CN108610038A - A kind of method that zirconium oxide prepares YAG crystalline ceramics with the sintering of YAG powder double-layer embedments - Google Patents
A kind of method that zirconium oxide prepares YAG crystalline ceramics with the sintering of YAG powder double-layer embedments Download PDFInfo
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Abstract
The invention discloses a kind of zirconium oxides and YAG powder double-layer embedments to be sintered the method for preparing YAG crystalline ceramics, this method includes being pumped into ammonium bicarbonate soln into ruthenium ion and aluminum ions mixed solution, by ageing, washing, it is dry, sieving obtains presoma, again through calcining, ball milling, sieving, it is dry-pressing formed, after isostatic cool pressing obtains YAG biscuits, YAG biscuits are embedded according to the arrangement mode of Zirconium powder-YAG powders-YAG biscuits-YAG powders-Zirconium powder, it is handled then in turn through vacuum-sintering and grinding and polishing, it is final to obtain YAG crystalline ceramics.Present invention Zirconium powder in vacuum-sintering can provide oxonium ion to YAG powders and YAG biscuits, the generation of the internal Lacking oxygen of YAG ceramics in sintering stage can effectively be inhibited, to prevent the decline of YAG crystalline ceramics transmitances, and annealing steps are omitted, are more energy-saving and environmentally friendly.
Description
Technical field
The invention belongs to crystalline ceramics preparing technical fields, and in particular to a kind of zirconium oxide is burnt with YAG powder double-layer embedments
Tie the method for preparing YAG crystalline ceramics.
Background technology
YAG crystalline ceramics has the characteristics that intensity is big, heat-resist, corrosion resistance is strong, and equal to visible light and infrared light
There is good permeability, these properties make YAG crystalline ceramics can be applied to high pressure gas fluorescent tube, high temperature window material, laser
The fields such as ceramics, scintillating ceramic.Therefore, it prepares YAG crystalline ceramics to have broad application prospects, is the heat of material science research
One of point.
In traditional crystalline ceramics preparation process, most common sintering processing is vacuum-sintering.Vacuum-sintering relative to
Other sintering processings (such as hot isostatic pressing, discharge plasma sintering) have the characteristics that efficient, energy saving.But in vacuum-sintering
There is also can color burnt hair after many problems, such as YAG crystalline ceramics vacuum-sinterings in the process.Reason is primarily due in vacuum
In sintering process, due to being anoxia condition in vacuum drying oven, the oxonium ion in YAG ceramics will escape, to generate oxygen sky
Position.For this problem, previous researcher often after vacuum-sintering to YAG ceramics carry out for a long time (10h or more) air or
Person's oxygen atmosphere is annealed, and Lacking oxygen is eliminated with this.But after annealing, due to remaining in the impurity meetings such as carbon, sulphur inside ceramics
It is excluded in annealing stage, to leave some nanoapertures, these holes can seriously reduce the transmitance of crystalline ceramics.
Invention content
The object of the present invention is to provide the sides that a kind of zirconium oxide and the sintering of YAG powder double-layer embedments prepare YAG crystalline ceramics
Method, YAG ceramics do not have color burnt hair phenomenon, ceramic transmitance to significantly improve after vacuum-sintering, and need not subsequently be moved back
Fire.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of method that zirconium oxide prepares YAG crystalline ceramics with the sintering of YAG powder double-layer embedments, it includes the following steps：
1) presoma is prepared：Compound concentration is the yttrium nitrate solution of 0.1~0.3mol/L, and ten are added into yttrium nitrate solution
Two hydrazine aluminum sulfate ammonium crystal, stir evenly, and form mixed solution, wherein ruthenium ion and aluminum ions molar ratio are 3:5；It is stirring
It mixes and the ammonium bicarbonate soln of a concentration of 1.5~2mol/L is pumped in mixed solution with peristaltic pump under state；Monitor reactant
The pH value of system stops pumping and stirring when pH value reaches 8.0~8.2, by reaction system still aging 12~for 24 hours, to ageing
