CN104744045A - Method for preparing MgAlON transparent ceramic biscuit by direct coagulation casting - Google Patents
Method for preparing MgAlON transparent ceramic biscuit by direct coagulation casting Download PDFInfo
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Abstract
The invention relates to a method for preparing MgAlON transparent biscuit by direct coagulation casting. The method comprises the following steps: (1) preparing MgAlON ceramic slurry, namely adding an aqueous solution of a dispersant of which the pH is preadjusted to 8-11 into to-be-molded MgAlON powder, mixing and stirring, and leading the adding amount of the dispersant in the aqueous solution to 0.1-0.5wt% of the mass of the to-be-molded MgAlON powder to obtain the MgAlON ceramic slurry; (2) adding additive, namely adding coagulator into the MgAlON ceramic slurry obtained in the step (1) under an ice bath condition, and stirring to uniformly disperse the coagulator in the MgAlON ceramic slurry; (3) defoaming; (4) molding by injection and solidifying; and (5) drying the biscuit. The method is simple, the condition is easily controlled, the prepared MgAlON transparent ceramic biscuit has complete shape and uniform microscopic structure, and the sintered MgAlON transparent ceramic sample has good optical transmission.
Description
Technical field
The present invention relates to a kind of method utilizing Direct Coagulation Casting to prepare MgAlON crystalline ceramics biscuit, belong to field of transparent ceramic material preparation.
Background technology
Crystalline ceramics not only has the performances such as pottery intrinsic high temperature resistant, corrosion-resistant, high insulation, high strength, also has excellent optical characteristics, therefore can be widely used in the fields such as illumination, optics, transparent armor, sun power, infrared eye.Wherein non-oxidized substance aluminium oxynitride system (AlON, MgAlON, LiAlON etc.) crystalline ceramics has isotropic optical property, high transmittance, therefore more and more causes interest and the attention of people.
Due to requirements such as good optical perviousness require transparent ceramic material to possess crystal boundary do not have impurity and second-phase, relative density high.Therefore should ensure in crystalline ceramics preparation process, there is no impurity, shaping blank structure even compact.The complicated shape of ceramic component also proposes requirement to forming technique.At present, complicated shape ceramic component can be prepared compare again the method being applicable to formed transparent ceramics base substrate and have Direct Coagulation Casting in numerous forming methods.
Direct Coagulation Casting (Direct Coagulation Casting, DCC) is a kind of dead size forming process of ceramics technology that biological enzyme chemistry, colloid chemistry and ceramic technology are combined together.This technology mainly adopts corresponding reactant generation chemical reaction in biological enzyme ceramic size, thus change slurry pH value to iso-electric point or compressed ceramic particle surface electrostatic double layer, make repulsion elimination between solid particulate in slurry, particle is reunited (Si Wenjie under Van der Waals force effect, Miao He washes, Huang Yong. " it is shaping that pottery directly solidifies injection molding (DCC) ", modern technologies pottery, 1995,40-44).Current people have adopted the Direct Coagulation Casting of traditional substrate for enzymatic activity reaction to prepare the ceramic component of the complicated shape such as knee joint, rotor.But the scope of the method for this Direct Coagulation Casting to suitable ceramic powder has limitation, more applicable for the alumina-ceramic about isoelectric pH=9, and is not suitable for the lower ceramic powder of iso-electric point.Because not easily pH value is reduced to iso-electric point from alkalescence by the internal-response of slurry.For this reason, some Direct Coagulation Castings improved are developed, comprise high price gegenion Direct Coagulation Casting, using MgO as (K.Prabhakaran such as the Direct Coagulation Castings of peptizer, A.Melkei, N.M.Gokhale et al. " Direct coagulation casting of YSZ powder suspensions using MgOas coagulating agent ", Ceramics International, 35,2009,1487-1492).
