CN102584238A - Method for preparing semitransparent yttrium vanadate ceramic - Google Patents
Method for preparing semitransparent yttrium vanadate ceramic Download PDFInfo
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- CN102584238A CN102584238A CN2012100324815A CN201210032481A CN102584238A CN 102584238 A CN102584238 A CN 102584238A CN 2012100324815 A CN2012100324815 A CN 2012100324815A CN 201210032481 A CN201210032481 A CN 201210032481A CN 102584238 A CN102584238 A CN 102584238A
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Abstract
The invention relates to a method for preparing semitransparent yttrium vanadate ceramic, which belongs to the technical field of preparation of functional ceramics and inorganic materials. Yttrium vanadate polycrystal powder is used as a raw material, and the polycrystal powder, solvent, a dispersing agent and a defoaming agent are mixed by mass ratio and subjected to ball milling for 12-24 hours. A plasticizer and a binder are added into a paste material, and then the ball milling is further performed for 8-16 hours. The knife edge height is fixed in a range of 300-1000 mum, the casting speed and the temperature are adjusted, and the paste material after being subjected vacuum defoaming is placed in a casting machine hopper to be casted and formed. Formed casting sheets are fetched out, and samples are collected. After degreasing in the temperature atmosphere of 600-900 DEG C, the semitransparent yttrium vanadate ceramic is obtained through sintering at the temperature of 1500-1650 DEG C under the protection of oxygen environment. The semitransparent yttrium vanadate ceramic prepared by the method has the advantages of being low in temperature, simple in device, convenient to operate, low in cost and the like.
Description
Technical field
The present invention relates to a kind of preparation method of translucent vanadic acid yttrium pottery, belong to the technical field of function ceramics and inorganic materials preparation.
Background technology
Yttrium vanadate crystal is a kind of monocrystalline of common employing Czochralski grown and since its have good birefringent characteristic and from 400-5000nm very wide see through wave band, the big (21-28GW/cm of light injury value
2), good (the Δ n=10 of optical homogeneity
-6), the advantage that high firmness etc. are outstanding, thereby become the ideal material of making the optical polarization components and parts.At the alternative calcite (CaCO of many application facet
3) and rutile (TiO
2) make that light pricker shield retaining, ring-type mirror, light come displacing device, the device of assigning to, Glan (Glan) polariscope and other polarizer.
At present, yttrium vanadate crystal has been widely used in the communication of light pricker in optoisolator, circulator, beam splitter and the infrared polarizer.In light pricker communication system, every in each light source and the light pricker circuit at a distance from about 1km, need an optoisolator; The light pricker leads to first branch of user, all needs a circulator.And each optoisolator and circulator need two and three yttrium vanadate crystals respectively.According to the market statistics of Lucent, because implementing the communication of light pricker, many developed countries advance the door engineering, light pricker communications market is annual in 10 years of the past increases more than 50%, very huge to the demand of yttrium vanadate crystal.
But up to now; The preparation of yttrium vanadate crystal is only limited to monocrystalline; The domestic and international research emphasis is only in the improvement of single crystal growing technology and the research of new growth method; Like improved CZ growing technology (its volume of can growing is bigger, and quality is crystal preferably), improved float zone growth method, Verneuil method, laser heated pedestal method (LHPG), push up brilliant method (TSSG) etc.Because the single crystal growing technology limitation, high-quality yttrium vanadate crystal growth both at home and abroad rests on the level of little magnitude always, can not satisfy big polarizer and use the demand that goes up the large size gem-quality crystal.Therefore; The preparation research of vanadic acid yttrium pottery not only provides the research thinking of a new yttrium vanadate crystal; With the restriction of breakthrough yttrium vanadate single crystal growing technology, and because pottery has more excellent intensity and toughness than monocrystalline, so the mechanical property of yttrium vanadate crystal can further improve.