Presoma afterwards is washed, is filtered, is dried successively, obtains precursor powder；
2) it calcines：The precursor powder that step 1) is obtained carries out sieving processing, is put into after sieving in Muffle furnace in 1100
~1300 DEG C of 2~4h of calcining, obtain a nanometer YAG powders；
3) ball milling：The ethyl orthosilicate of 0.4~0.6wt.% is added in the nanometer YAG powders obtained to step 2), then adds
Enter absolute ethyl alcohol and high purity aluminium oxide abrading-ball, carries out ball milling mixing and obtain slurry, sieving processing is carried out after slurry is dried；
4) it is molded：By step 3) be sieved after powder be put into mold, using it is dry pressure formed go out round YAG biscuits, with
Isostatic cool pressing processing is carried out afterwards；
5) it is sintered：The YAG biscuits that step 4) obtains are placed in Muffle furnace and carry out biscuiting, remove residual organic matter；Again will
YAG biscuits after biscuiting are placed in tungsten crucible A, according to Zirconium powder-YAG powders-YAG biscuits-YAG powders-oxidation
The arrangement mode of zirconium powder body is embedded；After embedding, the bigger tungsten crucible B of bore is buckled to above tungsten crucible A, to prevent
Powder is taken away by mechanical pump or molecular pump, is then placed in vacuum sintering furnace and carries out vacuum-sintering；
6) grinding and polishing：Potsherd after vacuum-sintering is subjected to Two sides milling and polishing to 1~3mm, obtains the transparent potteries of YAG
Porcelain.
Preferably, in step (1) when pumping ammonium bicarbonate soln, pump rate is 1~6mL/min, mixing speed 300
~500rpm.
Preferably, washing described in step (1) is first to be washed with deionized water 2~4 times, then washed 2~4 times with absolute ethyl alcohol；
The drying temperature is 40~60 DEG C, and drying time is 12~36h.
Preferably, it is 100~200 mesh that sieving, which uses sieve specification, in step (2), and sieving number is 3~5 times.
Preferably, rotational speed of ball-mill described in step (3) be 160~200rpm, Ball-milling Time be 12~for 24 hours, the drying
Temperature is 40~60 DEG C, and drying time is 12~36h, and the sieve specification is 100~200 mesh, and sieving number is 3~5 times.
Preferably, dry-pressing pressure described in step (4) is 25~35MPa, and the dwell time is 1~3min, round YAG biscuits
A diameter of 16~30mm；The pressure of the isostatic cool pressing is 200~240Mpa, and the dwell time is 4~8min.
Preferably, biscuiting temperature described in step (5) is 800~900 DEG C, and the biscuiting time is 5~8h；In vacuum sintering furnace
Vacuum degree be 1.0 × 10-5~1.0 × 10-3Pa, vacuum-sintering temperature are 1760~1800 DEG C, and sintering time is 8~20h.
Preferably, the thickness ratio of Zirconium powder layer and YAG biscuits is 1.0~3.0, YAG powders when embedding in step (5)
The thickness ratio of layer and YAG biscuits is 3.0~4.0.
Preferably, the internal diameter of the tungsten crucible B is 1.2~2.0 times of the outer diameter of tungsten crucible A.
The present invention prepares YAG crystalline ceramics using coprecipitation, in the vacuum-sintering stage, using zirconium oxide and YAG bilayers
Powder embeds biscuit of ceramics, to inhibit the generation of Lacking oxygen, improves the optical quality of YAG ceramics.
Compared with prior art, the present invention has the advantages that：
(1) in the vacuum-sintering stage, using a certain proportion of zirconium oxide and YAG powders, by biscuit according to zirconia powder
Body-YAG powders-YAG biscuits-YAG powders-Zirconium powder mode is embedded, and is then carried out in vacuum sintering furnace
Vacuum-sintering.Since in vacuum-sintering, Zirconium powder can provide oxonium ion to YAG powders and YAG biscuits, therefore can effectively press down
The generation for making the Lacking oxygen in sintering stage, to prevent YAG ceramics transmitances from declining.
(2) due to inhibiting the generation of Lacking oxygen in the vacuum-sintering stage, traditional annealing process is not needed, is reduced
Due to stay in the impurity such as the carbon in ceramics, sulphur be excluded in annealing process and the generation of nanoaperture that leaves.And due to
The step for annealing is omitted is more energy-saving and environmentally friendly, and has great impetus to the mass production of YAG ceramics.