The principle of high price gegenion Direct Coagulation Casting is the release by controlling high price gegenion in ceramic size, and increase gegenion intensity in slurry, compressing grains surface electric double layer reaches the effect of ceramic slurry curing.Use peptizer content few in high price gegenion Direct Coagulation Casting process, therefore the introducing of peptizer can not affect composition and the optical property of crystalline ceramics.And base substrate organic content prepared by high price gegenion Direct Coagulation Casting is low, can direct sintering and without the need to degreasing.Compared with Coagulation Casting, the peptizer toxicological harmless that high price gegenion Direct Coagulation Casting adds, is conducive to environment protection.Compared with traditional Direct Coagulation Casting, by higher (the Jie Xu of intensity of high price gegenion Direct Coagulation Casting gained base substrate, Yanan Qu, Xiaoqing Xi et al. " Properties of alumina coagulated Bodies prepared by direct coagulation casting via high valence counter ions (DCC-HVCI) ", Journal of the American Ceramics Society, 95(11), 2012,3415-3420), base substrate is conducive to without the distortion demoulding.Based on these features of high price gegenion Direct Coagulation Casting and the preparation requirement of crystalline ceramics, high price gegenion Direct Coagulation Casting is suitable for the crystalline ceramics parts preparing big-size complicated shape.
People (the Jie Xu such as Jie Xu, Ning Wen, Fei Qi et al. " Direct Coagulation Casting of Positively Charged Alumina Suspension by Controlled Release of High Valence Counter Ions from Calcium Phosphate ", Journal of the American Ceramics Society, 95(7), 2012,2155-2160) in alumina system with Ca
3(PO
4)
2insoluble calcium salt, as peptizer, passes through Ca
3(PO
4)
2the concentration of high price gegenion in ceramic size is increased, to reach the effect of Direct Coagulation Casting with the chemical reaction calcium ion discharged in insoluble calcium salt of HCl.Subsequently, people (the Jie Xu such as Jie Xu, Ning Wen, Hexin Li et al. " Direct Coagulation Casting of Alumina Suspension by High Valence Counter Ions Using as Coagulating Agent ", Journal of the American Ceramics Society, 95(8), 2012,2525-2530) in alumina system with Ca (IO
3)
26H
2o microsolubility calcium salt, as peptizer, increases the concentration of high price gegenion in ceramic size, to reach the effect of Direct Coagulation Casting by the release of calcium ion in raised temperature control microsolubility calcium salt.People (the Jinlong Yang such as Jinlong Yang, Jie Xu, Ning Wen et al. " Direct Coagulation Casting of Alumina Suspension via Controlled Release of High Valence Counterions from Thermo-sensitive Liposomes ", Journal of the American Ceramics Society, 96(1), 2013, 62-67) in alumina system using soluble calcium salt as peptizer, soluble calcium salt is wrapped in thermal sensitive liposome, the phase transition temperature adjusting the temperature to thermal sensitive liposome makes soluble calcium salt discharge from thermal sensitive liposome, to reach the effect of directly solidifying injection molding.
Although high price gegenion Direct Coagulation Casting can meet the requirement preparing complicated shape crystalline ceramics parts, it is Shortcomings still.Although compared with traditional Direct Coagulation Casting, the blank strength prepared by high price gegenion Direct Coagulation Casting is higher, compared with the intensity of base substrate prepared by gel casting forming, also differs greatly.Therefore in high price gegenion Direct Coagulation Casting process, suitable additive is added significant with the intensity strengthening base substrate.
At present, high price gegenion Direct Coagulation Casting method has been successfully applied to the preparation of alumina-ceramic base substrate, and has no report in MgAlON crystalline ceramics.
Summary of the invention
Main purpose of the present invention is to provide a kind of method that Direct Coagulation Casting prepares MgAlON crystalline ceramics biscuit, the method is simple, condition is easily controlled, the MgAlON crystalline ceramics biscuit shape prepared is intact, uniform microstructure, sinters the MgAlON crystalline ceramics sample optical transmission obtained good.
