CN105906346A - Method for preparing MgAlON crystalline ceramic pellets by gelcasting - Google Patents
Method for preparing MgAlON crystalline ceramic pellets by gelcasting Download PDFInfo
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Abstract
The invention belongs to the technical field of ceramic preparation. A method for preparing MgAlON crystalline ceramic pellets by gelcasting is characterized by comprising the following steps: 1) burdening: adjusting the pH value of deionized water by using stronger ammonia water to obtain a water solution having the a pH value of 10 to 12; adding MgAlON powder, methacrylamide, methylene bisacrylamide and citric acid triamine, wherein an addition amount of the MgAlON powder is 45 to 50vol% of the water solution, an addition amount of the methacrylamide is 15 to 25vol% of the water solution, an addition amount of the methylene bisacrylamide is 4 to 6vol% of the water solution, and an addition amount of the citric acid triamine is 0.2 to 0.5wt% of the mass of the MgAlON powder; mixing and stirring for at least 4 h to obtain ceramic slurry having the viscosity of 60 to 100mPa.S; 2) pelleting; 3) drying and glue removal; 4) sintering: sintering the glue-removed ceramic pellet blanks in an atmosphere furnace, wherein the firing temperature is not lower than 1850 DEG C, and the heat preservation time is 2 to 3h; 5) hot isostatic pressing: carrying out hot isostatic pressing treatment on the pre-sintered ceramic pellet sintered bodies at the temperature of not lower than 1850 DEG C and the pressure of not less than 150MPa, wherein the heat preservation time is 2 to 3 h. The prepared MgAlON crystalline ceramic pellets have good sphericity degree and optical transmission, and can be used in a ball milling process of the MgAlON ceramic powder, such that the introduction of impurities is reduced and the ball milling efficiency is improved.
Description
Technical field
The invention belongs to field of ceramic preparation technology, be specifically related to the preparation method of a kind of MgAlON crystalline ceramics bead.
Background technology
Single dispersing grade (hundreds of micron-several millimeters) ceramic bead is obtained for enough attention in various fields and is widely used.
As high due to intensity in porous ceramics bead, stable chemical nature, there is again rule, uniform gap structure, be used as separating more
The medium purified；High-wearing feature, high intensity and hardness, corrosion resistant ceramic bead relative to metal grinding media to grinding charge
The pollution of matter is less, and ceramic bead just by substituted metal abrasive media, is increasingly widely applied at each industrial circle.
And prepared by the crystalline ceramics that purity requirement is high, ceramic bead is optimal abrasive media.
At present, the method preparing grade ceramic bead mainly has mould pressing, extrusion-spheronization, spray drying method, gel
Injection molding etc..Mould pressing is that a certain amount of organic additive is added powder, then injects mould, relies on external pressure to be allowed to
The method of molding.This legal system product percent of firing shrinkage is little, is unlikely to deform, and the ceramic bead size prepared is relatively big, but spherical bad,
Base substrate apparent form is poor.Extrusion spheronization technique is to add deionized water etc. as coagulating agent or binding agent to powder, is led to by wet feed
Cross hole or the sieve of tool certain diameter, be squeezed into cylindrical strip extrudate, make plastic cylindrical material exist by the effect of frictional force
Ceaselessly roll on plate, be gradually rolled into spheroidal.Extrusion-spheronization process production efficiency is high, the ceramic bead biscuit intensity prepared
Greatly, but sphericity is poor, and impurity content is higher.The balling-up mechanism being spray-dried is then that material liquid nebulizer is disperseed mist formation
Dripping, droplet is formed spherical under capillary effect, and this technique prepares that ceramic microsphere is simple to operate flexibly, it is big to be particularly adapted to
The advantages such as commercial production, but there is the shortcomings such as investment cost is higher, the thermal efficiency is on the low side, and only prepare ceramic bead diameter range
Within being limited to 500 μm.