Description of the drawings
Fig. 1 is the device of the invention figure；
Fig. 2 is the installation drawing of comparative example of the present invention.
In figure, 1- tungsten crucibles A, 2- Zirconium powder layer, 3-YAG powder layers, 4-YAG biscuits, 5- tungsten crucibles B.
Fig. 3 is the crystalline ceramics sample drawing that the embodiment of the present invention 1 obtains.
In figure, (a) is the crystalline ceramics sample after vacuum-sintering, is (b) the crystalline ceramics sample after direct grinding and polishing.
Fig. 4 is the crystalline ceramics sample drawing that comparative example of the present invention obtains.
In figure, (a) is the crystalline ceramics sample after vacuum-sintering, is (b) the crystalline ceramics sample after annealing, grinding and polishing
Product.
Specific implementation mode
The invention will be further described with specific example below in conjunction with the accompanying drawings, but the protection of the present invention should not be limited with this
Range.
Embodiment 1：d(ZrO2):D (YAG biscuits)=1.0 prepares YAG crystalline ceramics
Y (NO are poured into container3)3·6H2O crystal adds deionized water to be diluted to Y (NO3)3Solution, Y3+Solution concentration is
NH is added into yttrium nitrate solution by 0.1mol/L4Al(SO4)2·12H2O crystal ensures Y3+With Al3+Molar ratio is 3:5, with stirring
It mixes device to stir evenly, mixing speed 300rpm, forms mixed solution；It will be a concentration of with peristaltic pump under stirring
The NH of 1.5mol/L4HCO3It is pumped in mixed solution, the mode that precipitating reagent is pumped into mixed solution is to spray into, and pump rate is
1mL/min；The pH value that reaction system is measured with pH meter stops pumping and stirring when pH value reaches 8.0, and reaction system is quiet
Set ageing 12h.Presoma after ageing is first washed with deionized water 2 times, then is washed 2 times with absolute ethyl alcohol, is incited somebody to action after suction filtration
To presoma be placed in oven and dried, drying temperature be 40 DEG C, drying time 12h.
Precursor powder after drying is subjected to sieving processing, sieve specification is 100 mesh, is sieved 5 times.Horse is put into after sieving
2h not is calcined in 1100 DEG C in stove, obtains a nanometer YAG powders.
The TEOS of 0.4wt.% will be added in the powder calcined, adds absolute ethyl alcohol and high purity aluminium oxide abrading-ball, into
Row ball milling mixing, rotational speed of ball-mill 160rpm, Ball-milling Time 12h.Then slurry is placed in oven and dried, drying temperature is
40 DEG C, drying time 12h, sieving processing is then carried out, sieve specification is 100 mesh, is sieved 5 times.
The progress of gained powder is dry-pressing formed, and dry-pressing pressure is 25MPa, dwell time 1min, is pressed as a diameter of 16mm
Round biscuit.Isostatic cool pressing processing is then carried out, the pressure of isostatic cool pressing is 200Mpa, dwell time 4min.
Biscuit is placed in Muffle furnace in 800 DEG C of biscuiting 5h, residual organic matter is removed；As shown in Figure 1, by the element after biscuiting
Base is placed in tungsten crucible A1, according to Zirconium powder-YAG powders-YAG biscuits-YAG powders-Zirconium powder mode
It is embedded, the thickness ratio of the Zirconium powder layer 2 that wherein covering uses and YAG biscuits 4 is plain for 1.0, YAG powder layers 3 and YAG
The thickness ratio of base 4 is 3.0.The bigger tungsten crucible B5 of one bore of back-off above tungsten crucible A1, to prevent powder by mechanical pump or
Person's molecular pump is taken away, wherein tungsten crucible B5 internal diameters are 1.2 times of tungsten crucible A1 outer diameters.Then vacuum sintering furnace is placed it in
Middle carry out vacuum-sintering, the vacuum degree in vacuum sintering furnace are 1.0 × 10-5Pa, vacuum-sintering temperature are 1760 DEG C, sintering time
For 20h.Since during vacuum-sintering, Zirconium powder can provide oxonium ion to YAG powders and YAG biscuits, can effectively press down
The generation of Lacking oxygen in potting porcelain.Therefore, the phenomenon that YAG crystalline ceramics after vacuum-sintering not will produce color burnt hair, is not required to
Take further annealing, the high optical quality of crystalline ceramics that can be ensured.Fig. 3 (a) is the transparent potteries of YAG after vacuum-sintering
Porcelain sample, sample illustrates that almost anaerobic is empty inside vacuum-sintering stage ceramics without burnt hair phenomenon after vacuum-sintering as seen from the figure
Position generates, and need not take further annealing.
