CN105130414B - A kind of method for preparing the heat-insulated Yb3Al5O12 ceramic components of superhigh temperature - Google Patents
A kind of method for preparing the heat-insulated Yb3Al5O12 ceramic components of superhigh temperature Download PDFInfo
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Abstract
The present invention provides one kind and prepares the heat-insulated Yb of superhigh temperature3Al5O12The method of ceramic component, it comprises the following steps：(1) raw material is Yb2O3And Al2O3Powder, Yb is obtained through high temperature solid state reaction3Al5O12Ceramic powders；(2) by Yb3Al5O12Ceramic powders, water and isobutene maleic anhydride copolymer are mixed to form stable Yb3Al5O12Ceramic aqueous slurry；Yb is obtained after cold curing is crosslinked3Al5O12Ceramic green；(3) finally at 1450~1680 DEG C, sinter 1~4 hour, sintering atmosphere is Ar gas or air, you can obtain the Yb of the complicated shape of densification3Al5O12Superhigh temperature thermal insulation ceramicses element.Yb provided by the invention3Al5O12The preparation method technique of superhigh temperature thermal insulation ceramicses element is simple, does not need high-tension apparatus, is easily achieved, and has stronger practicality.
Description
Technical field
The invention belongs to superhigh temperature thermal insulation ceramicses technical field, and in particular to one kind is coagulated with single water-soluble non-toxic additive
Glue casting prepares the heat-insulated Yb of superhigh temperature3Al5O12The method of ceramic component.
Background technology
Yb3Al5O12Superhigh temperature thermal insulation ceramicses have high-melting-point (2000 DEG C), moderate density (solid density 6.67g/cm3,
With aoxidizing the yttrium partially stabilized close (6.46g/cm of zirconium oxide (YSZ)3), (theoretical minimum thermal conductivity is 1.22W/ to lower thermal conductivity
M.K, the theoretical minimum thermal conductivity less than YSZ are 1.49W/m.K), relatively low modulus of elasticity (282GPa) and modulus of shearing
(114GPa) and thermal coefficient of expansion (8.22 × 10 close YSZ-6/ K), good high temperature resistance vapor corrosion performance etc. is excellent
Combination property, turn into the high temperature insulating of hypersonic aircraft, high warm seal, the water resistant on blade of aviation engine surface and steam
Vapour corrosion resistant coating, silicon based ceramic and composite (including SiC, Si3N4, C/SiC, SiC/SiC) Environmental Barrier Coatings on Si-based Ceramics candidate's material
Material.Then the high temperature insulating as hypersonic aircraft, high warm seal flexible member material, realize complicated shape it is low into
This preparation is extremely important.But there is presently no complicated shape Yb3Al5O12The preporm of superhigh temperature thermal insulation ceramicses and preparation side
The report of method.
[the Opt.Mater.33 of document 1:1179-1184 (2011)] report and utilize aluminum nitrate and Yb2O3For raw material, use
Sol-gel process prepares Yb3Al5O12Powder, this method low yield, synthesis cycle length, and it is not involved with Yb3Al5O12Block
The preparation of material.[the Ceram.Inter.35 of document 2:25-27 (2009)] report with coprecipitation method, i.e., in metal salt solution
In be gradually added into the hydroxide precipitation that urea obtains Al, Yb, through washing repeatedly, dry, final high temperature calcines to obtain
Yb3Al5O12Powder.The process of this method is complicated, low yield, and is also not involved with Yb3Al5O12The preparation of block materials.It is multiple
The forming method of miscellaneous shaped ceramic mainly includes the methods of dry-pressing formed, injection moulding, injection forming, gel casting forming.It is dry
Molded cost is low, but is difficult to ensure that even intensity for the product of complicated shape；Injection moulding is suitable for small size, complexity
The product molding of shape, but due to containing substantial amounts of additive in the ceramic body of preparation, high temperature de-waxing process can produce to environment
Raw pollution, while it is difficult to ensure that the dimensional accuracy of product.Injection forming is primarily adapted for use in the hollw article for preparing complicated shape,
Shaping to solid base substrate, the density of core are difficult to ensure that.