It is to use for reference gel injection-moulding to prepare large scale, the technique of complicated shape ceramic part that gel injection-moulding prepares ceramic bead.Solidifying
The ultimate principle of glue injection molding and forming technology is: ceramic powders is dispersed in organic monomer solution, and organic monomer is at catalyst and draws
Send out under the effects such as agent, occur home position polymerization reaction to form network structure and ceramic powders is wrapped up wherein, become and have some strength
Base substrate.Gel injection-moulding is prepared ceramic bead technology and is utilized the immiscible principle of water-thinned ceramic slurry and oil solvent dexterously, makes
Slurry liquid drops in and exists with balled form under capillary effect.The ceramic slurry prepared is dripped in deep fat shorter by root
Time inner gel fix its shape, it is ensured that it drops down onto bottom and does not crosslinks, and the flat phenomenon then binder removal such as collapse obtains.Research
Report point out when interfacial tension difference is 30, ceramic slurry can quickly become spherical (Jin long Yang, Juan li Yu,
Yong Huang, Recent developments in gelcasting of ceramics, Journal of the European Ceramic
Society, 31 (2011), 2,569 2591).Zhu Honglong successfully prepares 29.5wt% solid concentration by gel casting process
The ZrO of 0.6mm-2mm controllable diameter2Ceramic microsphere, size uniformity is spherical good and have good microstructure (Zhu Hong
Dragon, Gel-casting process prepares ZrO2Ceramic microsphere, Zaozhuang University's journal, 28 (2), 2011,4)；Xiong Peipei etc. lead to
Crossing drop-condensation method and prepare phosphate ceramics microsphere particle, profile rounding, any surface finish is white, and granular size is essentially identical,
(Xiong Peipei, Dong Yinsheng, Lin Pinghua, drop-condensation method prepares phosphate ceramics microsphere particle, silicon to a diameter of about 1mm
Hydrochlorate journal, 37 (3), 2009,3)；Chen Xing, Yang Hongguang obtain 45-50% solid phase by gel nodularization-solid state reaction-sintering
Content 1.2mm-1.4mmLi4SiO4Ceramic bead, sphere diameter distribution is unified, sphericity be better than 1.04 (Chen Xing, Yang Hongguang,
Gel nodularization-solid state reaction-sintering process prepares Li4SiO4Ceramic microsphere, material heat treatment journal, 35 (6), 2014,6)；
Guo Wenli, Liang Tongxiang, Hao Shaochang prepare UO by gel-casting2Microsphere, average diameter is 0.71mm, density
10.70g/cm3(Guo Wenli, Liang Tongxiang, Hao Shaochang, gel-casting prepares UO2Ceramic fuel nuclear core, core association of China core
Material branch 2007 year seminar).
MgAlON is a kind of novel transparent ceramic material, has excellent optical transmittance and mechanical performance.Ball milling is pottery
In preparation process indispensable rapid, select conjunction grinding media of trying material powder is mixed and grinds, miscellaneous in minimizing mechanical milling process
The introducing of matter improves grinding efficiency, is significant for the ceramic powder going out high-purity transparent.For high transparent of purity requirement
Ceramic is standby, needs strict that control impurity content, and MgALON crystalline ceramics bead will be that to prepare MgAlON powder body optimal
Abrasive media, its wearability is high, will not pollute raw material, have important researching value.On the other hand, its have widely should
With, pavement strip is to ensure that the critical facility of traffic safety, adds bead and be to ensure that graticule night can in pavement strip material
Important means depending on property.And wherein glass bead presentation quality, particle diameter distribution, refractive index, wearability, corrosion resistance are for being primarily upon
Content, transparent MgAlON Ceramic Balls has significant advantage in wearability, corrosion resistance relative to glass bead, and future can replace glass
Ball is applied to pavement strip material, extends its service life；Undersized microsphere can as the packing material of composite,
The rigidity of matrix, intensity and wearability etc. is increased while reducing density.
At present, gel injection-moulding is prepared the method for ceramic bead and be have not been reported in MgAlON crystalline ceramics.
Summary of the invention
It is an object of the invention to provide a kind of method that gel injection-moulding prepares MgAlON crystalline ceramics bead, prepared MgAlON
The good sphericity of crystalline ceramics bead also has optical transmittance, can be used for the mechanical milling process of MgAlON ceramic powder, reduces miscellaneous
The introducing of matter, improves grinding efficiency.