Potsherd after vacuum-sintering is directly carried out to Two sides milling and polishing to 1mm, obtains YAG crystalline ceramics.Fig. 3 (b)
For the YAG crystalline ceramics samples after polishing, it is seen that almost without scattering point inside crystalline ceramics, optical quality is high.
Embodiment 2：d(ZrO2):D (YAG biscuits)=2.0 prepares YAG crystalline ceramics
Y (NO are poured into container3)3·6H2O crystal adds deionized water to be diluted to Y (NO3)3Solution, Y3+Solution concentration is
NH is added into yttrium nitrate solution by 0.2mol/L4Al(SO4)2·12H2O crystal ensures Y3+With Al3+Molar ratio is 3:5, with stirring
It mixes device to stir evenly, mixing speed 400rpm, forms mixed solution；It will be a concentration of with peristaltic pump under stirring
The NH of 1.8mol/L4HCO3It is pumped in mixed solution, the mode that precipitating reagent is pumped into yttrium nitrate solution is to spray into, pump rate
For 2mL/min；The pH value that reaction system is measured with pH meter stops pumping and stirring, by reaction system when pH value reaches 8.1
Still aging 16h.Presoma after ageing is first washed with deionized water 3 times, then is washed 3 times with absolute ethyl alcohol, it will after suction filtration
Obtained presoma is placed in oven and dried, and drying temperature is 50 DEG C, and drying time is for 24 hours.
Precursor powder after drying is subjected to sieving processing, sieve specification is 150 mesh, is sieved 4 times.Horse is put into after sieving
3h not is calcined in 1200 DEG C in stove, obtains a nanometer YAG powders.
The TEOS of 0.5wt.% will be added in the powder calcined, adds absolute ethyl alcohol and high purity aluminium oxide abrading-ball, into
Row ball milling mixing, rotational speed of ball-mill 180rpm, Ball-milling Time 20h.Then slurry is placed in oven and dried, drying temperature is
50 DEG C, drying time 20h, sieving processing is then carried out, sieve specification is 150 mesh, is sieved 4 times.
The progress of gained powder is dry-pressing formed, and dry-pressing pressure is 30MPa, dwell time 2min, is pressed as a diameter of 20mm
Round biscuit.Isostatic cool pressing processing is then carried out, the pressure of isostatic cool pressing is 220Mpa, dwell time 5min.
Biscuit is placed in Muffle furnace in 850 DEG C of biscuiting 6h, residual organic matter is removed；As shown in Figure 1, by the element after biscuiting
Base is placed in tungsten crucible A1, according to Zirconium powder-YAG powders-YAG biscuits-YAG powders-Zirconium powder mode
It is embedded, the thickness ratio of the Zirconium powder layer 2 that wherein covering uses and YAG biscuits 4 is plain for 2.0, YAG powder layers 3 and YAG
The thickness ratio of base 4 is 3.5.The bigger tungsten crucible B5 of one bore of back-off above tungsten crucible A1, to prevent powder by mechanical pump or
Person's molecular pump is taken away, wherein tungsten crucible B5 internal diameters are 1.5 times of tungsten crucible A1 outer diameters.Then vacuum sintering furnace is placed it in
Middle carry out vacuum-sintering, the vacuum degree in vacuum sintering furnace are 1.0 × 10-4Pa, vacuum-sintering temperature are 1780 DEG C, sintering time
For 16h.Since during vacuum-sintering, Zirconium powder can provide oxonium ion to YAG powders and YAG biscuits, can effectively press down
The generation of Lacking oxygen in potting porcelain.Therefore, the YAG crystalline ceramics after vacuum-sintering is without color burnt hair phenomenon, need not take into
The high optical quality of one step annealing, crystalline ceramics is ensured.
Potsherd after vacuum-sintering is subjected to Two sides milling and polishing to 1.2mm, obtains YAG crystalline ceramics.