For achieving the above object, the technical scheme taked of the present invention is as follows:
Direct Coagulation Casting prepares a method for MgAlON crystalline ceramics biscuit, and it comprises the steps:
1) MgAlON ceramic size is prepared: in MgAlON powder to be formed, add the aqueous solution that pH preconditioning is the dispersion agent of 8-11, mix and stir, in the aqueous solution of described dispersion agent, the add-on of dispersion agent is 0.1 ~ 0.5wt% of MgAlON powder quality to be formed, obtains MgAlON ceramic size;
2) add additive: the MgAlON ceramic size of gained in step 1) (0 ~ 5 DEG C) under condition of ice bath is added peptizer, stir, make it dispersed in MgAlON ceramic size;
3) de-bubble: to step 2) ceramic size of gained carries out froth in vacuum under condition of ice bath;
4) injection molding solidification: the ceramic size of step 3) gained is injected mould, and cure and demold obtains MgAlON ceramic body;
5) body drying: carry out isostatic cool pressing process to it after MgAlON ceramic blank drying step 4) obtained, obtains MgAlON crystalline ceramics biscuit.
By such scheme, in described step 1), pH value is the aqueous dispersant of 8 ~ 11 is in the aqueous solution of dispersion agent, add strong aqua adjustment obtain.
By such scheme, the churning time of described step 1) is 3 ~ 12h.
By such scheme, in described step 1), in MgAlON ceramic size, the solid phase amount of MgAlON is not less than 50vol%.
By such scheme, described step 2) in the final concentration of peptizer in MgAlON ceramic size be 1.5 ~ 6g/L.The range of viscosities of the slurry obtained after adding peptizer is 450 ~ 1800mPas, and this slurry viscosity better can meet forming requirements.
By such scheme, described step 2) be included in MgAlON ceramic size and add ammonium polyacrylate liquation, the add-on of ammonium polyacrylate is no more than the 0.1wt% of MgAlON powder quality to be formed.
By such scheme, described dispersion agent is three ammonium citrates (Ammonium citrate tribasic, TAC); Peptizer is six water calcium iodates.
By in such scheme, in step 3), the froth in vacuum time is 20 ~ 40min, and vacuum tightness is 5 ~ 15kPa.
By such scheme, the solidification value of step 4) 50 ~ 70 DEG C, set time 1 ~ 4h.
By in such scheme, the drying in step 5) is divided into two parts, and the first step is dry 18 ~ 36h at room temperature; Second step is dry 12 ~ 24h at 100 DEG C.
Advantage of the present invention is:
(1) high price gegenion Direct Coagulation Casting applies in new system MgAlON crystalline ceramics by the present invention, and with six water calcium iodates for peptizer, applied widely compared with traditional Direct Coagulation Casting method, gained biscuit intensity is higher; Peptizer consumption is little, can not have an impact to the composition of crystalline ceramics and optical property, and agents useful for same toxicological harmless, be conducive to environment protection.
(2) the inventive method is simple, and condition is easily controlled, and the MgAlON crystalline ceramics biscuit shape prepared is intact, uniform microstructure, and density is higher.Sinter the MgAlON crystalline ceramics sample optical transmission that obtains good, be applicable to the preparation of crystalline ceramics parts of large size, complicated shape.
(3) the present invention can prepare high solid phase amount (solid phase amount >50vol%), low viscous ceramic size, is conducive to the density and the intensity that improve base substrate thus.
(4) the polymer poly acrylamide PAA that the present invention adds can strengthen blank strength, and institute to add PAA content few, base substrate is without the need to degreasing.
Accompanying drawing explanation
Fig. 1 is that MgAlON powder of the present invention is adding the pH-zeta potential variation figure before and after dispersion agent.
The viscosity relationship figure of 50vol%MgAlON ceramic size after adding different amounts dispersion agent that Fig. 2 prepares for the embodiment of the present invention 1.