Summary of the invention
In order to break through the restriction of yttrium vanadate crystal growing technology, the present invention provides the preparation method of a vanadic acid yttrium pottery.This method sintering temperature is low, and sintering only needs 1500-1650 ℃, and is low for equipment requirements, thereby cost is low; The vanadic acid yttrium pottery of preparation has translucency.
The present invention is realized by following technical scheme:
(1) adopt self-control vanadic acid yttrium polycrystal powder as raw material, polycrystal powder, solvent, dispersion agent, defrother are pressed 1: (0.5-1.5): (0.02-0.10): (0.01-0.05) mass ratio mixes, ball milling 12-24h;
(2) in step (1) gained slurry, add softening agent, sticker, the amount of institute's adding additives is the 2%-8% of powder quality, and plasticising dosage is 0.4-1.0 times of sticker quality, and then ball milling 8-16h;
(3) slurry that step (2) is obtained carries out froth in vacuum, pours into afterwards in the casting machine hopper, carries out flow casting molding: dead knife open height 300-1000 μ m, regulate curtain coating speed 0.20-0.50m/min, drying temperature 30-40 ℃;
(4) take out the curtain coating thin slice, be trimmed to suitable size, collect biscuit;
(5) with biscuit degreasing under atmosphere protection;
(6) carry out atmosphere sintering at last, obtain translucent vanadic acid yttrium pottery.
The object of the present invention is to provide a kind of new vanadic acid yttrium to prepare scheme, the ceramic preparation that is provided can be prepared translucent vanadic acid yttrium polycrystal, thereby can break through the restriction of yttrium vanadate crystal growing technology, widens the research thinking of yttrium vanadate crystal.Ceramic methods is prepared translucent yttrium vanadate crystal, has also carried out successfully attempting for the research of the alternative single crystal technology of vanadic acid yttrium pottery.
With the single crystal growing compared with techniques, the advantage of the inventive method is:
(1) temperature of reaction is low, and sintering temperature only needs 1500-1650 ℃, and the required melt temperature of single crystal growing technology is up to more than 1820 ℃.
(2) low for equipment requirements, major equipment is that a casting machine and retort furnace or box-type furnace or tube furnace get final product, and need not the specific installations such as iridium crucible of the required costliness of single crystal growing.
(3) casting technique is stable, and is repeated and workable, can realize large-scale industrialization production.
(4) prepared vanadic acid yttrium pottery has than the better mechanical property of monocrystalline, and can realize the preparation of large size yttrium vanadate crystal.
(5) than single crystal growing technology obvious reduction is arranged owing to sintering temperature with to equipment requirements, thereby cost descends significantly.
Description of drawings
Below in conjunction with accompanying drawing and embodiment to further explain of the present invention.
Fig. 1,2,3 is respectively the translucent YVO4 photo of embodiment 1, embodiment 2, embodiment 3.
Embodiment
Embodiment 1
Polycrystalline vanadic acid yttrium powder, YLENE, menhaden fish oil, silicone oil were pressed 1: 1: 0.03: 0.01 mass ratio mixes, and ball milling 12h is to even for the first time; In the gained slurry, add PAG, PVB, the PVB amount is 5% of powder quality, and PAG: the PVB mass ratio is 0.6, once more ball milling 12h; After the froth in vacuum, slurry is poured in the casting machine hopper, carried out flow casting molding: dead knife open height 500 μ m, regulate curtain coating speed 0.35m/min, 35 ℃ of curtain coating temperature; After drying, take out the curtain coating thin slice, be trimmed to suitable size, collect biscuit; 800 ℃ of degreasings; Under the oxygen environment protection, through 1570 ℃ of sintering, behind the insulation 10h, obtain translucent vanadic acid yttrium pottery, as shown in Figure 1.