Embodiment 3：d(ZrO2):D (YAG biscuits)=3.0 prepares YAG crystalline ceramics
Y (NO are poured into container3)3·6H2O crystal adds deionized water to be diluted to Y (NO3)3Solution, Y3+Solution concentration is
NH is added into yttrium nitrate solution by 0.3mol/L4Al(SO4)2·12H2O crystal ensures Y3+With Al3+Molar ratio is 3:5, with stirring
It mixes device to stir evenly, mixing speed 500rpm, forms mixed solution；With peristaltic pump by a concentration of 2mol/L under stirring
NH4HCO3It is pumped in mixed solution, the mode that precipitating reagent is pumped into yttrium nitrate solution is to spray into, pump rate 6mL/
min；The pH value that reaction system is measured with pH meter stops pumping and stirring, reaction system is stood old when pH value reaches 8.2
Change 20h.It presoma after ageing is first washed with deionized water 4 times, then is washed 4 times with absolute ethyl alcohol, will obtained after suction filtration
Presoma is placed in oven and dried, and drying temperature is 60 DEG C, drying time 36h.
Precursor powder after drying is subjected to sieving processing, sieve specification is 200 mesh, is sieved 3 times.Horse is put into after sieving
1300 DEG C of calcining 4h are not carried out in stove, obtain a nanometer YAG powders.
The TEOS of 0.6wt.% will be added in the powder calcined, adds absolute ethyl alcohol and high purity aluminium oxide abrading-ball, into
Row ball milling mixing, rotational speed of ball-mill 200rpm, Ball-milling Time are for 24 hours.Then slurry is placed in oven and dried, drying temperature is
60 DEG C, drying time 36h, after carry out sieving processing, sieve specification is 200 mesh, is sieved 3 times.
The progress of gained powder is dry-pressing formed, and dry-pressing pressure is 35MPa, dwell time 3min, is pressed as a diameter of 30mm
Round biscuit.Isostatic cool pressing processing is then carried out, the pressure of isostatic cool pressing is 240Mpa, dwell time 8min.
Biscuit is placed in Muffle furnace in 900 DEG C of biscuiting 8h, residual organic matter is removed；As shown in Figure 1, by the element after biscuiting
Base is placed in tungsten crucible A1, according to Zirconium powder-YAG powders-YAG biscuits-YAG powders-Zirconium powder mode
It is embedded, the thickness ratio of the Zirconium powder layer 2 that wherein covering uses and YAG biscuits 4 is plain for 3.0, YAG powder layers 3 and YAG
The thickness ratio of base 4 is 4.0.The bigger tungsten crucible B5 of one bore of back-off above tungsten crucible A1, to prevent powder by mechanical pump or
Person's molecular pump is taken away, wherein tungsten crucible B5 internal diameters are 2.0 times of tungsten crucible A1 outer diameters.Then vacuum sintering furnace is placed it in
Middle carry out vacuum-sintering, the vacuum degree in vacuum sintering furnace are 1.0 × 10-3Pa, vacuum-sintering temperature are 1800 DEG C, sintering time
For 20h.Since during vacuum-sintering, Zirconium powder can provide oxonium ion to YAG powders and YAG biscuits, can effectively press down
The generation of Lacking oxygen in potting porcelain.Therefore, the YAG crystalline ceramics after vacuum-sintering is without color burnt hair phenomenon, need not take into
The high optical quality of one step annealing, crystalline ceramics is ensured.
Potsherd after vacuum-sintering is subjected to Two sides milling and polishing to 3mm, obtains YAG crystalline ceramics.
Comparative example：The embedding of single layer YAG powders prepares YAG crystalline ceramics
Y (NO are poured into container3)3·6H2O crystal adds deionized water to be diluted to Y (NO3)3Solution, Y3+Solution concentration is
NH is added into yttrium nitrate solution by 0.1mol/L4Al(SO4)2·12H2O crystal ensures Y3+With Al3+Molar ratio is 3:5, with stirring
It mixes device to stir evenly, mixing speed 300rpm, forms mixed solution；It will be a concentration of with peristaltic pump under stirring
The NH of 1.5mol/L4HCO3It is pumped in mixed solution, the mode that precipitating reagent is pumped into mixed solution is to spray into, and pump rate is
1mL/min；The pH value that reaction system is measured with pH meter stops pumping and stirring when pH value reaches 8.0, and reaction system is quiet
Set ageing 12h.Presoma after ageing is first washed with deionized water 2 times, then is washed 2 times with absolute ethyl alcohol, is incited somebody to action after suction filtration
To presoma be placed in oven and dried, drying temperature be 40 DEG C, drying time 12h.
