CN108516818A - A method of YAG crystalline ceramics is prepared based on improved Isobam gel rubber systems - Google Patents
A method of YAG crystalline ceramics is prepared based on improved Isobam gel rubber systems Download PDFInfo
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- CN108516818A CN108516818A CN201810516526.3A CN201810516526A CN108516818A CN 108516818 A CN108516818 A CN 108516818A CN 201810516526 A CN201810516526 A CN 201810516526A CN 108516818 A CN108516818 A CN 108516818A
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- 238000000034 method Methods 0.000 title claims abstract description 39
- 229910002106 crystalline ceramic Inorganic materials 0.000 title claims abstract description 35
- 239000011222 crystalline ceramic Substances 0.000 title claims abstract description 35
- 229920001971 elastomer Polymers 0.000 title claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 52
- 238000005245 sintering Methods 0.000 claims abstract description 32
- 235000015895 biscuits Nutrition 0.000 claims abstract description 25
- 239000000919 ceramic Substances 0.000 claims abstract description 25
- 239000002270 dispersing agent Substances 0.000 claims abstract description 24
- 239000011268 mixed slurry Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000498 ball milling Methods 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 238000000137 annealing Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 239000003822 epoxy resin Substances 0.000 claims abstract description 9
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 9
- 238000007711 solidification Methods 0.000 claims abstract description 9
- 230000008023 solidification Effects 0.000 claims abstract description 9
- 238000005266 casting Methods 0.000 claims abstract description 8
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 7
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 238000005498 polishing Methods 0.000 claims abstract description 7
- 238000009849 vacuum degassing Methods 0.000 claims abstract description 6
- 239000003002 pH adjusting agent Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000011805 ball Substances 0.000 claims abstract description 3
- 238000001354 calcination Methods 0.000 claims abstract 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 43
- 238000010792 warming Methods 0.000 claims description 39
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 claims description 38
- 238000010438 heat treatment Methods 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 8
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 6
- 229920002873 Polyethylenimine Polymers 0.000 claims description 6
- 229910052681 coesite Inorganic materials 0.000 claims description 6
- 229910052906 cristobalite Inorganic materials 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 229920002635 polyurethane Polymers 0.000 claims description 6
- 239000004814 polyurethane Substances 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 229910052682 stishovite Inorganic materials 0.000 claims description 6
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 6
- 229910052905 tridymite Inorganic materials 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 claims description 5
- 239000004925 Acrylic resin Substances 0.000 claims description 4
- 229920000178 Acrylic resin Polymers 0.000 claims description 4
- 239000004677 Nylon Substances 0.000 claims description 4
- 229920001778 nylon Polymers 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 239000005011 phenolic resin Substances 0.000 claims description 4
- 229920000058 polyacrylate Polymers 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 239000000908 ammonium hydroxide Substances 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 239000007787 solid Substances 0.000 abstract description 12
- 239000002002 slurry Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000009740 moulding (composite fabrication) Methods 0.000 description 13
- 239000000243 solution Substances 0.000 description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 5
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 4
- 239000010937 tungsten Substances 0.000 description 4
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 235000005979 Citrus limon Nutrition 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003349 gelling agent Substances 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 210000001161 mammalian embryo Anatomy 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 244000248349 Citrus limon Species 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 239000004971 Cross linker Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 239000011954 Ziegler–Natta catalyst Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- MTNDZQHUAFNZQY-UHFFFAOYSA-N imidazoline Chemical compound C1CN=CN1 MTNDZQHUAFNZQY-UHFFFAOYSA-N 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
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Abstract
The invention discloses a kind of methods preparing YAG crystalline ceramics based on improved Isobam gel rubber systems, it includes the following steps：1) abrading-ball, organic solvent, dispersant A, sintering aid, ceramic powder are put into ball grinder, ball milling mixing obtains mixed slurry A；2) mixed slurry A is dry, be sieved, calcining obtains the raw material powder of gel casting forming；3) deionized water, Isobam solution, epoxy resin cross-linking agent, pH adjusting agent, dispersant B, abrading-ball are added in ball grinder, is eventually adding the raw material powder, carries out ball milling mixing again after preliminary stirring, obtains the mixed slurry B of high solids content；4) vacuum degassing, casting, gel drying solidification, dumping；5) by the biscuit vacuum-sintering after dumping, annealing, up to YAG crystalline ceramics after polishing.Method provided by the invention improves the solid content of ceramic slurry, improves the density of biscuit, and the YAG crystalline ceramics transmitances prepared through vacuum-sintering increase substantially, and simple for process, are conducive to industrialized production.