For achieving the above object, the technical solution used in the present invention is as follows: it is little that a kind of gel injection-moulding prepares MgAlON crystalline ceramics
The method of ball, it is characterised in that comprise the steps:
1) dispensing: use strong aqua ammonia regulation deionized water pH value, it is thus achieved that the aqueous solution of pH=10-12；
It is aqueous solution 45-50vol% by the addition of MgAlON powder body (ceramic powder), Methacrylamide (MAM)
Addition is aqueous solution 15-25vol%, and the addition of methylene-bisacrylamide (MBAM) is aqueous solution 4-6vol%, Fructus Citri Limoniae
The 0.2-0.5wt% that addition is MgAlON powder body (ceramic powder) weight of acid triamine (TAC), chooses MgAlON
Powder body (ceramic powder), Methacrylamide (MAM), methylene-bisacrylamide (MBAM), triammonium citrate (TAC)；
By MgAlON powder body (ceramic powder), Methacrylamide (MAM), methylene-bisacrylamide (MBAM),
After triammonium citrate (TAC) and aqueous solution, at least stirring 4h (such as: after stirring 4-6h), it is thus achieved that viscosity is 60-100mPa s
Ceramic serosity；
2) ball processed: pottery serosity (or claiming low-viscosity ceramic slurry) is placed in vacuum environment (froth in vacuum machine, vacuum stirring
Machine) stirring 20-40min (carrying out de-bubble)；Take out and add peroxo disulfate acid ammonium (APS), peroxo disulfate acid ammonium (APS)
Addition is the 4-15.6vol% of aqueous solution, obtains ceramic slurry；Quantitative charger is used quantitatively to be instilled the most not by ceramic slurry
Less than 130cm (such as 130-150cm, the gel reaction time that height is enough to ensure ceramic bead no less than 130cm), temperature
Being not less than in the dimethyl-silicon oil solvent of 60 DEG C (such as 60-90 DEG C) (to ensure quickly carrying out of gelation reaction), insulation is at least
After 6h (such as: after insulation 6-10h), the ceramic bead biscuit prepared is taken out；
3) it is dried and binder removal: prepared ceramic bead biscuit is placed in 40-60 DEG C of drying baker inside holding 4-8h, takes out and is placed on high temperature
In tube furnace, 630-800 DEG C of insulation 6-8h, carry out binder removal, get rid of Organic substance in ceramic bead biscuit；
4) sintering: the ceramic bead biscuit after binder removal is sintered (sintering atmosphere is nitrogen) in atmosphere furnace, and firing temperature is the lowest
In 1850 DEG C, temperature retention time is 2-3h, obtains the Ceramic Balls sintered body after pre-burning；
5) high temperature insostatic pressing (HIP): the Ceramic Balls sintered body after pre-burning carries out hip treatment, 1850-1900 DEG C, under 160-200MPa
Insulation 2-3h, obtains MgAlON crystalline ceramics bead.
The particle diameter of described MgAlON powder body is 0.3-0.5 μm, is evenly distributed, and purity is not less than 99.99wt%.
The viscosity scope of used dimethyl-silicon oil solvent is 300000-600000cps.
The concentration of described strong aqua ammonia is 80wt%-95wt%.
The vacuum of described vacuum environment is 5-15kPa.
Controlled MgAlON crystalline ceramics bead biscuit is obtained by the content of regulation temperature and peroxo disulfate acid ammonium (APS),
Sphere diameter is 1-4mm.
Molding mode utilizes surface tension official post aqueous-based ceramic slip to become spherical in dimethyl-silicon oil solvent.
The present invention is with MgAlON powder body as raw material, through dispensing, slurrying, dry, binder removal, sintering, optical manufacturing acquisition.
The present invention compared with prior art, has the advantage that
1, MgAlON crystalline ceramics bead preparation method of the present invention is simple, convenient to operate, has no relevant report both at home and abroad.
2, the MgAlON crystalline ceramics bead biscuit good sphericity obtained, sphere diameter scope is wide (1mm-4mm), sintering system
The MgAlON crystalline ceramics bead obtained is from wear rate low (43.6r/min, 0.2%).
3, the MgAlON crystalline ceramics bead prepared has potential use value, because its wearability, corrosion resistance are far above glass
Glass ball, can replace glass bead to be applied to pavement strip measuring technology, extends graticule service life.