The 50vol%MgAlON ceramic size that Fig. 3 prepares for the embodiment of the present invention 1 adds different amounts Ca (IO under ice bath
3)
26H
2viscosity relationship figure after O.
The SEM picture of the MgAlON biscuit of ceramics of Fig. 4 prepared by the embodiment of the present invention 1.
The photo of the MgAlON biscuit of ceramics of Fig. 5 prepared by the embodiment of the present invention 1.
The MgAlON biscuit of ceramics of Fig. 6 prepared by the embodiment of the present invention 1 sinters the photo of the MgAlON ceramic product obtained.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with accompanying drawing, embodiment, but content of the present invention is not only confined to the following examples.
Embodiment 1:
Be the 0.2wt% of MgAlON powder quality to be formed by 0.072gTAC(dispersion agent) be dissolved in 10ml deionized water, with strong aqua regulator solution pH to 9, stir preparation premixed liquid, in premixed liquid, add MgAlON powder 36.45g, after using magnetic stirrer 6h, obtain the MgAlON ceramic size that solid phase amount is 50vol%; Fig. 1 is that MgAlON powder is adding the pH-zeta potential variation figure before and after dispersion agent.After adding TAC as seen from Figure 1 in MgAlON, the absolute value of its zeta current potential obviously increases in the basic conditions, is conducive to the stability of slurry, and wherein pH value is 8 ~ 11 time, and zeta current potential absolute value is comparatively large, and the stability of slurry is better.Fig. 2 adds the viscosity relationship figure after different amounts dispersion agent in the 50vol%MgAlON ceramic size prepared at the present embodiment.Add the viscosity that appropriate TAC can reduce slurry as seen from Figure 2, wherein when adding TAC content and being the 0.2wt% of powder, viscosity is minimum, and slurry is the most stable.Gained slurry is placed in ice bath (0 ~ 5 DEG C), adds six water calcium iodate 0.06g(3g/L), stir, make it dispersed in MgAlON ceramic size.Fig. 3 adds different amounts Ca (IO in the 50vol%MgAlON ceramic size prepared in embodiment under ice bath
3)
26H
2viscosity relationship figure after O.As seen from Figure 3 in the MgAlON ceramic size of 50vol%, the amount adding six water calcium iodates can affect the viscosity of the slurry of acquisition, and time in certain amount ranges, the viscosity of the slurry obtained better can meet forming requirements; Stirring 1h again makes peptizer be dispersed in ceramic size; Use rotary evaporation to carry out ice bath froth in vacuum 20min to ceramic size, vacuum tightness is 10kPa; By after de-bubble slurry inject mould, at being placed in 60 DEG C leave standstill, the demoulding after 2.5h and under being placed on air at room temperature dry 18h be placed on dry 24h in 100 DEG C of loft drier, then isostatic cool pressing process is carried out to it, obtains MgAlON ceramic body.
The solid phase amount of above-mentioned preparation is the viscosity of 50vol%MgAlON ceramic size be 130mPa(shearing rate is 56s
-1), after adding peptizer at low temperatures, its viscosity is 556mPa(shearing rate is 10.29s
-1), now MgAlON ceramic size good fluidity, stability are high, and injection molding is easy, and Fig. 5 is shown in by the photo of shaping difform base substrate, and Fig. 4 is shown in by SEM photo, by finding out in Fig. 4 that blank shape is intact, uniform microstructure.Base substrate relative density after isostatic cool pressing is 58.76%, and bending strength is 1.14MPa.The MgAlON biscuit of ceramics obtained by the present embodiment sinters the MgAlON ceramic product photo obtained and sees Fig. 6, and MgAlON pottery has good optical transmission in visible-range as seen from Figure 6.