Description
Technical field
The invention belongs to crystalline ceramics preparing technical fields, and in particular to one kind being based on improved Isobam gel rubber system systems
The method of standby YAG crystalline ceramics.
Background technology
Yttrium-aluminium-garnet (abbreviation YAG) has stable cube phase structure, and birefringent phenomenon is not present, and fusing point is high, chemistry
It is good with photochemical stability, it is widely used in laser host gain material, it may also be used for make high temperature visible light and infrared window
Mouthful.Compared with YAG monocrystal, YAG crystalline ceramics, which can meet, to be prepared large scale needed for high power laser and higher mixes
Miscellaneous concentration, therefore YAG almost has the advantages that all of ideal laser host material, is had shown that in terms of replacing YAG monocrystalline good
Good application prospect.The preparation of YAG crystalline ceramics includes prepared by powder, molding, the processes such as sintering and machining.Wherein it is molded work
The purpose of sequence is to obtain high density, dense green that is high uniform and having some strength.
The preparation of YAG crystalline ceramics includes the processes such as powder preparation, molding, sintering and machining.Wherein molding procedure
Purpose is to obtain high density, dense green that is high uniform and having some strength.The control of moulding process link is for entire ceramics
Preparing for material is most important, to improving uniformity, repeatability and the yield rate of material, reduces manufacturing cost etc. all with important
Meaning.Therefore forming method has become a key link in prepared by high-performance ceramic.
Chinese patent application CN107721424A discloses a kind of method that gel casting forming prepares YAG crystalline ceramics.
This method uses Isobam as dispersant and gelling agent, while using Ziegler-Natta catalyst system, ammonium persulfate-
Tetramethylethylenediamine catalyst system and catalyzing and 2, one kind in 2- azos [2- (2- imidazoline -2- bases) propane] hydrochloride catalyst system and catalyzing are come
Gel time is controlled, shortens the gel forming time, prepares the higher YAG crystalline ceramics of transmitance.
However, the gel forming technology is in order to ensure that the preferable mobility of slurry, general solid content are less than at present
70wt.%, inadequate so as to cause biscuit compactness extentization, density is relatively low.Again since the intrinsic property of Isobam gel rubber systems is led
Cause the intensity of biscuit not high, gel time is also longer, influences the efficiency prepared.So the lower solid content of slurry and biscuit compared with
Small density greatly reduces the transmitance of YAG crystalline ceramics, finally influences this forming method in YAG crystalline ceramics
Practical application.
Invention content
The object of the present invention is to provide a kind of method preparing YAG crystalline ceramics based on improved Isobam gel rubber systems,
The solid content of slurry is high, and plain embryo density is big, and ceramic transmitance is high.
To achieve the above object, the present invention adopts the following technical scheme that：
A method of YAG crystalline ceramics being prepared based on improved Isobam gel rubber systems, it includes the following steps：
Step 1: according to Y3Al5O12The stoichiometric ratio of molecular formula weighs nanometer Y respectively2O3Powder, nanometer Al2O3Powder；
Step 2: abrading-ball, organic solvent, dispersant A, sintering aid and load weighted nano oxide powder are put into ball
In grinding jar, mixed slurry A is obtained after carrying out ball milling mixing；
Step 3: taking out the mixed slurry A is dried processing, 100~200 mesh sieve is crossed, the powder after sieving is set
It is calcined in Muffle furnace, the raw material powder as gel casting forming；
Step 4: deionized water, Isobam solution, epoxy resin cross-linking agent, dispersant B, abrading-ball are added in ball grinder,
It is eventually adding the raw material powder, is 9~11 with pH adjusting agent regulation system pH value, ball milling mixing is carried out again after preliminary stirring, obtains
The mixed slurry B that solid content is 76~78%；
Step 5: vacuum degassing, keeps mixed slurry B uniformly still, good fluidity reinjects die for molding；
Step 6: obtaining wet biscuit after gel drying solidification, wet biscuit is dried into back glue；
Step 7: the biscuit after dumping is placed in the sintering of vacuum atmosphere high temperature, annealing, up to the transparent potteries of YAG after polishing
Porcelain.