4, the good sphericity of MgAlON crystalline ceramics bead for preparing also has optical transmittance, MgAlON under macroscopic observation
Ceramic Balls is glittering and translucent, and permeable Ceramic Balls profile view observes font, has optical transmittance.Can be used for MgAlON pottery
The mechanical milling process of powder body, reduces the introducing of impurity, improves grinding efficiency.
Accompanying drawing explanation
Fig. 1 is the preparation technology route map of the present invention.
Fig. 2 is the ceramic bead biscuit figure obtained by present example 3.
Fig. 3 is the sintered rear internal microstructure figure of ceramic bead biscuit obtained by present example 3.
Fig. 4 is the ceramic bead internal microstructure figure that present example 3 obtains after high temperature insostatic pressing (HIP).
Fig. 5 (a) is the outside drawing of the crystalline ceramics ball that present example 3 obtains.
Fig. 5 (b) is the profile of the crystalline ceramics ball that present example 3 obtains.
Detailed description of the invention
With specific embodiment, technical scheme is described below, but protection scope of the present invention is not limited to this:
A kind of gel injection-moulding prepares the method for MgAlON crystalline ceramics bead, with MgAlON powder body as raw material, through dispensing,
Ball processed, dry and binder removal, sintering, high temperature insostatic pressing (HIP) acquisition (optical manufacturing again).
Embodiment 1
Prepared by ceramic size: prepared the solution 10ml of PH=10 by strong aqua ammonia regulation deionized water；Weigh MgAlON powder body
25.25g (solid concentration is aqueous solution 45vol%), MAM1.5g (15vol% of aqueous solution), MBAM0.4g be (aqueous solution
4vol%), TAC0.050g (0.2wt% of MgAlON powder quality), uniformly mixing is placed on blender stirring 4h, obtains
Obtain the ceramic serosity that viscosity is 60-100mPa s；Pottery serosity (or weighing slurry, the most identical) is placed in vacuum environment (true
Reciprocal of duty cycle 5kPa) stir bubble in 20min eliminating serosity, add peroxo disulfate acid ammonium 400ul (4vol% of aqueous solution) afterwards
Mix homogeneously；Quantitatively be added dropwise to temperature be 60 DEG C of height be 130cm dimethyl-silicon oil solvent (i.e. deep fat, η=30000cps,
η is viscosity) in, take out after 6h；Ceramic bead biscuit after taking out is de-after being dried 4h in being placed in 40 DEG C of thermostatic drying chambers
Skin；Using high temperature process furnances to biscuit binder removal, dump temperature is 630 DEG C, and temperature retention time is 6 hours；By the biscuit after binder removal
Sintering in the sintering furnace that sintering atmosphere is nitrogen, sintering temperature is 1850 DEG C, temperature retention time 2 hours, after quiet through heat etc.
Pressure obtains MgAlON crystalline ceramics bead after processing (1850 DEG C, 200MPa be incubated 2h).
The present embodiment configuration the viscosity that solid phase amount is 45vol%MgAlON ceramic slurry be 78mPa s, it is thus achieved that MgAlON
Ceramic bead biscuit sphere diameter is uniform, and sphere diameter mean size is 1mm, and out-of-roundness is 1.25% (explanation good sphericity), makes pottery after pre-burning
Porcelain bead consistency is 94.3%, and after high temperature insostatic pressing (HIP), ceramic bead 24h is 0.2% from wear rate (43.6r/min, 24h).Macroscopic view
Observe lower MgAlON Ceramic Balls glittering and translucent, and permeable Ceramic Balls profile view observes font, illustrates have optical transmittance.
