CN102584238B - Method for preparing semitransparent yttrium vanadate ceramic - Google Patents
Method for preparing semitransparent yttrium vanadate ceramic Download PDFInfo
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- CN102584238B CN102584238B CN201210032481.5A CN201210032481A CN102584238B CN 102584238 B CN102584238 B CN 102584238B CN 201210032481 A CN201210032481 A CN 201210032481A CN 102584238 B CN102584238 B CN 102584238B
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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 semitransparent yttrium vanadate ceramic, belong to technical field prepared by function ceramics and inorganic materials.
Background technology
Yttrium vanadate crystal is a kind of monocrystalline of common employing Czochralski grown, due to its have good birefringent characteristic and from 400-5000nm very wide see through the large (21-28GW/cm of wave band, light injury value
2), good (the Δ n=10 of optical homogeneity
-6), the advantage that high rigidity etc. are outstanding, thereby become the ideal material of making optical polarization components and parts.At the alternative calcite (CaCO of many application aspect
3) and rutile (TiO
2) make that light pricker shield retaining, ring-type mirror, light carry out 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 infrared polarizer.In light pricker communication system, in each light source and light pricker circuit, every about 1km, need an optoisolator; Light pricker leads to first branch of user, all needs a circulator.And each optoisolator and circulator need respectively two and three yttrium vanadate crystals.According to the market statistics of Lucent, because implementing the communication of light pricker, many developed countries enter door engineering, and in 10 years of the past, light pricker communications market increases more than 50% every year, very huge to the demand of yttrium vanadate crystal.
But up to now, the preparation of yttrium vanadate crystal is only limited to monocrystalline, research emphasis both domestic and external is only in the improvement of Crystal Growth Technique and the research of new growth method, as improved CZ growing technology (its volume of can growing is larger, the good crystal of quality), improved float zone growth method, Verneuil method, laser heated pedestal method (LHPG), push up brilliant method (TSSG) etc.Due to the restriction of Crystal Growth Technique, high-quality yttrium vanadate crystal growth both at home and abroad rests on the level of little magnitude always, can not meet the upper demand to large size gem-quality crystal of larger polarizer application.Therefore, the preparation research of yttrium vanadate ceramic not only provides the Research Thinking of a new yttrium vanadate crystal, to break through the restriction of yttrium vanadate single crystal growing technology, and because pottery has more excellent intensity and toughness than monocrystalline, therefore 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 invention provides the preparation method of a yttrium vanadate ceramic.The method sintering temperature is low, and sintering only needs 1500-1650 DEG C, low for equipment requirements, thereby cost is low; The yttrium vanadate ceramic of preparation has translucency.
The present invention is realized by following technical scheme:
(1) adopt self-control Yttrium Orthovanadate polycrystal powder as raw material, polycrystal powder, solvent, dispersion agent, defrother are pressed to 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, binding agent, the 2%-8% that the amount of institute's adding additives is powder quality, plasticising dosage is 0.4-1.0 times of binding agent quality, and then ball milling 8-16h;
(3) slurry step (2) being obtained carries out froth in vacuum, pours into afterwards in casting machine hopper, carries out flow casting molding: dead knife open height 300-1000 μ m, regulates curtain coating speed 0.20-0.50m/min, drying temperature 30-40 DEG C;
(4) take out curtain coating thin slice, be trimmed to suitable size, collect biscuit;
(5) by biscuit degreasing under atmosphere protection;
(6) finally carry out atmosphere sintering, obtain semitransparent yttrium vanadate ceramic.
The object of the present invention is to provide a kind of new Yttrium Orthovanadate to prepare scheme, the ceramic preparation providing can be prepared semitransparent yttrium vanadate 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 semitransparent yttrium vanadate crystal, also for the research of the alternative single crystal technology of yttrium vanadate ceramic has been carried out successfully attempting.
Compared with Crystal Growth Technique, the advantage of the inventive method is:
(1) temperature of reaction is low, and sintering temperature only needs 1500-1650 DEG C, and the required melt temperature of Crystal Growth Technique is up to more than 1820 DEG C.
(2) low for equipment requirements, major equipment is a casting machine and retort furnace or box-type furnace or tube furnace, without specific installations such as the iridium crucibles of the required costliness of single crystal growing.
(3) casting technique is stable, repeated and workable, can realize large-scale industrialization and produce.
(4) prepared yttrium vanadate ceramic has than the better mechanical property of monocrystalline, and can realize the preparation of large size yttrium vanadate crystal.
(5) have obvious reduction due to sintering temperature with to equipment requirements than Crystal Growth Technique, thereby cost significantly declines.
Brief description of the drawings
Below in conjunction with drawings and Examples, the present invention is described in more detail.
Fig. 1,2,3 is respectively the translucent YVO4 photo of embodiment 1, embodiment 2, embodiment 3.
Embodiment
Embodiment 1
Polycrystalline Yttrium Orthovanadate powder, dimethylbenzene, menhaden fish oil, silicone oil are pressed 1: 1: 0.03: 0.01 mass ratio mixes, ball milling 12h is to even for the first time; In gained slurry, add PAG, PVB, PVB amount is 5% of powder quality, PAG: PVB mass ratio is 0.6, again ball milling 12h; After froth in vacuum, slurry is poured in casting machine hopper, carried out flow casting molding: dead knife open height 500 μ m, regulate curtain coating speed 0.35m/min, 35 DEG C of curtain coating temperature; After drying, take out curtain coating thin slice, be trimmed to suitable size, collect biscuit; 800 DEG C of degreasings; Under oxygen environment protection, through 1570 DEG C of sintering, after insulation 10h, obtain semitransparent yttrium vanadate ceramic, as shown in Figure 1.