Preferably, in step 1, the Y2O3The size controlling of powder is in 500~600nm, Al2O3Diameter of particle controls
In 200~600nm, ensure the mixed particle size of powder and rational size distribution, is conducive to prepare stable elements and rationally
The slurry of powder grading.
Preferably, in step 2, the abrading-ball is high purity aluminium oxide abrading-ball, and the abrading-ball and nano oxide powder are total
Mass ratio is 1~3：1, rotational speed of ball-mill is 120r/min~160r/min, and Ball-milling Time is 15~24 hours.
The organic solvent is absolute ethyl alcohol, and the organic solvent is 1 with nano oxide powder total mass ratio：1~
1.5。
The dispersant A is polyethylenimine solution (abbreviation PEI), and the addition of the dispersant A accounts for nano-oxide
The percentage by volume of powder gross mass is 0.1~0.8%.
The sintering aid includes MgO, SiO2, one or more of CaO, the addition of the sintering aid is nanometer
The 0.1~0.5% of oxide powder gross mass；Sintering aid can be used alone or be applied in combination；Wherein, MgO, SiO2Combination
Dosage both when use is respectively the 0.05~0.2% of nano oxide powder gross mass, 0.05~0.3%.
The material of the ball grinder is one kind in nylon, aluminium oxide ceramics, polytetrafluoroethylene (PTFE) or polyurethane.
Preferably, in step 3, the drying temperature is 50~60 DEG C, and drying time is 24~48 hours；It is described to forge
The detailed process of burning is：From room temperature to 700~900 DEG C, heating rate is 2~3 DEG C/min, keeps the temperature 6~8 hours, then
Room temperature~100 DEG C are cooled to, rate of temperature fall is 1~3 DEG C/min.
Preferably, in step 4, the solute of the Isobam solution is in Isobam04, Isobam104, Isobam600
It is one or more, powder solute be completely dissolved in deionized water prepare mass fraction be 15~25% solution.
The epoxy resin cross-linking agent be water soluble phenol resin, water-based acrylic resin, one kind in polyurethane or
A variety of, the addition of epoxy resin cross-linking agent is 1~5 times of the Solute mass of Isobam solution.
The pH adjusting agent is ammonium hydroxide or tetramethylammonium hydroxide.
The dispersant B be one kind in the aqueous-based ceramics dispersant such as ammonium citrate, ammonium polyacrylate, polyethylene glycol or
A variety of, the addition of dispersant B is the 0.1~0.5% of the raw material powder gross mass.
10~30 minutes time tentatively stirred.
The rotational speed of ball-mill is 250~350r/min, and Ball-milling Time is 20~60min.
Preferably, in step 5, vacuum degassed pressure is 1 × 10-3~2 × 10-3Pa, time are 2~10min.
Preferably, in step 6, the cured detailed process of gel drying is：Gel solidification 0.5 at ambient temperature
It after~2 hours, is put into drying oven, 24~72 hours is kept the temperature at a temperature of 25~35 DEG C；It is warming up to 55~80 DEG C again, heat preservation
24~72 hours.
Preferably, in step 6, the detailed process of the dumping is：It is heated up at room temperature with 0.5~2 DEG C/min of rate
To 400~500 DEG C, 4~8 hours are kept the temperature, then 800~900 DEG C are warming up to 0.5~2 DEG C/min, and keeps the temperature 4~8 hours.
Preferably, in step 7, the sintering refers specifically to be sintered under vacuum high-temperature tungsten silk screen stove.
Preferably, in step 7, the detailed process of the sintering is：It is warming up to first by 5~10 DEG C/min at room temperature
200 DEG C, 10~30 minutes are kept the temperature, be secondly warming up to 1000 DEG C by 10~20 DEG C/min and keeps the temperature 10~30 minutes, presses 3 again
~10 DEG C/min be warming up to 1300 DEG C and keep the temperature 1~2 hour, then by 1~5 DEG C/min be warming up to 1780 DEG C and keep the temperature 6~
20 hours, room temperature finally is cooled to 5~10 DEG C/min, vacuum degree is maintained at 1 × 10 in entire sintering process-2~1 × 10- 5Pa。
Preferably, in step 7, the detailed process of the annealing is：It is warming up to first by 2~5 DEG C/min at room temperature
200 DEG C, secondly by 5~15 DEG C/min be warming up to 1200 DEG C, again by 3~10 DEG C/min be warming up to annealing temperature 1400~
1500 DEG C, and 8~12 hours are kept the temperature, finally room temperature is cooled to 5~10 DEG C/min.
Preferably, in step 7, described is finished to two-sided mirror finish.