Precursor powder after drying is subjected to sieving processing, sieve specification is 100 mesh, is sieved 5 times.Horse is put into after sieving
2h not is calcined in 1100 DEG C in stove, obtains a nanometer YAG powders.
The TEOS of 0.4wt.% will be added in the powder calcined, adds absolute ethyl alcohol and high purity aluminium oxide abrading-ball, into
Row ball milling mixing, rotational speed of ball-mill 160rpm, Ball-milling Time 12h.Then slurry is placed in oven and dried, drying temperature is
40 DEG C, drying time 12h, sieving processing is then carried out, sieve specification is 100 mesh, is sieved 5 times.
The progress of gained powder is dry-pressing formed, and dry-pressing pressure is 25MPa, dwell time 1min, is pressed as a diameter of 16mm
Round biscuit.Isostatic cool pressing processing is then carried out, the pressure of isostatic cool pressing is 200Mpa, dwell time 4min.
Biscuit is placed in Muffle furnace in 800 DEG C of biscuiting 5h, residual organic matter is removed；As shown in Fig. 2, by the element after biscuiting
Base is placed in tungsten crucible A1, is embedded according to YAG powders-YAG biscuits-YAG powder modes, wherein covering YAG powders
The thickness ratio of layer 3 and YAG biscuits 4 is 3.0.The bigger tungsten crucible B5 of one bore of back-off above tungsten crucible A1, to prevent powder
It is taken away by mechanical pump or molecular pump, wherein tungsten crucible B5 internal diameters are 1.2 times of tungsten crucible A1 outer diameters.Then it places it in
Vacuum-sintering is carried out in vacuum sintering furnace.Vacuum degree in vacuum sintering furnace is 1.0 × 10-5Pa, vacuum-sintering temperature are 1760
DEG C, sintering time 20h.Due to not embedded using Zirconium powder, lacks in sintering process and provided to YAG biscuits
The oxygen-enriched environment of oxonium ion, therefore, the phenomenon that ceramic surface after vacuum-sintering will produce color burnt hair, needs to take further
Annealing operation.Fig. 4 (a) is the YAG crystalline ceramics samples after vacuum-sintering, it is seen that sample burnt hair phenomenon is very tight after vacuum-sintering
Weight illustrates that ceramics produce serious Lacking oxygen phenomenon after vacuum-sintering, needs further to anneal.
Ceramics after vacuum-sintering are made annealing treatment, annealing temperature is 1450 DEG C, annealing time 10h.After annealing
Potsherd is subjected to Two sides milling and polishing to 1mm, obtains YAG crystalline ceramics.Fig. 4 (b) is the crystalline ceramics sample after polishing, can
Seeing inside crystalline ceramics has a large amount of " mists " to exist, and optical quality is not high.This is because remaining carbon, sulphur in ceramics after vacuum-sintering
Equal impurity will be excluded in annealing process, to generate hole, cause optical quality not high.