Embodiment 2
Polycrystalline Yttrium Orthovanadate powder, dimethylbenzene, menhaden fish oil, silicone oil are pressed 1: 1.5: 0.03: 0.01 mass ratio mixes, ball milling 12h is to even for the first time; In gained slurry, add BBP, PVB, PVB amount is 4% of powder quality, PAG: PVB mass ratio is 0.8, again ball milling 12h; After froth in vacuum, slurry is poured in casting machine hopper, carried out flow casting molding: dead knife open height 400 μ m, regulate curtain coating speed 0.35m/min, 35 DEG C of curtain coating temperature; After drying, take out curtain coating thin slice, be trimmed to suitable size, collect biscuit; 800 DEG C of degreasings; Under oxygen environment protection, through 1580 DEG C of sintering, after insulation 10h, obtain semitransparent yttrium vanadate ceramic, as shown in Figure 2 again.
Embodiment 3
Polycrystalline Yttrium Orthovanadate powder, dimethylbenzene, menhaden fish oil, silicone oil are pressed 1: 1.5: 0.03: 0.01 mass ratio mixes, ball milling 24h is to even for the first time; In gained slurry, add PAG+BBP, PVB amount for 4% of powder quality, PAG+BBP: PVB mass ratio is 0.8, again ball milling 12h; After froth in vacuum, slurry is poured in casting machine hopper, carried out flow casting molding: dead knife open height 800 μ m, regulate curtain coating speed 0.40m/min, 35 DEG C of curtain coating temperature; After drying, take out curtain coating thin slice, be trimmed to suitable size, collect biscuit; 800 DEG C of degreasings; Under the protection of bad border of hypoxemia, through 1550 DEG C of sintering, after insulation 10h, obtain semitransparent yttrium vanadate ceramic, as shown in Figure 3 again.
Claims (5)
1. a preparation method for semitransparent yttrium vanadate ceramic, comprises the steps:
(1) adopting self-control Yttrium Orthovanadate polycrystal powder is raw material, polycrystal powder, solvent, dispersion agent, defrother are pressed to 1:(0.5-1.5): (0.02-0.10): (0.01-0.05) mass ratio mixes, ball milling 12-24h; Described solvent is that one or several in ethanol, methyl ethyl ketone, butanols, zellon, toluene and dimethylbenzene are used simultaneously; Described dispersion agent is that one or several in gum arabic, carboxymethyl cellulose, menhaden fish oil, poly-(methyl) vinylformic acid, poly-(methyl) acrylate, polymine, sodium acrylate, methacrylic acid, MALEIC ANHYDRIDE, sulfonated lignin, sulfamate, polycarboxylate, poly carboxylic acid multipolymer, poly carboxylic acid sodium, melamine sulfonate, formaldehyde, ethanol, glycerol are used simultaneously; Described defrother is tributyl phosphate, organic silicone oil;
(2) in step (1) gained slurry, add softening agent, binding agent, the 2%-8% that the amount of institute's adding additives is powder quality, plasticising dosage is 0.4-1.0 times of binding agent quality, and then ball milling 8-16h; Described softening agent is that one or several in dimethyl phthalate, polyoxyethylene glycol, polyoxyethylene and polyoxypropylene copolymer are used simultaneously; Described binding agent is that one or several in polyvinyl alcohol, polyvinyl acetate (PVA), polyvinylpyrrolidone, polyvinyl butyral acetal, gelatin are used simultaneously;
(3) slurry step (2) being obtained carries out froth in vacuum, pours into afterwards in casting machine hopper, carries out flow casting molding: dead knife open height 300-1000 μ m, regulates curtain coating speed 0.20-0.50m/min, drying temperature 30-40 DEG C;
(4) take out curtain coating thin slice, be trimmed to suitable size, collect biscuit;
(5) by biscuit degreasing under atmosphere protection;
(6) finally under oxygen atmosphere, carry out sintering, acquisition semitransparent yttrium vanadate ceramic in 1500-1650 DEG C.
2. the preparation method of yttrium vanadate ceramic according to claim 1, is characterized in that: the ball milling of described step (1) and step (2) need reach rotating speed 180-260rpm, and ball milling envrionment temperature is controlled at 20-25 DEG C.
3. the preparation method of yttrium vanadate ceramic according to claim 1, it is characterized in that: the froth in vacuum of described step (3) need be carried out in sealing stirred pot, vacuum tightness is-and below 0.1Mpa, stirring velocity is 60-120 rev/min, and the de-bubble time is more than 20 minutes.
4. the preparation method of yttrium vanadate ceramic according to claim 1; it is characterized in that: the degreasing process of described step (5) is raised to organic substance decomposing temperature spot with 0.5～5 DEG C/min temperature rise rate under atmosphere protection; be incubated 1～100 hour; treat that organic substance decomposing is complete; naturally cool to room temperature; oxygen flow is per minute 50～100ml, and wherein protective atmosphere uses oxygen or rare gas element.
5. the preparation method of yttrium vanadate ceramic according to claim 1, is characterized in that: the sintering time of described step (6) is 0.5～100 hour.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (2)
| 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》.2003,第26卷(第4期),第64-66页. |
| 钒酸钇晶体多晶原料的合成研究;李建利 等;《长春理工大学学报》;20031231;第26卷(第4期);第64-66页 * |
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