The present invention uses Isobam as dispersant and gelling agent, while using ammonium citrate, ammonium polyacrylate, poly- second again
The aqueous-based ceramics dispersant such as glycol increases substantially the solid content of ceramic slurry, improves the transmitance of YAG crystalline ceramics.Simultaneously again
Using epoxy resin such as water soluble phenol resin, water-based acrylic resin, polyurethane as cross-linking system, biscuit is significantly increased
Intensity.
Compared with prior art, the present invention has the advantages that：
1, it to improve the solid content and mobility of YAG ceramic slurries in Isobam gel rubber systems, is used in this system
The aqueous-based ceramic dispersant system to work well, is greatly improved the solid content of slurry, the density of biscuit is improved, through true
The YAG crystalline ceramics transmitances that sky sintering is prepared increase substantially, close to theoretical transmission.
2, to be effectively improved the not high problem of biscuit intensity intrinsic in Isobam gel rubber systems, epoxy resin friendship is introduced
Conjuncted system, chemically reacting quintessence's level two-dimentional chain structure in the original gel rubber systems of Isobam is transformed into three-dimensional network knot
Structure is effectively controlled time and the mode of gel solidification, improves gelation efficacy.Ceramics are made after the final dry dumping of demoulding
Biscuit density is big, and intensity is good.
3, aqueous-based ceramic dispersant system and cross linker system provided by the invention solve in Isobam gel rubber systems
The light transmittance of final YAG ceramic products is greatly improved in essential attribute problem, and simple for process, and operability is strong, favorably
Develop to (partly) industrialized production in the Isobam gel formings of YAG transparent ceramic materials.
Description of the drawings
Fig. 1 is the ceramics sample of twin polishing after different shape biscuit and corresponding vacuum-sintering in the embodiment of the present invention 1
Pictorial diagram；
Fig. 2 is the embodiment of the present invention 1 after 1780 DEG C of vacuum-sintering, the transmittance curve in kind of twin polishing to 3mm
Figure.
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
A method of YAG crystalline ceramics being prepared based on improved Isobam gel rubber systems, it includes the following steps：
Step 1: according to Y3Al5O12The stoichiometric ratio of molecular formula weighs high-purity nm Y respectively2O3Powder (average grain diameter
For 500nm) 53.676g, high-purity nm Al2O3Powder (average grain diameter 200nm) 71.324g；
Step 2: by high purity aluminium oxide abrading-ball 375g, absolute ethyl alcohol 156.25ml, dispersant PEI 0.5ml, sintering aid
SiO20.625g is put into togerther with load weighted nano oxide powder in nylon ball grinder, is mixed with the rotating speed of 160r/min
Ball milling obtains mixed slurry A in 15 hours；
It is dried 24 hours Step 3: taking out the mixed slurry A and being placed in 60 DEG C of baking oven, 150 mesh sieve is crossed, after sieving
Powder is placed in Muffle furnace and calcines, and from room temperature to 700 DEG C, heating rate is 2 DEG C/min, keeps the temperature 8 hours, then cools down
To room temperature, rate of temperature fall is 3 DEG C/min, the raw material powder as gel casting forming；
Step 4: the Isobam04 powder produced with Kuraray Corporation is completely dissolved in deionized water and is configured to mass fraction
Additive amount for 20% solution, Isobam04 solution is 3.125g,
Deionized water 36.43ml, Isobam solution, water soluble phenol resin 0.625g, lemon are added in nylon ball grinder
Lemon acid ammonium 0.25g, high purity aluminium oxide abrading-ball 125g, are eventually adding raw material powder 125g, with 25wt% tetramethyl ammonium hydroxide solutions
Regulation system pH is 10, carries out ball milling mixing, rotational speed of ball-mill 350r/min again after preliminary hand operated mixing 10min, and the time is
20min obtains mixed slurry B, and it is 76% to measure its solid content；
Step 5: in the case where vacuum degree is 0.001pa, 10min is steeped in vacuum degassing, uniformly in rear injection Teflon mould
Molding；
Step 6: natural gel solidification is after 0.5 hour at room temperature, gel forming, then wet biscuit is put at 25 DEG C of baking oven