Gel casting forming or note solidification forming are a kind of potteries of U.S.'s Oak Ridge National Laboratory invention the 1990s
Porcelain billet body precision molding technology (document 3 [and Am.Ceram.Soc.Bull, 70:1641-1649 (1991)]), the technology will pass
The ceramic grout forming technique of system and the theoretical ingenious combination of macromolecule, make it possible the near-net-shape of complicated shape.Note
Note the practical of solidification forming, the green body quality of water-based slurry are good in solidification forming method.But the note solidification forming of water-based slurry is usual
Acrylamide monomer, N are needed, N ' methylene-bisacrylamides crosslinking agent, tetramethylethylenediamine catalyst, also needs to add in addition
The multiple additives such as dispersant, initiator, reducing agent, pH value regulator, and acrylamide and its derivative have moderate malicious
Property, the central nervous system of people is endangered, has strong stimulation effect to eye, skin and mucous membrane.In order to solve complicated shape high temperature insulating,
High warm seal Yb3Al5O12The formation problems of flexible member, while overcome the toxicity of acrylamide system and slurry to prepare
Need to add in journey crosslinking agent, catalyst, dispersant, initiator, reducing agent, the multiple additives such as pH value regulator it is complicated into
Point and process, the invention provides a kind of only with single water-soluble non-toxic additive isobutene-maleic anhydride copolymer
Realize that gel casting forming prepares the heat-insulated Yb of complicated shape superhigh temperature in room temperature, air3Al5O12The method of ceramics.
The content of the invention
It is an object of the invention to provide a kind of prepared only with single water-soluble non-toxic additive gel casting to surpass
High temperature insulating Yb3Al5O12The method of ceramics.
Realize the technical scheme of the object of the invention：One kind prepares the heat-insulated Yb of superhigh temperature3Al5O12The method of ceramic component, its
Comprise the following steps：
(1) raw material is Yb2O3And Al2O3Powder, Yb is obtained through high temperature solid state reaction3Al5O12Ceramic powders；Described
Yb2O3And Al2O3The mol ratio of dosage is Yb2O3：Al2O3=(3.01~3.05)：5；The reaction temperature of described high temperature solid state reaction
Spend for 1000-1350 DEG C, the reaction time is 1-4 hours；
(2) by step (1) obtained by Yb3Al5O12Ceramic powders, water and isobutene-maleic anhydride copolymer mixing shape
Into stable Yb3Al5O12Ceramic aqueous slurry；At room temperature, Yb in air3Al5O12Ceramic aqueous slip casting is to metal die
In, obtain Yb after cold curing is crosslinked3Al5O12Ceramic green；
Described Yb3Al5O12Yb in ceramic aqueous slurry3Al5O12Solids content be 45-55wt%, crosslinking agent isobutyl
The content of alkene-maleic anhydride copolymer is 0.1-0.8wt%, and remaining is water；
(3) finally at 1450~1680 DEG C, sinter 1~4 hour, sintering atmosphere is Ar gas or air, you can obtain fine and close
Complicated shape Yb3Al5O12Superhigh temperature thermal insulation ceramicses element.
One kind as described above prepares the heat-insulated Yb of superhigh temperature3Al5O12The method of ceramic component, this method step (1) are specific
For：By raw material Yb2O3And Al2O3Powder weighing, mixing, mixing condition are：Anhydrous ethanol medium, rotating speed turn for 80-200/, mix
The material time is 24-48 hours；Then processing is dried in well mixed raw material, drying temperature is 20~40 DEG C, when drying
Between be 12~24 hours；By the raw material after drying process, in atmosphere, reaction temperature is 1000~1350 DEG C, the reaction time 1
~4 hours, Yb is made3Al5O12Ceramic powders.