Claims (9)
1. a kind of zirconium oxide is sintered the method for preparing YAG crystalline ceramics with YAG powder double-layer embedments, which is characterized in that it includes
Following steps：
1) presoma is prepared：Compound concentration is the yttrium nitrate solution of 0.1~0.3mol/L, and 12 water are added into yttrium nitrate solution
Ammonium aluminum sulfate crystal is closed, is stirred evenly, forms mixed solution, wherein ruthenium ion and aluminum ions molar ratio are 3:5；In stirring shape
The ammonium bicarbonate soln of a concentration of 1.5~2mol/L is pumped in mixed solution with peristaltic pump under state；Monitor reaction system
PH value stops pumping and stirring when pH value reaches 8.0~8.2, by reaction system still aging 12~for 24 hours, after ageing
Presoma is washed, is filtered, is dried successively, obtains precursor powder；
2) it calcines：The precursor powder that step 1) is obtained carries out sieving processing, be put into after sieving in Muffle furnace in 1100~
1300 DEG C of 2~4h of calcining, obtain a nanometer YAG powders；
3) ball milling：The ethyl orthosilicate of 0.4~0.6wt.% is added in the nanometer YAG powders obtained to step 2), adds nothing
Water-ethanol and aluminium oxide abrading-ball carry out ball milling mixing and obtain slurry, sieving processing is carried out after slurry is dried；
4) it is molded：By step 3) be sieved after powder be put into mold, using it is dry pressure formed go out round YAG biscuits, with laggard
The processing of row isostatic cool pressing；
5) it is sintered：The YAG biscuits that step 4) obtains are placed in Muffle furnace and carry out biscuiting, remove residual organic matter；Again by biscuiting
YAG biscuits afterwards are placed in tungsten crucible A (1), according to Zirconium powder-YAG powders-YAG biscuits-YAG powders-zirconium oxide
The arrangement mode of powder is embedded；After embedding, the bigger tungsten crucible B (5) of back-off bore above tungsten crucible A (1), so
After be put into vacuum sintering furnace and carry out vacuum-sintering；
6) grinding and polishing：Potsherd after vacuum-sintering is subjected to Two sides milling and polishing to 1~3mm, obtains YAG crystalline ceramics.
2. a kind of zirconium oxide according to claim 1 prepares the side of YAG crystalline ceramics with the sintering of YAG powder double-layer embedments
Method, which is characterized in that in step (1) when pumping ammonium bicarbonate soln, pump rate is 1~6mL/min, mixing speed 300
~500rpm.
3. a kind of zirconium oxide according to claim 1 or 2 prepares YAG crystalline ceramics with the sintering of YAG powder double-layer embedments
Method, which is characterized in that washing is first to be washed with deionized water 2~4 times, then washed 2~4 times with absolute ethyl alcohol described in step (1)；
The drying temperature is 40~60 DEG C, and drying time is 12~36h.
4. a kind of zirconium oxide according to claim 1 or 2 prepares YAG crystalline ceramics with the sintering of YAG powder double-layer embedments
Method, which is characterized in that sieving is 100~200 mesh using sieve specification in step (2), and sieving number is 3~5 times.
5. a kind of zirconium oxide according to claim 1 or 2 prepares YAG crystalline ceramics with the sintering of YAG powder double-layer embedments
Method, which is characterized in that rotational speed of ball-mill described in step (3) be 160~200rpm, Ball-milling Time be 12~for 24 hours, the drying
Temperature is 40~60 DEG C, and drying time is 12~36h, and the sieve specification is 100~200 mesh, and sieving number is 3~5 times.
6. a kind of zirconium oxide according to claim 1 or 2 prepares YAG crystalline ceramics with the sintering of YAG powder double-layer embedments
Method, which is characterized in that dry-pressing pressure described in step (4) is 25~35MPa, and the dwell time is 1~3min, round YAG elements
A diameter of 16~30mm of base；The pressure of the isostatic cool pressing is 200~240Mpa, and the dwell time is 4~8min.
7. a kind of zirconium oxide according to claim 1 or 2 prepares YAG crystalline ceramics with the sintering of YAG powder double-layer embedments
Method, which is characterized in that biscuiting temperature described in step (5) is 800~900 DEG C, and the biscuiting time is 5~8h；Vacuum sintering furnace
Interior vacuum degree is 1.0 × 10-5~1.0 × 10-3Pa, vacuum-sintering temperature be 1760~1800 DEG C, sintering time be 8~
20h。
8. a kind of zirconium oxide according to claim 1 or 2 prepares YAG crystalline ceramics with the sintering of YAG powder double-layer embedments
Method, which is characterized in that the thickness ratio of Zirconium powder layer (2) and YAG biscuits (4) is 1.0~3.0 when embedding in step (5),
The thickness ratio of YAG powder layers (3) and YAG biscuits (4) is 3.0~4.0.
9. a kind of zirconium oxide according to claim 1 or 2 prepares YAG crystalline ceramics with the sintering of YAG powder double-layer embedments
Method, which is characterized in that the internal diameter of the tungsten crucible B (5) is 1.2~2.0 times of the outer diameter of tungsten crucible A (1).
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