It is 24 hours dry, then 55 DEG C are increased the temperature to, keep the temperature 72 hours.Biscuit dumping first from from room temperature with 0.5 DEG C/min of rate liter
Temperature keeps the temperature 4 hours to 400 DEG C, then is warming up to 800 DEG C with 1 DEG C/min, keeps the temperature 4 hours；
Step 7: the biscuit after dumping is placed in tungsten filament vacuum sintering furnace, 5 DEG C/min of heatings are pressed first at room temperature
To 200 DEG C, 10 minutes are kept the temperature, be secondly warming up to 1000 DEG C by 10 DEG C/min and keeps the temperature 10 minutes, presses 3 DEG C/min of heatings again
To 1300 DEG C and 1 hour is kept the temperature, be then warming up to 1780 DEG C by 1 DEG C/min and keeps the temperature 6 hours, is finally cooled down with 10 DEG C/min
To room temperature, vacuum degree is maintained at 1 × 10 in entire sintering process-2~1 × 10-5Pa；
Sintered ceramics annealing is taken out, 200 DEG C is warming up to by 2 DEG C/min first at room temperature, secondly presses 10 DEG C/min
1200 DEG C are warming up to, 1450 DEG C of annealing temperature is warming up to by 3 DEG C/min again, and keep the temperature 8 hours, is finally dropped with 10 DEG C/min
Temperature arrives room temperature.
YAG crystalline ceramics, twin polishing to 3mm are obtained after two-sided mirror finish.
In Fig. 1 above a row be different mold injections obtain the plain embryo pictorial diagram after dumping of different shapes, below a row
For the ceramics sample pictorial diagram of twin polishing after corresponding vacuum-sintering, it can be clearly seen that the word under ceramics sample covering
It is female.
It is 84.4% (as shown in Figure 2) to measure transmitance of one of ceramics sample at 1064nm wavelength.
Embodiment 2
A method of YAG crystalline ceramics being prepared based on improved Isobam gel rubber systems, it includes the following steps：
Step 1: according to Y3Al5O12The stoichiometric ratio of molecular formula weighs high-purity nm Y respectively2O3Powder (average grain diameter
For 600nm) 34.352g, high-purity nm Al2O3Powder (average grain diameter 600nm) 45.648g；
Step 2: by high purity aluminium oxide abrading-ball 80g, absolute ethyl alcohol 66.67ml, dispersant PEI 0.08ml, sintering aid
SiO20.04g and MgO 0.04g are put into togerther with load weighted nano oxide powder in aluminium oxide ceramics ball grinder, with
The rotating speed mixing and ball milling of 120r/min obtains mixed slurry A in 24 hours；
It dries 48 hours, sieves with 100 mesh sieve, after sieving Step 3: taking out the mixed slurry A and being placed in 50 DEG C of baking oven
Powder is placed in Muffle furnace and calcines, and from room temperature to 800 DEG C, heating rate is 2 DEG C/min, keeps the temperature 6 hours, then cools down
To room temperature, rate of temperature fall is 2 DEG C/min, the raw material powder as gel casting forming；
Step 4: the Isobam600 powder produced with Kuraray Corporation, which is completely dissolved in deionized water, is configured to quality point
Number is 15% solution, and the additive amount of Isobam600 solution is 1.6g,
Deionized water 21.08ml, Isobam solution, water-based acrylic resin are added in aluminium oxide ceramics ball grinder
1.2g, ammonium polyacrylate 0.4g, high purity aluminium oxide abrading-ball 240g, are eventually adding raw material powder 80g, with 25wt% tetramethyl hydroxides
Ammonium salt solution regulation system pH is 9, and ball milling mixing, rotational speed of ball-mill 250r/min, time are carried out again after preliminary hand operated mixing 30min
For 40min, mixed slurry B is obtained, it is 78% to measure its solid content；
Step 5: vacuum degree be 0.002pa under vacuum degassing steep 2min, uniformly after injection Teflon mould at
Type；
Step 6: natural gel solidification is after 2 hours at room temperature, gel forming, then wet biscuit is put at 35 DEG C of baking oven and is done
Dry 72 hours, then 80 DEG C are increased the temperature to, keep the temperature 24 hours；Biscuit dumping is first warming up to from room temperature with 2 DEG C/min of rate
500 DEG C, 8 hours are kept the temperature, then 900 DEG C are warming up to 0.5 DEG C/min, keeps the temperature 8 hours；
Step 7: the biscuit after dumping is placed in tungsten filament vacuum sintering furnace, 10 DEG C/min of heatings are pressed first at room temperature