One kind as described above prepares the heat-insulated Yb of superhigh temperature3Al5O12The method of ceramic component, this method step (2) are specific
For：By the Yb obtained by step (1)3Al5O12Ceramic powders planetary ball mill ball milling, ball-milling medium are absolute ethyl alcohol, ball milling
Time is 24~36 hours, and rotating speed is 200~300 revs/min；Yb3Al5O12Yb in ceramic aqueous slurry3Al5O12Solids content
For 45~55wt%, the content of crosslinking agent isobutene-maleic anhydride copolymer is 0.1~0.8wt%, Yb3Al5O12Ceramic water
The Ball-milling Time of base-material slurry is 0.1~5.0 hour, obtains that stability is good, the finely dispersed Yb of particle after ball milling3Al5O12It is water base
Slurry；Again by Yb3Al5O12Mould used in ceramic aqueous slurry note solidification forming is stainless steel mould, and injection molding temperature is room temperature 20-
38 DEG C, injection molding environment is air, it is not necessary to takes isolation air measure；Then by Yb3Al5O12The crosslinking of ceramic aqueous slurry is consolidated
Change, solidification temperature is 20~45 DEG C, and hardening time is 0.5~8 hour, and curing environment is air；The height obtained after crosslinking curing
Intensity Yb3Al5O12The drying temperature of ceramic body is 35~85 DEG C, and drying time is 5~20 hours, obtains Yb3Al5O12Ceramics
Green compact.
One kind as described above prepares the heat-insulated Yb of superhigh temperature3Al5O12The method of ceramic component, the crosslinking agent used in this method
Isobutene-maleic anhydride copolymer, mean molecule quantity are 55000-65000, and the ratio of isobutene and maleic anhydride is 1：
1。
Effect of the invention is that：
The present invention is that isobutene-maleic anhydride copolymer forms aqueous slurries note with single water-soluble non-toxic additive
Solidification forming prepares the heat-insulated Yb of superhigh temperature3Al5O12The method of ceramic component.Raw material used in this method is Yb2O3And Al2O3Powder,
Yb is obtained through high temperature solid state reaction3Al5O12Ceramic powders, by Yb3Al5O12Ceramic powders, water and isobutene-maleic anhydride are common
Polymers is mixed to form stable slurry, is poured at room temperature, in air in metal die, height is obtained after cold curing is crosslinked
The Yb of intensity, complicated shape3Al5O12Ceramic green, finally it can obtain answering for densification in 1450-1680 DEG C of sintering 1-4 hour
The Yb of miscellaneous shape3Al5O12Superhigh temperature thermal insulation ceramicses element.Specific advantage is as follows：
(1) present invention is first with Yb2O3And Al2O3Powder is raw material, by weighing, wet-mixing, high temperature solid state reaction close
Prepared into, aqueous slurries, note solidification forming, solidification, drying and high temperature pressure-free sintering obtain the Yb of complicated shape3Al5O12Superhigh temperature
Thermal insulation ceramicses element, through analysis shows Yb3Al5O12Superhigh temperature thermal insulation ceramicses have purity height, intensity is high, thermal conductivity is low, shape
The advantages that can accurately being controlled with size.
(2) present invention prepares the Yb of complicated shape3Al5O12Superhigh temperature thermal insulation ceramicses component technology process is simple, water base
Yb3Al5O12A kind of isobutene-maleic anhydride copolymer is only needed in superhigh temperature ceramics slurry, it is not necessary to catalyst, disperse
The complicated ingredients such as the multiple additives such as agent, initiator, reducing agent and process.
(3) isobutene-maleic anhydride copolymer that the present invention uses is nontoxic, tasteless, and usage amount is small, to human body without wound
Evil；The Yb of preparation3Al5O12Superhigh temperature thermal insulation ceramicses slurry in room temperature, air can spontaneous crosslinking curing, the ceramics after solidification
Blank strength is high, machinability is strong.
(4) solid state reaction kinetics temperature provided by the invention is relatively low, and high-purity can be obtained at 1000-1300 DEG C
Yb3Al5O12Superhigh temperature powder.
(5) Yb of the present invention by lot of experiments to complicated shape3Al5O12Superhigh temperature thermal insulation ceramicses element preparation technology enters
Gone the composition of optimization, especially raw material, solid state reaction kinetics, aqueous slurries prepare, note solidification forming, solidification, drying and high temperature
The process conditions of pressureless sintering are optimized, and further increase Yb3Al5O12Superhigh temperature thermal insulation ceramicses component size and shape
Control accuracy.
