powders, water and cross-linking agent, line 3 is Yb3Al5O12Ceramic powders, water, cross-linking agent and foaming agent carry out the viscosity curve figure of mixed aqueous slurries；
Fig. 2 (a) burns through high temperature for adding the foaming agent that volume content is 0.05% and volume content is 0.1% Yb after knot3Al5O12The x-ray diffraction pattern of porous ceramics；
Fig. 2 (b) is Yb3Al5O12The relation of the density of porous ceramics and the porosity and foaming agents content；
Fig. 3 is the Yb of the different porosity3Al5O12The microstructure of porous ceramics, uses in preparation process The content of foaming agent is respectively (a) 0.005vol%, (b), 0.01vol%, (c) 0.1vol%, (d) 1 Vol%.The porosity is marked on the upper left corner of microstructure photograph；
Fig. 4 (a) is Yb3Al5O12The pass of the bending strength of porous ceramics and compressive strength density corresponding thereto System；
Fig. 4 (b) is Yb3Al5O12The gas permeability of porous ceramics and the relation of the porosity.
Detailed description of the invention
A kind of Yb3Al5O12Porous ceramics, the molecular formula of this porous ceramics is Yb3Al5O12, this porous ceramics The porosity be 60%-80%, intensity is 5-20MPa, and gas permeability is 2 × 10-11-8×10-11m2。
A kind of Yb3Al5O12The preparation method of porous ceramics, step is:
(1) by Yb3Al5O12Powder, cross-linking agent mix with water, obtain aqueous slurries, the material obtained Yb in slurry3Al5O12Solids content be 45-55%；The quality of cross-linking agent is Yb3Al5O12Powder quality 0.2%-0.8%；
(2) in the slip that step (1) obtains, add foaming agent, carry out strength and foam, obtain containing sending out The slip of infusion；
(3) slip that step (2) obtains is poured note solidification forming in mould into: described mould is resin mold Tool or stainless steel mould, injection molding temperature is 20-35 DEG C, and injection molding environment is air, it is not necessary to take isolation sky Gas measure；
(4) base substrate of note solidification forming in step (3) is carried out crosslinking curing process；
Described crosslinking curing condition is: crosslinking curing temperature is 30-45 DEG C, and hardening time is 4-10 hour, Curing environment is air；
(5) base substrate after step (4) crosslinking curing is dried process；
Described drying condition is: baking temperature 35-85 DEG C, 5-20 hour drying time, and dry environment is Air；
(6) by the Yb after step (5) dried3Al5O12Ceramic body carries out pressureless sintering to obtain Yb3Al5O12Porous ceramics；
Described pressureless sintering condition is: sintering temperature is 1400-1700 DEG C, and sintering time is 1-4 hour, Sintering atmosphere is air.
The Yb that will obtain after crosslinking curing3Al5O12Ceramic body is carried out.
In described step (1), cross-linking agent is isobutene .-maleic anhydride copolymer, isobutene .-maleic two The molecular weight of anhydride copolymer be the ratio of 55000-65000, isobutene. and maleic anhydride be 1:1, be A kind of nontoxic, tasteless flocculation aid；
Yb in described step (1)3Al5O12The mean diameter of powder is 0.6 μm；
Being stirred, in described step (1), the aqueous slurries obtained, mixing time is 0.5-3.0 hour, Mixing speed is 60-120 rev/min, obtains Yb after stirring3Al5O12Good stability, Yb3Al5O12Granule divides Dissipate uniform aqueous slurries；
In described step (2), the molecular formula of foaming agent is (C12H25OSO3H·N(C2H4OH)3, added The volume of the foaming agent entered is the 0.05%-2% of the volume of the slip that step (1) obtains；
In described step (2), the condition of strength foaming is: mixing speed 900-1200 rev/min, foaming 0.1-0.5 hour time.
The present invention is further detailed explanation with specific embodiment below in conjunction with the accompanying drawings:
Embodiment 1
Take the Yb of particle size 0.6 μm3Al5O12Ceramic powders, joins deionized water, Yb3Al5O12 The solids content of ceramic powders is 48%, adds 0.4wt% cross-linking agent isobutene .