To 200 DEG C, 30 minutes are kept the temperature, be secondly warming up to 1000 DEG C by 20 DEG C/min and keeps the temperature 30 minutes, is risen again by 10 DEG C/min
Temperature is to 1300 DEG C and keeps the temperature 2 hours, is then warming up to 1780 DEG C by 5 DEG C/min and keeps the temperature 20 hours, is finally dropped with 5 DEG C/min
Temperature arrives room temperature, and vacuum degree is maintained at 1 × 10 in entire sintering process-2~1 × 10-5Pa；
Sintered ceramics annealing is taken out, 200 DEG C is warming up to by 2 DEG C/min first at room temperature, secondly presses 15 DEG C/min
1200 DEG C are warming up to, 1500 DEG C of annealing temperature is warming up to by 10 DEG C/min again, and keep the temperature 12 hours, finally with 5 DEG C/min
Room temperature is cooled to, YAG crystalline ceramics is obtained after then carrying out two-sided mirror finish.
Embodiment 3
A method of YAG crystalline ceramics being prepared based on improved Isobam gel rubber systems, it includes the following steps：
Step 1: according to Y3Al5O12The stoichiometric ratio of molecular formula weighs high-purity nm Y respectively2O3Powder (average grain diameter
For 550nm) 214.703g, high-purity nm Al2O3Powder (average grain diameter 400nm) 285.297g；
Step 2: by high purity aluminium oxide abrading-ball 1200g, absolute ethyl alcohol 604.17ml, dispersant PEI 4ml, sintering aid
SiO21.25g is put into togerther with load weighted nano oxide powder in polytetrafluoroethylene (PTFE) ball grinder, with the rotating speed of 150r/min
Mixing and ball milling obtains mixed slurry A in 20 hours；
It is dried 36 hours Step 3: taking out the mixed slurry A and being placed in 55 DEG C of baking oven, 200 mesh sieve is crossed, after sieving
Powder is placed in Muffle furnace and calcines, and from room temperature to 900 DEG C, heating rate is 3 DEG C/min, keeps the temperature 7 hours, then cools down
To 100 DEG C, rate of temperature fall is 1 DEG C/min, the raw material powder as gel casting forming；
Step 4: with the Isobam104 and Isobam600 in mass ratio 3 of Kuraray Corporation production:2 mixed powders
It being completely dissolved in and is configured to the solution that mass fraction is 25% in deionized water, the additive amount of Isobam mixed solutions is 10g,
Deionized water 145.58ml, Isobam mixed solution is added in polytetrafluoroethylene (PTFE) ball grinder, polyurethane 10g, gathers
Ethylene glycol 2.5g, high purity aluminium oxide abrading-ball 500g, are eventually adding raw material powder 500g, are 11 with ammonia water conditioning system pH, preliminary hand
Ball milling mixing, rotational speed of ball-mill 300r/min are carried out again after dynamic stirring 20min, and time 60min obtains mixed slurry B, measures it
Solid content is 77%；
Step 5: 5min is steeped in vacuum degassing in the case where vacuum degree is 0.015pa, uniformly it is molded in rear injection stainless steel mould；
Step 6: natural gel solidification is after 1 hour at room temperature, gel forming, then wet biscuit is put at 30 DEG C of baking oven and is done
Dry 48 hours, then 70 DEG C are increased the temperature to, keep the temperature 48 hours；Biscuit dumping is first warming up to from room temperature with 1 DEG C/min of rate
450 DEG C, 5 hours are kept the temperature, then 850 DEG C are warming up to 2 DEG C/min, keeps the temperature 6 hours；
Step 7: the biscuit after dumping is placed in tungsten filament vacuum sintering furnace, 5 DEG C/min of heatings are pressed first at room temperature
To 200 DEG C, 20 minutes are kept the temperature, be secondly warming up to 1000 DEG C by 15 DEG C/min and keeps the temperature 20 minutes, presses 5 DEG C/min of heatings again
To 1300 DEG C and 1.5 hours are kept the temperature, be then warming up to 1780 DEG C by 2 DEG C/min and keeps the temperature 10 hours, is finally dropped with 3 DEG C/min
Temperature arrives room temperature, and vacuum degree is maintained at 1 × 10 in entire sintering process-2~1 × 10-5Pa；
Sintered ceramics annealing is taken out, 200 DEG C is warming up to by 5 DEG C/min first at room temperature, secondly presses 10 DEG C/min
1200 DEG C are warming up to, 1400 DEG C of annealing temperature is warming up to by 5 DEG C/min again, and keep the temperature 8 hours, is finally dropped with 8 DEG C/min
Temperature arrives room temperature, then carries out two-sided mirror finish, obtains YAG crystalline ceramics.