Embodiment 2:
Prepared by ceramic size: prepared the solution 10ml of PH=10 by strong aqua ammonia regulation deionized water；Weigh MgAlON powder body
25.25g (solid concentration is 45vol%), Methacrylamide 1.5g (15vol% of aqueous solution), MBAM0.4g (aqueous solution
4vol%), TAC0.125g (0.5wt% of MgAlON powder quality), uniformly mixing is placed on blender stirring 4h,
Obtain pottery serosity；Pottery serosity (slip) is placed in vacuum environment (vacuum 5kPa) stirring 20min and gets rid of gas in serosity
Bubble, adds peroxo disulfate acid ammonium 400ul (4vol% of aqueous solution) mix homogeneously afterwards；Quantitatively being added dropwise to temperature is 90 DEG C high
In the degree dimethyl-silicon oil solvent (i.e. deep fat, η=30000cps) for 150cm, take out after 6h；Pottery after taking out
Bead biscuit is dried 4h rear peeling in being placed in 40 DEG C of thermostatic drying chambers；Biscuit binder removal, dump temperature are by use high temperature process furnances
630 DEG C, temperature retention time is 6 hours；Being sintered in the sintering furnace that sintering atmosphere is nitrogen by biscuit after binder removal, sintering temperature is
1850 DEG C, temperature retention time 2 hours, after after hip treatment (1880 DEG C, 200MPa be incubated 2h), obtain MgAlON
Crystalline ceramics bead.
The present embodiment configuration the viscosity that solid phase amount is 50vol%MgAlON ceramic slurry be 64mPa s, it is thus achieved that MgAlON
Ceramic bead biscuit sphere diameter is uniform, and sphere diameter mean size is 2mm, and out-of-roundness is 1.45% (explanation good sphericity), makes pottery after pre-burning
Porcelain bead consistency is 94.1%, and after high temperature insostatic pressing (HIP), ceramic bead 24h is 0.23% from wear rate (43.6r/min, 24h).Grand
Observe lower MgAlON Ceramic Balls glittering and translucent, and permeable Ceramic Balls profile view observes font, illustrates have optical transmittance.
Embodiment 3:
As it is shown in figure 1, prepared by ceramic size: prepared the solution 10ml of PH=11.6 by strong aqua ammonia regulation deionized water；Weigh
MgAlON powder body 33.6g (solid concentration is 48vol%), MAM2.0g (20vol% of aqueous solution), MBAM0.4g (water
The 4vol% of solution), TAC0.16g (0.5wt% of MgAlON powder quality), uniformly mixing is placed on blender stirring
4h, it is thus achieved that pottery serosity；Pottery serosity (slip) is placed in vacuum environment (vacuum 15kPa) stirring 30min and gets rid of slurry
Bubble in liquid, adds peroxo disulfate acid ammonium 400ul (7vol% of aqueous solution) mix homogeneously afterwards；Quantitatively being added dropwise to temperature is 90
DEG C height is in the dimethyl-silicon oil solvent (i.e. deep fat, η=30000cps) of 150cm, takes out after 8h；After taking out
Ceramic bead biscuit is dried 6h rear peeling in being placed in 40 DEG C of thermostatic drying chambers；Use high temperature process furnances to biscuit binder removal, binder removal temperature
Degree is 630 DEG C, and temperature retention time is 6 hours；Biscuit after binder removal is sintered in the sintering furnace that sintering atmosphere is nitrogen, sintering
Temperature is 1850 DEG C, temperature retention time 3 hours, after after the hip treatment (1880 DEG C, 200MPa be incubated 2h)
To MgAlON crystalline ceramics bead.
The present embodiment configuration the viscosity that solid phase amount is 48vol%MgAlON ceramic slurry be 76mPa s, it is thus achieved that MgAlON
Ceramic bead biscuit sphere diameter is uniform, and sphere diameter mean size is 2mm, and out-of-roundness is 1.30% (explanation good sphericity), makes pottery after pre-burning
Porcelain bead consistency is 95.0%, and after high temperature insostatic pressing (HIP), ceramic bead 24h is 0.2% from wear rate (43.6r/min, 24h).Macroscopic view
Observe lower MgAlON Ceramic Balls glittering and translucent, and permeable Ceramic Balls profile view observes font.
Fig. 2 illustrates that the Ceramic Balls biscuit diameter Distribution that Gel-casting process prepares is consistent, and discreteness is little, Fig. 3 then illustrate through
After pressureless sintering, Ceramic Balls internal porosity isolates, is positioned at grain boundaries, can eliminate pore through hip treatment, and Fig. 4 illustrates
After HIP sintering, consistency improves further, and pore is basically eliminated, and Fig. 5 (a) illustrates the MgAlON pottery prepared
Porcelain ball is the most glittering and translucent, has light transmission；Fig. 5 (b) illustrates by crystalline ceramics ball section it is observed that word,
The optical transmittance of Ceramic Balls is reflected from side.