Embodiment 2:
Be the 0.2wt% of MgAlON powder quality to be formed by 0.072gTAC(dispersion agent) be dissolved in 10ml deionized water, with strong aqua regulator solution pH to 9, stir preparation premixed liquid, in premixed liquid, add MgAlON powder 36.45g, after using magnetic stirrer 6h, obtain the MgAlON ceramic size that solid phase amount is 50vol%; Gained slurry is placed in ice bath (0 ~ 5 DEG C), adds six water calcium iodate 0.09g, then stir 1h and make peptizer be dispersed in ceramic size; Use rotary evaporation to carry out ice bath froth in vacuum 30min to ceramic size, vacuum tightness is 10kPa; By after de-bubble slurry inject mould, at being placed in 50 DEG C leave standstill, the demoulding after 2.5h and under being placed on air at room temperature dry 24h be placed on dry 24h in 100 DEG C of loft drier, then isostatic cool pressing process is carried out to it, obtains MgAlON ceramic body.
The solid phase amount of above-mentioned preparation is the viscosity of 50vol%MgAlON ceramic size be 130mPa(shearing rate is 56s
-1), after adding peptizer at low temperatures, its viscosity is 625mPa(shearing rate is 10.29s
-1), now MgAlON ceramic size good fluidity, stability are high, and injection molding is easy, and institute's molding blank shape is intact, uniform microstructure, and base substrate relative density after isostatic cool pressing is 58.04%, and bending strength is 1.13MPa.
Embodiment 3:
Be the 0.2wt% of MgAlON powder quality to be formed by 0.072gTAC(dispersion agent) be dissolved in 10ml deionized water, with strong aqua regulator solution pH to 9, stir preparation premixed liquid, in premixed liquid, add MgAlON powder 36.45g, after using magnetic stirrer 6h, obtain the MgAlON ceramic size that solid phase amount is 50vol%; Gained slurry is placed in ice bath (0 ~ 5 DEG C), adds six water calcium iodate 0.12g, then stir 1h and make peptizer be dispersed in ceramic size; Use rotary evaporation to carry out ice bath froth in vacuum 30min to ceramic size, vacuum tightness is 5kPa; By after de-bubble slurry inject mould, at being placed in 50 DEG C leave standstill, the demoulding after 1.5h and under being placed on air at room temperature dry 36h be placed on dry 24h in 100 DEG C of loft drier, then isostatic cool pressing process is carried out to it, obtains MgAlON ceramic body.
The solid phase amount of above-mentioned preparation is the viscosity of 50vol%MgAlON ceramic size be 130mPa(shearing rate is 56s
-1), after adding peptizer at low temperatures, its viscosity is 1800mPa(shearing rate is 10.29s
-1), now MgAlON ceramic size good fluidity, stability are high, and injection molding is easy, and institute's molding blank shape is intact, uniform microstructure, and base substrate relative density after isostatic cool pressing is 56.93%, and bending strength is 1.10MPa.
Embodiment 4:
Be the 0.5wt% of MgAlON powder quality to be formed by 0.182gTAC(dispersion agent) be dissolved in 9.6ml deionized water, with strong aqua regulator solution pH to 10, stir preparation premixed liquid, in premixed liquid, add MgAlON powder 37.91g, after using magnetic stirrer 9h, obtain the MgAlON ceramic size that solid phase amount is 52vol%; Gained slurry is placed in ice bath (0 ~ 5 DEG C), adds six water calcium iodate 0.03g, then stir 1h and make peptizer be dispersed in ceramic size; Use rotary evaporation to carry out ice bath froth in vacuum 30min to ceramic size, vacuum tightness is 10kPa; By after de-bubble slurry inject mould, at being placed in 60 DEG C leave standstill, the demoulding after 4h and under being placed on air at room temperature dry 24h be placed on dry 12h in 100 DEG C of loft drier, then isostatic cool pressing process is carried out to it, obtains MgAlON ceramic body.
The solid phase amount of above-mentioned preparation is the viscosity of 52vol%MgAlON ceramic size be 350mPa(shearing rate is 56s
-1), after adding peptizer at low temperatures, its viscosity is 725mPa(shearing rate is 10.29s
-1), now MgAlON ceramic size good fluidity, stability are high, and injection molding is easy, and institute's molding blank uniform microstructure, base substrate relative density after isostatic cool pressing is 57.87%, and bending strength is 1.12MPa.