Embodiment 2
Polycrystalline vanadic acid yttrium powder, YLENE, menhaden fish oil, silicone oil were pressed 1: 1.5: 0.03: 0.01 mass ratio mixes, and ball milling 12h is to even for the first time; In the gained slurry, add BBP, PVB, the PVB amount is 4% of powder quality, and PAG: the PVB mass ratio is 0.8, once more ball milling 12h; After the froth in vacuum, slurry is poured in the casting machine hopper, carried out flow casting molding: dead knife open height 400 μ m, regulate curtain coating speed 0.35m/min, 35 ℃ of curtain coating temperature; After drying, take out the curtain coating thin slice, be trimmed to suitable size, collect biscuit; 800 ℃ of degreasings; Under the oxygen environment protection,, behind the insulation 10h, obtain translucent vanadic acid yttrium pottery again through 1580 ℃ of sintering, as shown in Figure 2.
Embodiment 3
Polycrystalline vanadic acid yttrium powder, YLENE, menhaden fish oil, silicone oil were pressed 1: 1.5: 0.03: 0.01 mass ratio mixes, and ball milling 24h is to even for the first time; PAG+BBP, the PVB amount that in the gained slurry, adds is 4% of powder quality, and PAG+BBP: the PVB mass ratio is 0.8, once more ball milling 12h; After the froth in vacuum, slurry is poured in the casting machine hopper, carried out flow casting molding: dead knife open height 800 μ m, regulate curtain coating speed 0.40m/min, 35 ℃ of curtain coating temperature; After drying, take out the curtain coating thin slice, be trimmed to suitable size, collect biscuit; 800 ℃ of degreasings; Under the protection of bad border of hypoxemia,, behind the insulation 10h, obtain translucent vanadic acid yttrium pottery again through 1550 ℃ of sintering, as shown in Figure 3.
Claims (10)
1. the preparation method of a translucent vanadic acid yttrium pottery comprises the steps:
(1) adopting self-control vanadic acid yttrium polycrystal powder is raw material, and polycrystal powder, solvent, dispersion agent, defrother are pressed 1: (0.5-1.5): (0.02-0.10): (0.01-0.05) mass ratio mixes, ball milling 12-24h;
(2) in step (1) gained slurry, add softening agent, sticker, the amount of institute's adding additives is the 2%-8% of powder quality, and plasticising dosage is 0.4-1.0 times of sticker quality, and then ball milling 8-16h;
(3) slurry that step (2) is obtained carries out froth in vacuum, pours into afterwards in the casting machine hopper, carries out flow casting molding: dead knife open height 300-1000 μ m, regulate curtain coating speed 0.20-0.50m/min, drying temperature 30-40 ℃;
(4) take out the curtain coating thin slice, be trimmed to suitable size, collect biscuit;
(5) with biscuit degreasing under atmosphere protection;
(6) carry out atmosphere sintering at last, obtain translucent vanadic acid yttrium pottery.
2. the preparation method of vanadic acid yttrium according to claim 1 pottery is characterized in that: the solvent of said step (1) is that a kind of in ethanol, methyl ethyl ketone, butanols, zellon, methyl ethyl ketone, toluene and the YLENE etc. or several use simultaneously.
3. the preparation method of vanadic acid yttrium according to claim 1 pottery is characterized in that: the dispersion agent of said step (1) is gum arabic, CMC 99.5, menhaden fish oil, gather a kind of in (methyl) vinylformic acid (salt), polymine, polyacrylate, sodium acrylate, methylacrylic acid, MALEIC ANHYDRIDE, sulfonated lignin, sulfamate, polycarboxylate, poly carboxylic acid multipolymer, poly carboxylic acid sodium, melamine sulfonate, formaldehyde, ethanol, the USP Kosher etc. or several use simultaneously.
4. the preparation method of vanadic acid yttrium pottery according to claim 1, it is characterized in that: the defrother of said step (1) is tributyl phosphate, organosilicon wet goods.
5. the preparation method of vanadic acid yttrium according to claim 1 pottery is characterized in that: the softening agent of said step (2) is that a kind of in dimethyl phthalate, phthalic ester, polyoxyethylene glycol, polyoxyethylene and the polyoxypropylene copolymer etc. or several use simultaneously.