Embodiment 4:
Prepared by ceramic size: prepared the solution 10ml of PH=12 by strong aqua ammonia regulation deionized water；Weigh MgAlON powder body
33.6g (solid concentration is 48vol%), Methacrylamide 2.5g (25vol% of aqueous solution), MBAM0.5g (aqueous solution
5vol%), TAC0.10g (0.3wt% of MgAlON powder quality), uniformly mixing is placed on blender stirring 5h,
Obtain pottery serosity；Pottery serosity (slip) is placed in vacuum environment (vacuum 10kPa) stirring 30min get rid of in serosity
Bubble, adds peroxo disulfate acid ammonium 720ul (7.2vol% of aqueous solution) mix homogeneously afterwards；Quantitatively being added dropwise to temperature is 90 DEG C
It is highly in the dimethyl-silicon oil solvent (i.e. deep fat, η=40000cps) of 150cm, takes out after 8h；Pottery after taking out
Porcelain bead biscuit is dried 6h rear peeling in being placed in 60 DEG C of thermostatic drying chambers；Use high temperature process furnances to biscuit binder removal, dump temperature
Being 630 DEG C, temperature retention time is 8 hours；Biscuit after binder removal is sintered in the sintering furnace that sintering atmosphere is nitrogen, sintering temperature
Degree is 1850 DEG C, temperature retention time 2 hours, after obtain after hip treatment (1900 DEG C, 200MPa be incubated 2h)
MgAlON crystalline ceramics bead.
The present embodiment configuration the viscosity that solid phase amount is 48vol%MgAlON ceramic slurry be 80mPa s, it is thus achieved that MgAlON
Ceramic bead biscuit sphere diameter is uniform, and sphere diameter mean size is 3mm, and out-of-roundness is 2.25% (explanation good sphericity), makes pottery after pre-burning
Porcelain bead consistency is 94.3%, and after high temperature insostatic pressing (HIP), ceramic bead 24h is 0.24% from wear rate (43.6r/min, 24h).Grand
Observe lower MgAlON Ceramic Balls glittering and translucent, and permeable Ceramic Balls profile view observes font.
Embodiment 5:
Prepared by ceramic size: prepared the solution 10ml of PH=10.5 by strong aqua ammonia regulation deionized water；Weigh MgAlON powder
Body 36.45g (solid concentration is 50vol%), MAM2g (20vol% of solution), MBAM0.4g (4vol% of solution),
TAC0.11g (0.3wt% of MgAlON powder quality), uniformly mixing is placed on blender stirring 4h, it is thus achieved that pottery serosity；
Pottery serosity (slip) is placed in vacuum environment (vacuum 10kPa) stirring 25min and gets rid of bubble in serosity, add afterwards
Peroxo disulfate acid ammonium 1360ul (13.6vol% of aqueous solution) mix homogeneously；Quantitatively be added dropwise to temperature be 90 DEG C of height be 150cm
Dimethyl-silicon oil solvent (i.e. deep fat, η=40000cps) in, after 8h take out；Ceramic bead biscuit after taking out is put
6h rear peeling it is dried in 60 DEG C of thermostatic drying chambers；Using high temperature process furnances to biscuit binder removal, dump temperature is 700 DEG C, insulation
Time is 6 hours；Being sintered in the sintering furnace that sintering atmosphere is nitrogen by biscuit after binder removal, sintering temperature is 1875 DEG C, protects
2 hours time of temperature, after after hip treatment (1900 DEG C, 200MPa be incubated 2h), obtain the transparent pottery of MgAlON
Porcelain bead.
The present embodiment configuration the viscosity that solid phase amount is 50vol%MgAlON ceramic slurry be 86mPa s, it is thus achieved that MgAlON
Ceramic bead biscuit sphere diameter is uniform, and sphere diameter mean size is 3mm, and out-of-roundness is 1.75% (explanation good sphericity), makes pottery after pre-burning
Porcelain bead consistency is 95.2%, and after high temperature insostatic pressing (HIP), ceramic bead 24h is 0.17% from wear rate (43.6r/min, 24h).Grand
Observe lower MgAlON Ceramic Balls glittering and translucent, and permeable Ceramic Balls profile view observes font.