(6) Yb provided by the invention3Al5O12The preparation method technique of superhigh temperature thermal insulation ceramicses element is simple, does not need height
Pressure equipment, it is easily achieved, there is stronger practicality.
Brief description of the drawings
Fig. 1 is the molecular structure (Fig. 1 (a)) for isobutene-maleic anhydride copolymer that the present invention uses, using containing isobutyl
The water-based slurry note solidification forming of alkene-maleic anhydride copolymer forms the schematic diagram of complicated shape ceramic body process.
Fig. 2 be the Zeta potential of the water-based slurry containing isobutene-maleic anhydride copolymer that is prepared of the present invention with
The relation of slurry pH value.Add 0.4wt% and 0.8wt% isobutene-maleic anhydride copolymer make isopotential point respectively from
PH=7.4 moves on to pH=5.2 and pH=3.3.
Fig. 3 is the water-based slurry viscosity and shear speed containing isobutene-maleic anhydride copolymer that the present invention is prepared
The relation of rate, built-in picture are respectively shear thickening and shear shinning model.
Fig. 4 (a) be isobutene in the water-based slurry containing isobutene-maleic anhydride copolymer that is prepared of the present invention-
Influence of the content of maleic anhydride copolymer to storage modulu；Fig. 4 (b) is the isobutyl containing 0.4wt% that the present invention is prepared
The solidification temperature of the water-based slurry of alkene-maleic anhydride copolymer and the relation for triggering the time.
Fig. 5 be the water-based slurry containing isobutene-maleic anhydride copolymer that is prepared of the present invention is cured, dry after
The microstructure photograph of obtained base substrate, built-in picture represent the controllability of complicated shape near net-shape and can processed respectively
Property.
Fig. 6 is the Yb that the present invention is prepared3Al5O12The microstructure photograph of superhigh temperature thermal insulation ceramicses element, it is built-in
X-ray diffraction pattern illustrates Yb in high-temperature sintering process3Al5O12Superhigh temperature thermal insulation ceramicses are not decomposed, stability is good.
Embodiment
The heat-insulated Yb of superhigh temperature is prepared to one kind of the present invention with specific embodiment below in conjunction with the accompanying drawings3Al5O12Ceramic component
Method is described in further detail：
Embodiment 1
One kind of the present invention prepares the heat-insulated Yb of superhigh temperature3Al5O12The method of ceramic component, it comprises the following steps：
(1) by Yb2O3And Al2O3Powder is according to Yb2O3：Al2O3=3.01:5 mol ratios are weighed, and absolute ethyl alcohol are added, with rolling
Cartridge type batch mixer is mixed 48 hours, and rotating speed is 80/ turn, and well mixed raw material is dried 24 hours at 20 DEG C and obtains Yb2O3With
Al2O3Mixed-powder, by the Yb after drying process2O3And Al2O3Mixed-powder is placed in molybdenum disilicide stove, is heated in atmosphere
To 1050 DEG C, it is Yb that insulation, which obtains principal phase in 4 hours,3Al5O12Superhigh temperature thermal insulation ceramicses powder.
(2) using absolute ethyl alcohol as medium planetary ball mill ball milling by step (1) obtained by Yb3Al5O12Ceramic powders
Ball milling 36 hours, rotating speed are 200 revs/min, obtain the Yb that granularity is less than 1 μm3Al5O12Superhigh temperature thermal insulation ceramicses powder.According to
Yb3Al5O12Solids content be 45wt%, the content of isobutene-maleic anhydride copolymer accounts for Yb3Al5O120.3wt% match somebody with somebody
Yb processed3Al5O12Ceramic aqueous slurry, slurry is with 300 revs/min of ball millings 0.1 hour, the slurry stablized, then by Yb3Al5O12
(injection molding temperature is 25 DEG C of room temperature, and injection molding environment is air, it is not necessary to takes isolation in ceramic aqueous slurry injection stainless steel mould
Air measure), it is crosslinked 8 hours in 20 DEG C of air sets and obtains Yb3Al5O12Ceramic body, in 35 DEG C, drying in 20 hours.