Claims (10)
1. a kind of method preparing YAG crystalline ceramics based on improved Isobam gel rubber systems, which is characterized in that it includes following
Step：
Step 1: according to Y3Al5O12The stoichiometric ratio of molecular formula weighs nanometer Y respectively2O3Powder, nanometer Al2O3Powder；
Step 2: abrading-ball, organic solvent, dispersant A, sintering aid and load weighted nano oxide powder are put into ball grinder
In, obtain mixed slurry A after carrying out ball milling mixing；
Step 3: taking out the mixed slurry A is dried processing, 100~200 mesh sieve is crossed, the powder after sieving is placed in horse
It is not calcined in stove, the raw material powder as gel casting forming；
Step 4: deionized water, Isobam solution, epoxy resin cross-linking agent, dispersant B, abrading-ball are added in ball grinder, finally
The raw material powder is added, is 9~11 with pH adjusting agent regulation system pH value, carries out ball milling mixing again after preliminary stirring, obtains and contain admittedly
The mixed slurry B that amount is 76~78%；
Step 5: mixed slurry B vacuum degassings are steeped, it is then injected into die for molding；
Step 6: obtaining wet biscuit after gel drying solidification, wet biscuit is dried into back glue；
Step 7: the biscuit after dumping is placed in the sintering of vacuum atmosphere high temperature, annealing, up to YAG crystalline ceramics after polishing.
2. the method according to claim 1 for preparing YAG crystalline ceramics based on improved Isobam gel rubber systems, feature
It is, in step 1, the Y2O3Diameter of particle is 500~600nm, Al2O3Diameter of particle is 200~600nm.
3. the method according to claim 1 for preparing YAG crystalline ceramics based on improved Isobam gel rubber systems, feature
It is, the abrading-ball is high purity aluminium oxide abrading-ball, and the abrading-ball is 1~3 with nano oxide powder total mass ratio：1, ball milling turns
Speed is 120r/min~160r/min, and Ball-milling Time is 15~24 hours；
The organic solvent is absolute ethyl alcohol, and the organic solvent is 1 with nano oxide powder total mass ratio：1~1.5；
The dispersant A is polyethylenimine solution, and the addition of the dispersant A accounts for the body of nano oxide powder gross mass
Product percentage is 0.1~0.8%；
The sintering aid includes MgO, SiO2, one or more of CaO, the addition of the sintering aid is nano oxidized
The 0.1~0.5% of powder gross mass；
The material of the ball grinder is one kind in nylon, aluminium oxide ceramics, polytetrafluoroethylene (PTFE) or polyurethane.
4. the method according to claim 1 for preparing YAG crystalline ceramics based on improved Isobam gel rubber systems, feature
It is, in step 3, the drying temperature is 50~60 DEG C, and drying time is 24~48 hours；The specific mistake of the calcining
Cheng Wei：From room temperature to 700~900 DEG C, heating rate is 2~3 DEG C/min, keeps the temperature 6~8 hours, then cools to room temperature
~100 DEG C, rate of temperature fall is 1~3 DEG C/min.