Embodiment 5:
Be the 0.2wt% of MgAlON powder quality to be formed by 0.072gTAC(dispersion agent) be dissolved in 10ml deionized water, with strong aqua regulator solution pH to 10, stir preparation premixed liquid, in premixed liquid, add MgAlON powder 36.45g, after using magnetic stirrer 3h, obtain the MgAlON ceramic size that solid phase amount is 50vol%; Gained slurry is placed in ice bath (0 ~ 5 DEG C), adds six water calcium iodate 0.06g, massfraction is the PAA aqueous solution 0.038ml of 42.8wt%, then stirs 1h and make peptizer be dispersed in ceramic size; Use rotary evaporation to carry out ice bath froth in vacuum 40min to ceramic size, vacuum tightness is 15kPa; By after de-bubble slurry inject mould, at being placed in 70 DEG C leave standstill, the demoulding after 2h and under being placed on air at room temperature dry 36h be placed on dry 12h in 100 DEG C of loft drier, then isostatic cool pressing process is carried out to it, obtains MgAlON ceramic body.
The solid phase amount of above-mentioned preparation is the viscosity of 50vol%MgAlON ceramic size be 135mPa(shearing rate is 56s
-1), after adding peptizer at low temperatures, its viscosity is 560mPa(shearing rate is 10.29s
-1), now MgAlON ceramic size good fluidity, stability are high, and injection molding is easy, and institute's molding blank uniform microstructure, base substrate relative density after isostatic cool pressing is 58.78%, and bending strength is 2.18MPa.
Embodiment 6:
Be the 0.2wt% of MgAlON powder quality to be formed by 0.072gTAC(dispersion agent) be dissolved in 10ml deionized water, with strong aqua regulator solution pH to 11, stir preparation premixed liquid, in premixed liquid, add MgAlON powder 36.45g, after using magnetic stirrer 3h, obtain the MgAlON ceramic size that solid phase amount is 50vol%; Gained slurry is placed in ice bath (0 ~ 5 DEG C), adds six water calcium iodate 0.06g, massfraction is the PAA aqueous solution 0.076ml of 42.8wt%, then stirs 1h and make peptizer be dispersed in ceramic size; Use rotary evaporation to carry out ice bath froth in vacuum 20min to ceramic size, vacuum tightness is 5kPa; By after de-bubble slurry inject mould, at being placed in 70 DEG C leave standstill, the demoulding after 2h and under being placed on air at room temperature dry 24h be placed on dry 12h in 100 DEG C of loft drier, then isostatic cool pressing process is carried out to it, obtains MgAlON ceramic body.
The solid phase amount of above-mentioned preparation is the viscosity of 50vol%MgAlON ceramic size be 140mPa(shearing rate is 56s
-1), after adding peptizer at low temperatures, its viscosity is 565mPa(shearing rate is 10.29s
-1), now MgAlON ceramic size good fluidity, stability are high, and injection molding is easy, and institute's molding blank uniform microstructure, base substrate relative density after isostatic cool pressing is 58.47%, and bending strength is 1.41MPa.
Embodiment 7:
Be the 0.2wt% of MgAlON powder quality to be formed by 0.072gTAC(dispersion agent) be dissolved in 10ml deionized water, with strong aqua regulator solution pH to 8, stir preparation premixed liquid, in premixed liquid, add MgAlON powder 36.45g, after using magnetic stirrer 12h, obtain the MgAlON ceramic size that solid phase amount is 50vol%; Gained slurry is placed in ice bath (0 ~ 5 DEG C), adds six water calcium iodate 0.09g, PAA aqueous solution 0.076ml stirs 1h again makes peptizer be dispersed in ceramic size; Use rotary evaporation to carry out ice bath froth in vacuum 20min to ceramic size, vacuum tightness is 5kPa; By after de-bubble slurry inject mould, at being placed in 60 DEG C leave standstill, the demoulding after 2h and under being placed on air at room temperature dry 36h be placed on dry 24h in 100 DEG C of loft drier, then isostatic cool pressing process is carried out to it, obtains MgAlON ceramic body.