(3) finally in 1680 DEG C, Ar gas pressureless sintering obtain within 1 hour relative density 98% fine and close superhigh temperature it is heat-insulated
Yb3Al5O12Ceramics.
The molecular formula of isobutene-maleic anhydride copolymer, its effect and note solidification forming process in solidification forming is noted is such as
Shown in Fig. 1.
The additive of the present invention is isobutene-maleic anhydride copolymer, nontoxic, tasteless, molecular weight 55000-
65000, the ratio of isobutene and maleic anhydride is 1 in copolymer：1, active-COO in the copolymer-HN4 +Group and-
CONH2Group, generated after hydrolysis-COOH group.Because the presence of these groups causes Yb3Al5O12Ceramic powders are containing isobutyl
Stability is good in the aqueous solution of alkene-maleic anhydride copolymer, therefore need not additionally add surface dispersant.In addition, isobutyl
It can occur spontaneous crosslinking in the alkene-air of maleic anhydride copolymer in aqueous at room temperature, therefore without needing to add
Catalyst and initiator.The molecular structure of isobutene-maleic anhydride copolymer, spontaneous crosslinking close note solidification forming process such as Fig. 1
It is shown.
Embodiment 2
One kind of the present invention prepares the heat-insulated Yb of superhigh temperature3Al5O12The method of ceramic component, it comprises the following steps：
(1) by Yb2O3And Al2O3Powder is according to Yb2O3：Al2O3=3.02:5 mol ratios are weighed, and absolute ethyl alcohol are added, with rolling
Cartridge type batch mixer is mixed 36 hours, and rotating speed is 100/ turn, and well mixed raw material is dried 12 hours at 35 DEG C and obtains Yb2O3With
Al2O3Mixed-powder, by the Yb after drying process2O3And Al2O3Mixed-powder is placed in molybdenum disilicide stove, is heated in atmosphere
1250 DEG C, insulation obtains the Yb of high-purity in 2 hours3Al5O12Superhigh temperature thermal insulation ceramicses powder.
(2) it is medium planetary ball mill ball milling by Yb using absolute ethyl alcohol3Al5O12Ceramic powders ball milling 24 hours, turn
Speed is 300 revs/min, obtains the Yb that granularity is less than 1 μm3Al5O12Superhigh temperature thermal insulation ceramicses powder, according to Yb3Al5O12Solid
Content is 50%, and the content of isobutene-maleic anhydride copolymer accounts for Yb3Al5O120.4 and 0.8wt% prepare Yb3Al5O12Pottery
Porcelain water-based slurry, slurry was with 200 revs/min of ball millings 0.5 hour, the slurry stablized, add as shown in Figure 2 0.4wt% and
0.8wt% isobutene-maleic anhydride copolymer makes isopotential point move on to pH=5.2 and pH=3.3 from pH=7.4 respectively,
In pH=7, the Zeta potential difference of the slurry of 0.4wt% and 0.8wt% isobutene-maleic anhydride copolymer is added
For -35mV and -60mV, illustrate that the dispersiveness of slurry and stability are all fine.By isobutene-maleic anhydride containing 0.8wt%
The Yb of copolymer3Al5O12(injection molding temperature is 20 DEG C of room temperature, and injection molding environment is sky in ceramic aqueous slurry injection stainless steel mould
Gas, it is not necessary to take the measure of isolation air), it is crosslinked 2 hours in 30 DEG C of air sets and obtains Yb3Al5O12Ceramic body, through 50
DEG C, drying in 10 hours.
(3) finally in 1600 DEG C, air pressureless sintering obtain within 4 hours relative density 97% fine and close superhigh temperature it is heat-insulated
Yb3Al5O12Ceramics.