6. the preparation method of vanadic acid yttrium according to claim 1 pottery is characterized in that: the sticker of said step (2) is that a kind of in Z 150PH, PVA, Vinylpyrrolidone polymer, polyvinyl butyral acetal, gelatin, the alginic acid salt glacier or several use simultaneously.
7. the preparation method of vanadic acid yttrium pottery according to claim 1, it is characterized in that: the ball milling of said step (1) and step (2) need reach rotating speed 180-260rpm, and the ball milling envrionment temperature is controlled at 20-25 ℃.
8. the preparation method of vanadic acid yttrium according to claim 1 pottery is characterized in that: the froth in vacuum of said step (3) needs in the sealing stirred pot, carry out, and vacuum tightness is-and below the 0.1Mpa, stirring velocity is 60-120 rev/min, and the de-bubble time is more than 20 minutes.
9. the preparation method of vanadic acid yttrium pottery according to claim 1; It is characterized in that: the degreasing process of said step (5) is raised to organism decomposition temperature point with 0.5～5 ℃/min temperature rise rate under atmosphere protection; Be incubated 1～100 hour, treat that organism decomposes fully, cools to room temperature naturally; Oxygen flow is PM 50～100ml, and wherein protective atmosphere uses oxygen or rare gas element.
10. the preparation method of vanadic acid yttrium pottery according to claim 1; It is characterized in that: the sintering of said step (6) carries out under oxygen atmosphere, with the reduction that the prevents vanadium volatilization of appraising at the current rate, sintering range 1500-1650 ℃; Size per sample, sintering time is 0.5～100 hour.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105185429A (en) * | 2015-08-07 | 2015-12-23 | 昆明贵信凯科技有限公司 | Packaging medium slurry for base-metal-contained electronic slurry and application thereof |
| CN109354496A (en) * | 2018-10-18 | 2019-02-19 | 九江学院 | A kind of preparation method of Yttrium Orthovanadate crystalline ceramics |
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| CN101698602A (en) * | 2009-11-04 | 2010-04-28 | 中国科学院上海硅酸盐研究所 | Preparation method of yttria-base transparent ceramics with designable component and structure |
| CN101855187A (en) * | 2007-09-14 | 2010-10-06 | 宾夕法尼亚州立大学研究基金会 | The manufacture method of crystalline ceramics |
| CN102060540A (en) * | 2009-11-16 | 2011-05-18 | 中国科学院福建物质结构研究所 | Method for preparing Re:YAG polycrystalline transparent ceramic by using different molding modes |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101855187A (en) * | 2007-09-14 | 2010-10-06 | 宾夕法尼亚州立大学研究基金会 | The manufacture method of crystalline ceramics |
| CN101698602A (en) * | 2009-11-04 | 2010-04-28 | 中国科学院上海硅酸盐研究所 | Preparation method of yttria-base transparent ceramics with designable component and structure |
| CN102060540A (en) * | 2009-11-16 | 2011-05-18 | 中国科学院福建物质结构研究所 | Method for preparing Re:YAG polycrystalline transparent ceramic by using different molding modes |
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| Title |
|---|
| 李建利 等: "钒酸钇晶体多晶原料的合成研究", 《长春理工大学学报》, vol. 26, no. 4, 31 December 2003 (2003-12-31), pages 64 - 66 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105185429A (en) * | 2015-08-07 | 2015-12-23 | 昆明贵信凯科技有限公司 | Packaging medium slurry for base-metal-contained electronic slurry and application thereof |
| CN109354496A (en) * | 2018-10-18 | 2019-02-19 | 九江学院 | A kind of preparation method of Yttrium Orthovanadate crystalline ceramics |
| CN109354496B (en) * | 2018-10-18 | 2021-06-11 | 九江学院 | Preparation method of yttrium vanadate transparent ceramic |
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