The solid phase amount of above-mentioned preparation is the viscosity of 50vol%MgAlON ceramic size be 135mPa(shearing rate is 56s
-1), after adding peptizer at low temperatures, its viscosity is 655mPa(shearing rate is 10.29s
-1), now MgAlON ceramic size good fluidity, stability are high, and injection molding is easy, and institute's molding blank uniform microstructure, base substrate relative density after isostatic cool pressing is 58.35%, and bending strength is 1.43MPa.
Embodiment 8:
Be the 0.1wt% of MgAlON powder quality to be formed by 0.036gTAC(dispersion agent) be dissolved in 9.8ml deionized water, with strong aqua regulator solution pH to 9, stir preparation premixed liquid, in premixed liquid, add MgAlON powder 37.18g, after using magnetic stirrer 9h, obtain the MgAlON ceramic size that solid phase amount is 51vol%; Gained slurry is placed in ice bath (0 ~ 5 DEG C), adds six water calcium iodate 0.09g and stir 1h again and make peptizer be dispersed in ceramic size; Use rotary evaporation to carry out ice bath froth in vacuum 30min to ceramic size, vacuum tightness is 10kPa; By after de-bubble slurry inject mould, at being placed in 60 DEG C leave standstill, the demoulding after 2h and under being placed on air at room temperature dry 36h be placed on dry 18h in 100 DEG C of loft drier, then isostatic cool pressing process is carried out to it, obtains MgAlON ceramic body.
The solid phase amount of above-mentioned preparation is the viscosity of 51vol%MgAlON ceramic size be 335mPa(shearing rate is 56s
-1), after adding peptizer at low temperatures its viscosity for 845mPa(shearing rate be 10.29s
-1), now MgAlON ceramic size good fluidity, stability are high, and injection molding is easy, and institute's molding blank uniform microstructure, base substrate relative density after isostatic cool pressing is 57.89%, and bending strength is 1.12MPa.
Each raw material cited by the present invention, and the bound of each raw material of the present invention, the bound of processing parameter, interval value can realize the present invention, do not enumerate embodiment at this.
Claims (10)
1. Direct Coagulation Casting prepares a method for MgAlON crystalline ceramics biscuit, it is characterized in that: it comprises the steps:
1) MgAlON ceramic size is prepared: in MgAlON powder to be formed, add the aqueous solution that pH preconditioning is the dispersion agent of 8-11, mix and stir, in the aqueous solution of described dispersion agent, the add-on of dispersion agent is 0.1 ~ 0.5wt% of MgAlON powder quality to be formed, obtains MgAlON ceramic size;
2) add additive: the MgAlON ceramic size of gained in step 1) (0 ~ 5 DEG C) under condition of ice bath is added peptizer, stir, make it dispersed in MgAlON ceramic size;
3) de-bubble: to step 2) ceramic size of gained carries out froth in vacuum under condition of ice bath;
4) injection molding solidification: the ceramic size of step 3) gained is injected mould, and cure and demold obtains MgAlON ceramic body;
5) body drying: carry out isostatic cool pressing process to it after MgAlON ceramic blank drying step 4) obtained, obtains MgAlON crystalline ceramics biscuit.
2. Direct Coagulation Casting according to claim 1 prepares the method for MgAlON crystalline ceramics biscuit, it is characterized in that: in described step 1), pH value is the aqueous dispersant of 8 ~ 11 is in the aqueous solution of dispersion agent, add strong aqua adjustment obtain.
3. Direct Coagulation Casting according to claim 1 prepares the method for MgAlON crystalline ceramics biscuit, it is characterized in that: in described step 1), in MgAlON ceramic size, the solid phase amount of MgAlON is not less than 50vol%.