5. the method according to claim 1 for preparing YAG crystalline ceramics based on improved Isobam gel rubber systems, feature
It is, in step 4, the solute of the Isobam solution is one kind or more in Isobam04, Isobam104, Isobam600
Kind, the mass fraction of the Isobam solution is 15~25%；
The epoxy resin cross-linking agent is water soluble phenol resin, water-based acrylic resin, one or more in polyurethane,
The addition of epoxy resin cross-linking agent is 1~5 times of the Solute mass of Isobam solution；
The pH adjusting agent is ammonium hydroxide or tetramethylammonium hydroxide；
The dispersant B is one kind or more in the aqueous-based ceramics dispersants such as ammonium citrate, ammonium polyacrylate, polyethylene glycol
Kind, the addition of dispersant B is the 0.2~0.5% of the raw material powder gross mass；
10~30 minutes time tentatively stirred；
The rotational speed of ball-mill is 250~350r/min, and Ball-milling Time is 20~60min.
6. the method according to claim 1 for preparing YAG crystalline ceramics based on improved Isobam gel rubber systems, feature
It is, in step 5, vacuum degassed pressure is 1 × 10-3~2 × 10-3Pa, time are 2~10min.
7. the method according to claim 1 for preparing YAG crystalline ceramics based on improved Isobam gel rubber systems, feature
It is, in step 6, the cured detailed process of gel drying is：Gel solidification is after 0.5~2 hour at ambient temperature,
It is put into drying oven, 24~72 hours is kept the temperature at a temperature of 25~35 DEG C；It is warming up to 55~80 DEG C again, heat preservation 24~72 is small
When.
8. the method according to claim 1 for preparing YAG crystalline ceramics based on improved Isobam gel rubber systems, feature
It is, in step 6, the detailed process of the dumping is：At room temperature 400~500 are warming up to 0.5~2 DEG C/min of rate
DEG C, 4~8 hours are kept the temperature, then 800~900 DEG C are warming up to 0.5~2 DEG C/min, and keep the temperature 4~8 hours.
9. the method according to claim 1 for preparing YAG crystalline ceramics based on improved Isobam gel rubber systems, feature
It is, in step 7, the detailed process of the sintering is：200 DEG C are warming up to by 5~10 DEG C/min first at room temperature, heat preservation
10~30 minutes, secondly 1000 DEG C are warming up to by 10~20 DEG C/min and keep the temperature 10~30 minutes, press 3~10 DEG C/min again
It is warming up to 1300 DEG C and keeps the temperature 1~2 hour, be then warming up to 1780 DEG C by 1~5 DEG C/min and keep the temperature 6~20 hours, finally
Room temperature is cooled to 5~10 DEG C/min, vacuum degree is maintained at 1 × 10 in entire sintering process-2~1 × 10-5Pa。
10. the method according to claim 1 for preparing YAG crystalline ceramics based on improved Isobam gel rubber systems, special
Sign is, in step 7, the detailed process of the annealing is：200 DEG C are warming up to by 2~5 DEG C/min first at room temperature,
It is secondary to be warming up to 1200 DEG C by 5~15 DEG C/min, it is warming up to 1400~1500 DEG C of annealing temperature by 3~10 DEG C/min again, and
Heat preservation 8~12 hours, finally cools to room temperature with 5~10 DEG C/min.
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| CN113149631A (en) * | 2021-01-20 | 2021-07-23 | 江苏师范大学 | Method for preparing YAG transparent ceramic by colloidal state curing molding |
| EP4063337A1 (en) * | 2021-03-26 | 2022-09-28 | Glassomer GmbH | Material and process for fabricating and shaping of transparent ceramics |
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| CN113213934A (en) * | 2021-05-06 | 2021-08-06 | 上海应用技术大学 | Preparation method of assembled luminous oscillation marking line |
| CN113402269A (en) * | 2021-06-29 | 2021-09-17 | 南通大学 | Preparation method of three-color transparent fluorescent ceramic capable of adjusting white light of different degrees |
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| CN114853462A (en) * | 2022-05-16 | 2022-08-05 | 新沂市锡沂高新材料产业技术研究院有限公司 | Method for preparing YAG-based transparent ceramic by direct writing forming |
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