Embodiment 3
One kind of the present invention prepares the heat-insulated Yb of superhigh temperature3Al5O12The method of ceramic component, it comprises the following steps：
(1) by Yb2O3And Al2O3Powder is according to Yb2O3：Al2O3=3.03:5 mol ratios are weighed, and absolute ethyl alcohol are added, with rolling
Cartridge type batch mixer is mixed 30 hours, and rotating speed is 150/ turn, and well mixed raw material is dried 12 hours at 40 DEG C and obtains Yb2O3With
Al2O3Mixed-powder, by the Yb after drying process2O3And Al2O3Mixed-powder is placed in molybdenum disilicide stove, is heated in atmosphere
1350 DEG C, insulation obtains the Yb of high-purity in 1 hour3Al5O12Superhigh temperature thermal insulation ceramicses powder.
(2) it is medium planetary ball mill ball milling by Yb using absolute ethyl alcohol3Al5O12Ceramic powders ball milling 30 hours, turn
Speed is 280 revs/min, obtains the Yb that granularity is less than 1 μm3Al5O12Superhigh temperature thermal insulation ceramicses powder, according to Yb3Al5O12Solid
Content is 50%, and the content of isobutene-maleic anhydride copolymer accounts for Yb3Al5O120.4,0.6 and 0.8wt% prepare
Yb3Al5O12Ceramic aqueous slurry, the viscosity of slurry and the relation of shearing are as shown in figure 3, add isobutene-maleic two
The content of anhydride copolymer is higher, and viscosity is lower, and the mobility of slurry is better.0.6wt% isobutenes-maleic anhydride copolymerization will be contained
The slurry of thing by Yb3Al5O12In ceramic aqueous slurry injection stainless steel mould, it is crosslinked 1 hour in 35 DEG C of air sets
To Yb3Al5O12Ceramic body, through 85 DEG C, drying in 5 hours.
(3) finally in 1650 DEG C, air pressureless sintering obtain within 3 hours relative density 98% fine and close superhigh temperature it is heat-insulated
Yb3Al5O12Ceramics.
Embodiment 4
One kind of the present invention prepares the heat-insulated Yb of superhigh temperature3Al5O12The method of ceramic component, it comprises the following steps：
(1) by Yb2O3And Al2O3Powder is according to Yb2O3：Al2O3=3.04:5 mol ratios are weighed, and absolute ethyl alcohol are added, with rolling
Cartridge type batch mixer is mixed 28 hours, and rotating speed is 180/ turn, and well mixed raw material is dried 24 hours at 25 DEG C and obtains Yb2O3With
Al2O3Mixed-powder, by the Yb after drying process2O3And Al2O3Mixed-powder is placed in molybdenum disilicide stove, is heated in atmosphere
1300 DEG C, insulation obtains the Yb of high-purity in 3 hours3Al5O12Superhigh temperature thermal insulation ceramicses powder.
(2) it is medium planetary ball mill ball milling by Yb using absolute ethyl alcohol3Al5O12Ceramic powders ball milling 28 hours, turn
Speed is 250 revs/min, obtains the Yb that granularity is less than 1 μm3Al5O12Superhigh temperature thermal insulation ceramicses powder, according to Yb3Al5O12Solid
Content is 50%, and the content of isobutene-maleic anhydride copolymer accounts for Yb3Al5O120.4,0.6 and 0.8wt% prepare
Yb3Al5O12Shown in ceramic aqueous slurry, the storage modulu of slurry and the relation of time such as Fig. 4 (a), isobutene-maleic is added
The content of two anhydride copolymers is higher, and induction time is longer.As shown in Fig. 4 (b), temperature is higher, and induction time is shorter, and solidification is got over
It hurry up.By the slurry of isobutene containing 0.4wt%-maleic anhydride copolymer by Yb3Al5O12Ceramic aqueous slurry injects stainless steel
In mould, it is crosslinked 0.5 hour in 45 DEG C of air sets and obtains Yb3Al5O12Ceramic body.Through 80 DEG C, drying in 6 hours.
(3) finally in 1700 DEG C, argon gas pressureless sintering obtain within 1 hour relative density 99% fine and close superhigh temperature it is heat-insulated
Yb3Al5O12Ceramics.