4. Direct Coagulation Casting according to claim 1 prepares the method for MgAlON crystalline ceramics biscuit, it is characterized in that: described step 2) in the final concentration of peptizer in MgAlON ceramic size be 1.5 ~ 6g/L.
5. Direct Coagulation Casting according to claim 1 prepares the method for MgAlON crystalline ceramics biscuit, it is characterized in that: described step 2) range of viscosities of slurry that obtains is 450 ~ 1800mPas.
6. Direct Coagulation Casting according to claim 1 prepares the method for MgAlON crystalline ceramics biscuit, it is characterized in that: it is characterized in that: described step 2) be included in MgAlON ceramic size and add ammonium polyacrylate liquation, the add-on of ammonium polyacrylate is no more than the 0.1wt% of MgAlON powder quality to be formed.
7. Direct Coagulation Casting according to claim 1 prepares the method for MgAlON crystalline ceramics biscuit, it is characterized in that: described dispersion agent is three ammonium citrates; Peptizer is six water calcium iodates.
8. Direct Coagulation Casting according to claim 1 prepares the method for MgAlON crystalline ceramics biscuit, it is characterized in that: in step 3), the froth in vacuum time is 20 ~ 40min, and vacuum tightness is 5 ~ 15kPa.
9. Direct Coagulation Casting according to claim 1 prepares the method for MgAlON crystalline ceramics biscuit, it is characterized in that: the solidification value of step 4) 50 ~ 70 DEG C, set time 1 ~ 4h.
10. Direct Coagulation Casting according to claim 1 prepares the method for MgAlON crystalline ceramics biscuit, it is characterized in that: the drying in step 5) is divided into two parts, and the first step is dry 18 ~ 36h at room temperature; Second step is dry 12 ~ 24h at 100 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105906346A (en) * | 2016-05-06 | 2016-08-31 | 武汉理工大学 | Method for preparing MgAlON crystalline ceramic pellets by gelcasting |
| CN106242577A (en) * | 2016-08-08 | 2016-12-21 | 屠秀芬 | The nano oxidized terbium of a kind of MgALON is combined the preparation method of magneto-optic crystalline ceramics |
| CN111138173A (en) * | 2020-03-10 | 2020-05-12 | 中原工学院 | Method for preparing low-temperature sintered ceramic composite material by rapid forming |
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| CN1680214A (en) * | 2004-04-09 | 2005-10-12 | 中国航空工业第一集团公司北京航空材料研究院 | Solid-phase reacting synthesis of composite ceramic powder non-toxic gel |
| CN102825649A (en) * | 2012-07-18 | 2012-12-19 | 武汉理工大学 | Method for preparing MgAlON transparent ceramic bisque by gel casting and molding |
| US20130220988A1 (en) * | 2010-10-25 | 2013-08-29 | Ngk Insulators, Ltd. | Heating device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1680214A (en) * | 2004-04-09 | 2005-10-12 | 中国航空工业第一集团公司北京航空材料研究院 | Solid-phase reacting synthesis of composite ceramic powder non-toxic gel |
| US20130220988A1 (en) * | 2010-10-25 | 2013-08-29 | Ngk Insulators, Ltd. | Heating device |
| CN102825649A (en) * | 2012-07-18 | 2012-12-19 | 武汉理工大学 | Method for preparing MgAlON transparent ceramic bisque by gel casting and molding |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105906346A (en) * | 2016-05-06 | 2016-08-31 | 武汉理工大学 | Method for preparing MgAlON crystalline ceramic pellets by gelcasting |
| CN106242577A (en) * | 2016-08-08 | 2016-12-21 | 屠秀芬 | The nano oxidized terbium of a kind of MgALON is combined the preparation method of magneto-optic crystalline ceramics |
| CN111138173A (en) * | 2020-03-10 | 2020-05-12 | 中原工学院 | Method for preparing low-temperature sintered ceramic composite material by rapid forming |
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