-maleic anhydride copolymer Stirring is mixed to form Yb3Al5O12Aqueous slurries, stirs 2.8 hours under the speed of 70 revs/min, obtains Yb3Al5O12Aqueous slurries that granule is uniformly dispersed stable (stability of slip and viscosity such as Fig. 1 (a) and Shown in Fig. 1 (b), from Fig. 1 (a) and Fig. 1 (b), add the dispersibility of the slip after cross-linking agent Preferably), at the Yb of mixed stability3Al5O12Slip adds the foaming agent of 0.5vol% (C12H25OSO3H·N(C2H4OH)3, within 0.1 hour, obtain 1200 revs/min of mixing speed strength foaming Foaming slip, by the Yb after strength foaming3Al5O12Aqueous slurries, 25 DEG C, air pours resin mold into Noting solidification forming, the most in atmosphere 30 DEG C of crosslinking curings 10 hours in tool, the viscosity of slip is relatively low and foaming Ability is strong, and when the volume content of foaming agent is increased to 1% by 0.01%, in foaming process, volume is original body Long-pending more than 500%, in the present embodiment, the volume content of foaming agent is 0.5%, and in foaming process, volume increases 400%.The Yb that will obtain after crosslinking curing3Al5O12Ceramic body 85 DEG C, air is dried Process and within 5 hours, obtain ceramic green, finally by the Yb after dried3Al5O12Green compact are at 1700 DEG C, sky In gas, pressureless sintering obtains the Yb that the porosity is 74% for 1 hour3Al5O12Porous ceramics；To the porous obtained Pottery carries out Mechanics Performance Testing, testing standard with reference to GB/T 14390-2008GB/T 6569-2006, Bending strength reaches 12MPa, compressive strength reaches 90MPa.
Embodiment 2
Take particle size 0.6 μm, solids content is the Yb of 55%3Al5O12Ceramic powders, adds deionization Water, 0.2wt% water crosslinking agent isobutene .-maleic anhydride copolymer stirring is mixed to form Yb3Al5O12Water base Slip, stirs 0.5 hour under the speed of 120 revs/min, obtains Yb3Al5O12Granule is uniformly dispersed stable Aqueous slurries, at the Yb of mixed stability3Al5O12Slip adds the foaming agent of 0.06vol% (C12H25OSO3H·N(C2H4OH)3, within 0.5 hour, sent out 900 revs/min of mixing speed strength foaming Foam material is starched, by the Yb after strength foaming3Al5O12Aqueous slurries, 20 DEG C, air pours resin die into Middle note solidification forming, the most in atmosphere 35 DEG C of crosslinking curings 8 hours, by obtain after crosslinking curing Yb3Al5O12Ceramic body 35 DEG C, air be dried process within 20 hours, obtain ceramic green, After by the Yb after dried3Al5O12Green compact 1400 DEG C, in air pressureless sintering within 4 hours, obtain gas Porosity is the Yb of 65%3Al5O12Porous ceramics, bending strength reaches 15MPa, compressive strength reaches 100 MPa。
Embodiment 3
Take particle size 0.6 μm, solids content is the Yb of 45%3Al5O12Ceramic powders, adds deionization Water, 0.8wt% water crosslinking agent isobutene .-maleic anhydride copolymer stirring is mixed to form Yb3Al5O12Water base Slip, stirs 1.0 hours under the speed of 100 revs/min, obtains Yb3Al5O12Granule is uniformly dispersed stable Aqueous slurries, at the Yb of mixed stability3Al5O12Slip adds the foaming agent of 1.0vol% (C12H25OSO3H·N(C2H4OH)3, within 0.4 hour, obtain 1000 revs/min of mixing speed strength foaming Foaming slip, by the Yb after strength foaming3Al5O12Aqueous slurries, 30 DEG C, air pours rustless steel into Mould is noted solidification forming, the most in atmosphere 45 DEG C of crosslinking curings 4 hours, by obtain after crosslinking curing Yb3Al5O12Ceramic body 50 DEG C, air be dried process within 10 hours, obtain ceramic green, After by the Yb after dried3Al5O12Green compact 1500 DEG C, in air pressureless sintering within 2 hours, obtain gas Porosity is the Yb of 87%3Al5O12Porous ceramics, its phase composition and the porosity such as Fig. 2 (a) and Fig. 2 (b) Shown in, the porous material prepared after high temperature sintering is pure Yb3Al5O12, microstructure such as Fig. 3 Shown in.
Embodiment 4
Take particle size 0.6 μm, solids content is the Yb of 50%3Al5O12Ceramic powders, adds deionization Water, 0.5wt% water crosslinking agent isobutene .-maleic anhydride copolymer stirring is mixed to form Yb3Al5O12Water base Slip, stirs 2.0 hours under the speed of 80 revs/min, obtains Yb3Al5O12Granule is uniformly dispersed stable Aqueous slurries, at the Yb of mixed stability3Al5O12Slip adds the foaming agent of 1.5vol% (C12H25OSO3H·N(C2H4OH)3, within 0.2 hour, obtain 1100 revs/min of mixing speed strength foaming Foaming slip, by the Yb after strength foaming3Al5O12Aqueous slurries, 35 DEG C, air pours rustless steel into Mould is noted solidification forming, the most in atmosphere 40 DEG C of crosslinking curings 6 hours, by obtain after crosslinking curing Yb3Al5O12Ceramic body 60 DEG C, air be dried process within 8 hours, obtain ceramic green, finally By the Yb after dried3Al5O12Green compact 1600 DEG C, in air pressureless sintering within 2 hours, obtain pore Rate is the Yb of 85%3Al5O12Porous ceramics, its bending strength reaches 5MPa, compressive strength reaches 16MPa, gas permeability reaches 7.8 × 10-11m2, as shown in Fig. 4 (a) and Fig. 4 (b).