Embodiment 5
One kind of the present invention prepares the heat-insulated Yb of superhigh temperature3Al5O12The method of ceramic component, it comprises the following steps：
(1) by Yb2O3And Al2O3Powder is according to Yb2O3：Al2O3=3.05:5 mol ratios are weighed, and absolute ethyl alcohol are added, with rolling
Cartridge type batch mixer is mixed 24 hours, and rotating speed is 200/ turn, and well mixed raw material is dried 18 hours at 33 DEG C and obtains Yb2O3With
Al2O3Mixed-powder, by the Yb after drying process2O3And Al2O3Mixed-powder is placed in molybdenum disilicide stove, is heated in atmosphere
1250 DEG C, insulation obtains the Yb of high-purity in 4 hours3Al5O12Superhigh temperature thermal insulation ceramicses powder.
(2) it is medium planetary ball mill ball milling by Yb using absolute ethyl alcohol3Al5O12Ceramic powders ball milling 26 hours, turn
Speed is 270 revs/min, obtains the Yb that granularity is less than 1 μm3Al5O12Superhigh temperature thermal insulation ceramicses powder, according to Yb3Al5O12Solid
Content is 50%, and the content of isobutene-maleic anhydride copolymer accounts for Yb3Al5O120.5wt% prepare Yb3Al5O12Ceramic water
Based sizing, inject in stainless steel mould after 22 DEG C of slurry ball milling 1 hour, be crosslinked 2 hours and obtain in 28 DEG C of air sets
Yb3Al5O12Ceramic body, the intensity of base substrate is high, can carry out the secondary operation such as turn hole.
(3) sample after processing through being sintered in 1600 DEG C of air as shown in figure 5, can obtain relative density for 4 hours more than 95%
Complicated shape ceramic component.
Embodiment 6
One kind of the present invention prepares the heat-insulated Yb of superhigh temperature3Al5O12The method of ceramic component, it comprises the following steps：
(1) by Yb2O3And Al2O3Powder is according to Yb2O3：Al2O3=3.03:5 mol ratios are weighed, and absolute ethyl alcohol are added, with rolling
Cartridge type batch mixer is mixed 40 hours, and rotating speed is 90/ turn, and well mixed raw material is dried 20 hours at 25 DEG C and obtains Yb2O3With
Al2O3Mixed-powder, by the Yb after drying process2O3And Al2O3Mixed-powder is placed in molybdenum disilicide stove, is heated in atmosphere
1200 DEG C, insulation obtains the Yb of high-purity in 4 hours3Al5O12Superhigh temperature thermal insulation ceramicses powder.
(2) it is medium planetary ball mill ball milling by Yb using absolute ethyl alcohol3Al5O12Ceramic powders ball milling 24 hours, turn
Speed is 300 revs/min, obtains the Yb that granularity is less than 1 μm3Al5O12Superhigh temperature thermal insulation ceramicses powder, according to Yb3Al5O12Solid
Content is 50%, and the content of isobutene-maleic anhydride copolymer accounts for Yb3Al5O120.5wt% prepare Yb3Al5O12Ceramic water
Based sizing, inject in stainless steel mould after 25 DEG C of slurry ball milling 1 hour, be crosslinked 2 hours and obtain in 30 DEG C of air sets
Yb3Al5O12Ceramic body, Yb3Al5O12Ceramic body is through 60 DEG C, drying in 5 hours.
(3) finally in 1600 DEG C, air pressureless sintering obtain within 4 hours relative density 95% fine and close superhigh temperature it is heat-insulated
Yb3Al5O12Ceramics, do not decompose in high-temperature sintering process, microstructure is as shown in fig. 6, the superhigh temperature being prepared is heat-insulated
Yb3Al5O12The bending strength of ceramics is 160MPa, and thermal conductivity during 1273K is 2.12W/m.K.