Embodiment 6:
Prepared by ceramic size: prepared the solution 10ml of PH=10.5 by strong aqua ammonia regulation deionized water；Weigh MgAlON powder
Body 36.45g (solid concentration is 50vol%), MAM2.5g (25vol% of aqueous solution), MBAM0.5g (5vol% of aqueous solution),
TAC0.11g (0.3wt% of MgAlON powder quality), uniformly mixing is placed on blender stirring 5h, it is thus achieved that pottery serosity；
Pottery serosity (slip) is placed in vacuum environment (vacuum 10kPa) stirring 30min and gets rid of bubble in serosity, add afterwards
Peroxo disulfate acid ammonium 1560ul (15.6vol% of aqueous solution) mix homogeneously；Quantitatively be added dropwise to temperature be 90 DEG C of height be 150cm
Dimethyl-silicon oil solvent (i.e. deep fat, η=30000cps) in, after 10h take out；Ceramic bead biscuit after taking out is put
8h rear peeling it is dried in 60 DEG C of thermostatic drying chambers；Using high temperature process furnances to biscuit binder removal, dump temperature is 700 DEG C, insulation
Time is 8 hours；Being sintered in the sintering furnace that sintering atmosphere is nitrogen by biscuit after binder removal, sintering temperature is 1875 DEG C, protects
2 hours time of temperature, after after hip treatment (1850 DEG C, 200MPa be incubated 2h), obtain the transparent pottery of MgAlON
Porcelain bead.
The present embodiment configuration the viscosity that solid phase amount is 50vol%MgAlON ceramic slurry be 90mPa s, it is thus achieved that MgAlON
Ceramic bead biscuit sphere diameter is uniform, and sphere diameter mean size is 4mm, and out-of-roundness is 2.05% (explanation good sphericity), makes pottery after pre-burning
Porcelain bead consistency is 94.6%, and after high temperature insostatic pressing (HIP), ceramic bead 24h is 0.21% from wear rate (43.6r/min, 24h).Grand
Observe lower MgAlON Ceramic Balls glittering and translucent, and permeable Ceramic Balls profile view observes font.
Embodiment 7:
Prepared by ceramic size: prepared the solution 10ml of PH=11.2 by strong aqua ammonia regulation deionized water；Weigh MgAlON powder
Body 36.45g (solid concentration is 50vol%), MAM2.5g (25vol% of aqueous solution), MBAM0.6g (6vol% of aqueous solution),
TAC0.14g (0.4wt% of MgAlON powder quality), uniformly mixing is placed on blender stirring 5h, it is thus achieved that pottery serosity；
Pottery serosity (slip) is placed in vacuum environment (vacuum 15kPa) stirring 40min and gets rid of bubble in serosity, add afterwards
Peroxo disulfate acid ammonium 1560ul (15.6vol% of aqueous solution) mix homogeneously；Quantitatively be added dropwise to temperature be 80 DEG C of height be 150cm
Dimethyl-silicon oil solvent (i.e. deep fat, η=60000cps) in, after 10h take out；Ceramic bead biscuit after taking out is put
8h rear peeling it is dried in 40 DEG C of thermostatic drying chambers；Using high temperature process furnances to biscuit binder removal, dump temperature is 800 DEG C, insulation
Time is 8 hours；Being sintered in the sintering furnace that sintering atmosphere is nitrogen by biscuit after binder removal, sintering temperature is 1875 DEG C, protects
3 hours time of temperature, after after hip treatment (1880 DEG C, 160MPa be incubated 3h), obtain the transparent pottery of MgAlON
Porcelain bead.
The present embodiment configuration the viscosity that solid phase amount is 50vol%MgAlON ceramic slurry be 90mPa s, it is thus achieved that MgAlON
Ceramic bead biscuit sphere diameter is uniform, and sphere diameter mean size is 3mm, and out-of-roundness is 1.85% (explanation good sphericity), makes pottery after pre-burning
Porcelain bead consistency is 94.6%, and after high temperature insostatic pressing (HIP), ceramic bead 24h is 0.23% from wear rate (43.6r/min, 24h).Grand
Observe lower MgAlON Ceramic Balls glittering and translucent, and permeable Ceramic Balls profile view observes font.