Claims (10)

1. a porous ceramics, it is characterised in that: the molecular formula of this porous ceramics is Yb3Al5O12, these are many The porosity of hole pottery is 60%-80%.
A kind of porous ceramics the most according to claim 1, it is characterised in that: the intensity of this porous ceramics For 5-20MPa.
A kind of porous ceramics the most according to claim 1, it is characterised in that: the gas of this porous ceramics Permeability is 2 × 10-11-8×10-11m2。
4. the preparation method of the arbitrary described porous ceramics of claim 1,2 or 3, it is characterised in that Step is:
(1) by Yb3Al5O12Powder, cross-linking agent mix with water, obtain aqueous slurries；
(2) in the aqueous slurries that step (1) obtains, add foaming agent, carry out strength and foam, contained There is the slip of foaming agent；
(3) slip that step (2) obtains is poured into and mould is noted solidification forming:
(4) base substrate of note solidification forming in step (3) is carried out crosslinking curing process；
(5) base substrate after step (4) crosslinking curing is dried process；
(6) by the Yb after step (5) dried3Al5O12Ceramic body carries out pressureless sintering, obtains Yb3Al5O12Porous ceramics.
The preparation method of a kind of porous ceramics the most according to claim 4, it is characterised in that: described In step (1), the Yb of addition3Al5O12The quality of powder is the 45%-55% of the aqueous slurries quality obtained； The quality of the cross-linking agent added is Yb3Al5O12The 0.2%-0.8% of powder quality；Cross-linking agent be isobutene .- Maleic anhydride copolymer, the molecular weight of isobutene .-maleic anhydride copolymer is 55000-65000, different The ratio of butylene and maleic anhydride is 1:1, Yb3Al5O12The mean diameter of powder is 0.6 μm, right The aqueous slurries obtained is stirred, and mixing time is 0.5-3.0 hour, mixing speed be 60-120 turn/ Point, obtain Yb after stirring3Al5O12Good stability, Yb3Al5O12The finely dispersed aqueous slurries of granule.
The preparation method of a kind of porous ceramics the most according to claim 4, it is characterised in that: described In step (2), in described step (2), the molecular formula of foaming agent is (C12H25OSO3H·N(C2H4OH)3, The volume of the foaming agent added is the 0.05%-2% of the volume of the aqueous slurries that step (1) obtains；Strongly The condition of foaming is: mixing speed 900-1200 rev/min, foamed time 0.1-0.5 hour.
The preparation method of a kind of porous ceramics the most according to claim 4, it is characterised in that: described In step (3), described mould is resin die or stainless steel mould, and injection molding temperature is 20-35 DEG C, note Modular ring border is air.
The preparation method of a kind of porous ceramics the most according to claim 4, it is characterised in that: described In step (4), crosslinking curing condition is: crosslinking curing temperature is 30-45 DEG C, and hardening time is 4-10 Hour, curing environment is air.
The preparation method of a kind of porous ceramics the most according to claim 4, it is characterised in that: described In step (5), drying condition is: baking temperature 35-85 DEG C, 5-20 hour drying time, is dried ring Border is air.
The preparation method of a kind of porous ceramics the most according to claim 4, it is characterised in that: described Step (6) in, pressureless sintering condition is: sintering temperature is 1400-1700 DEG C, and sintering time is 1-4 Hour, sintering atmosphere is air.
CN201610339747.9A 2016-05-19 2016-05-19 Porous ceramic and preparation method thereof Pending CN106007791A (en)

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* Cited by examiner, † Cited by third party
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US11326071B2 (en) * 2016-12-07 2022-05-10 Nec Corporation Coating material and solidified body of coating material

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CN104446625A (en) * 2014-11-28 2015-03-25 中国科学技术大学先进技术研究院 High-porosity porous ceramic and preparation method thereof
CN104926357A (en) * 2015-06-03 2015-09-23 中国科学院上海硅酸盐研究所 Method for preparing Ca-ZrO2 foam ceramic through novel gel-casting system and Ca-ZrO2 foam ceramic
CN105130414A (en) * 2015-08-13 2015-12-09 航天材料及工艺研究所 Method for preparing ultra-high-temperature thermal-insulation Yb3Al5O12ceramic component

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CN104446625A (en) * 2014-11-28 2015-03-25 中国科学技术大学先进技术研究院 High-porosity porous ceramic and preparation method thereof
CN104926357A (en) * 2015-06-03 2015-09-23 中国科学院上海硅酸盐研究所 Method for preparing Ca-ZrO2 foam ceramic through novel gel-casting system and Ca-ZrO2 foam ceramic
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* Cited by examiner, † Cited by third party
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US11326071B2 (en) * 2016-12-07 2022-05-10 Nec Corporation Coating material and solidified body of coating material

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