The additive of the present invention is isobutene-maleic anhydride copolymer, nontoxic, tasteless, molecular weight 55000-
65000, the ratio of isobutene and maleic anhydride is 1 in copolymer：1, active-COO in the copolymer-HN4 +Group and-
CONH2Group, generated after hydrolysis-COOH group.Because the presence of these groups causes Yb3Al5O12Ceramic powders are containing isobutyl
Stability is good in the aqueous solution of alkene-maleic anhydride copolymer, therefore need not additionally add surface dispersant.In addition, isobutyl
It can occur spontaneous crosslinking in the alkene-air of maleic anhydride copolymer in aqueous at room temperature, therefore without needing to add
Catalyst and initiator.The molecular structure of isobutene-maleic anhydride copolymer, spontaneous crosslinking close note solidification forming process such as Fig. 1
It is shown.
The heat-insulated Yb of superhigh temperature provided by the invention3Al5O12The preparation method of ceramics has the spy that technique is simple, practical
Point, surface dispersant, catalyst, crosslinking agent, initiator, reducing agent, high temperature sintering aid need not be added in technical process
Deng isobutene used-maleic anhydride copolymer is nontoxic, tasteless, good water solubility, can spontaneous cure in room temperature, air
Crosslinking.
Claims (2)
1. one kind prepares the heat-insulated Yb of superhigh temperature3Al5O12The method of ceramic component, it is characterised in that this method comprises the following steps：
(1) by raw material Yb2O3And Al2O3Powder weighing, mixing, mixing condition are：Anhydrous ethanol medium, rotating speed turn for 80-200/,
Mixing time is 24-48 hours；Then processing is dried in well mixed raw material, drying temperature is 20~40 DEG C, is dried
Time is 12~24 hours；By the raw material after drying process, in atmosphere, reaction temperature is 1000~1350 DEG C, the reaction time
For 1~4 hour, Yb is made3Al5O12Ceramic powders；Described Yb2O3And Al2O3The mol ratio of dosage is Yb2O3：Al2O3=
(3.01~3.05)：5；The reaction temperature of described high temperature solid state reaction is 1000-1350 DEG C, and the reaction time is 1-4 hours；
(2) by step (1) obtained by Yb3Al5O12Ceramic powders planetary ball mill ball milling, ball-milling medium are absolute ethyl alcohol, ball
Consume time as 24~36 hours, rotating speed is 200~300 revs/min；Yb3Al5O12Yb in ceramic aqueous slurry3Al5O12Solid contain
Measure as 45~55wt%, the content of crosslinking agent isobutene-maleic anhydride copolymer is 0.1~0.8wt%, Yb3Al5O12Ceramics
The Ball-milling Time of aqueous slurries is 0.1~5.0 hour, obtains that stability is good, the finely dispersed Yb of particle after ball milling3Al5O12Water
Base-material is starched；Again by Yb3Al5O12Mould used in ceramic aqueous slurry note solidification forming is stainless steel mould, and injection molding temperature is room temperature
20-38 DEG C, injection molding environment is air, it is not necessary to takes isolation air measure；Then by Yb3Al5O12The friendship of ceramic aqueous slurry
Connection solidification, solidification temperature are 20~45 DEG C, and hardening time is 0.5~8 hour, and curing environment is air；Obtained after crosslinking curing
High intensity Yb3Al5O12The drying temperature of ceramic body is 35~85 DEG C, and drying time is 5~20 hours, obtains Yb3Al5O12
Ceramic green；Described Yb3Al5O12Yb in ceramic aqueous slurry3Al5O12Solids content be 45-55wt%, crosslinking agent isobutyl
The content of alkene-maleic anhydride copolymer is 0.1-0.8wt%, and remaining is water；
(3) finally at 1450~1680 DEG C, sinter 1~4 hour, sintering atmosphere is Ar gas or air, you can obtain answering for densification
The Yb of miscellaneous shape3Al5O12Superhigh temperature thermal insulation ceramicses element.
2. one kind according to claim 1 prepares the heat-insulated Yb of superhigh temperature3Al5O12The method of ceramic component, it is characterised in that
Crosslinking agent isobutene-maleic anhydride copolymer used in this method, mean molecule quantity are 55000-65000, isobutene and suitable
The ratio of butylene dianhydride is 1：1.
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