Claims (10)
1. the method that a gel injection-moulding prepares MgAlON crystalline ceramics bead, it is characterised in that comprise the steps:
1) dispensing: use strong aqua ammonia regulation deionized water pH value, it is thus achieved that the aqueous solution of pH=10-12；
Being aqueous solution 45-50vol% by the addition of MgAlON powder body, the addition of Methacrylamide (MAM) is water-soluble
Liquid 15-25vol%, the addition of methylene-bisacrylamide (MBAM) is aqueous solution 4-6vol%, triammonium citrate (TAC)
The 0.2-0.5wt% that addition is MgAlON powder body weight, choose MgAlON powder body, Methacrylamide, methylene
Bisacrylamide, triammonium citrate；
By MgAlON powder body, Methacrylamide, methylene-bisacrylamide, triammonium citrate and aqueous solution, at least
After stirring 4h, it is thus achieved that pottery serosity；
2) ball processed: pottery serosity is placed in vacuum environment stirring 20-40min；Take out and add peroxo disulfate acid ammonium (APS),
The 4-15.6vol% that addition is aqueous solution of peroxo disulfate acid ammonium, obtains ceramic slurry；Ceramic slurry is instilled and is highly not less than
130cm, temperature is not less than in the dimethyl-silicon oil solvent of 60 DEG C, after being incubated at least 6h, takes out the ceramic bead biscuit prepared；
3) it is dried and binder removal: prepared ceramic bead biscuit is placed in 40-60 DEG C of drying baker inside holding 4-8h, takes out and is placed on tubular type
In stove, 630-800 DEG C is incubated at least 6h；
4) sintering: the ceramic bead biscuit after binder removal is sintered in atmosphere furnace, and firing temperature is not less than 1850 DEG C, temperature retention time
For 2-3h, obtain the Ceramic Balls sintered body after pre-burning；
5) high temperature insostatic pressing (HIP): the Ceramic Balls sintered body after pre-burning carries out hip treatment, 1850-1900 DEG C, 160-200MPa guarantor
Temperature 2-3h, obtains MgAlON crystalline ceramics bead.
The method that a kind of gel injection-moulding the most according to claim 1 prepares MgAlON crystalline ceramics bead, it is characterised in that:
The particle diameter of described MgAlON powder body is 0.3-0.5 μm, and purity is not less than 99.99wt%.
The method that a kind of gel injection-moulding the most according to claim 1 prepares MgAlON crystalline ceramics bead, it is characterised in that:
The viscosity scope of used dimethyl-silicon oil solvent is 300000-600000cps.
The method that a kind of gel injection-moulding the most according to claim 1 prepares MgAlON crystalline ceramics bead, it is characterised in that:
The concentration of described strong aqua ammonia is 80wt%-95wt%.
The method that a kind of gel injection-moulding the most according to claim 1 prepares MgAlON crystalline ceramics bead, it is characterised in that:
The vacuum of described vacuum environment is 5-15kPa.
The method that a kind of gel injection-moulding the most according to claim 1 prepares MgAlON crystalline ceramics bead, it is characterised in that:
Step 1) at least stirring 4h for stirring 4-6h.
The method that a kind of gel injection-moulding the most according to claim 1 prepares MgAlON crystalline ceramics bead, it is characterised in that:
Step 2) in vacuum environment in stirring for stirring in froth in vacuum machine or de-airing mixer stir.
The method that a kind of gel injection-moulding the most according to claim 1 prepares MgAlON crystalline ceramics bead, it is characterised in that:
Step 2) in height to be not less than 130cm be 130-150cm；Temperature is not less than 60 DEG C for 60-90 DEG C；Being incubated at least 6h is
6-10h。
The method that a kind of gel injection-moulding the most according to claim 1 prepares MgAlON crystalline ceramics bead, it is characterised in that:
Step 3) in insulation at least 6h be 6-8h.
The method that a kind of gel injection-moulding the most according to claim 1 prepares MgAlON crystalline ceramics bead, its feature exists
In step 4) in the sintering atmosphere that is sintered of atmosphere furnace be nitrogen.
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