CN103102156A - Re:YAG transparent ceramic prepared through gel casting molding - Google Patents

Re:YAG transparent ceramic prepared through gel casting molding Download PDF

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Publication number
CN103102156A
CN103102156A CN201110353652XA CN201110353652A CN103102156A CN 103102156 A CN103102156 A CN 103102156A CN 201110353652X A CN201110353652X A CN 201110353652XA CN 201110353652 A CN201110353652 A CN 201110353652A CN 103102156 A CN103102156 A CN 103102156A
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gel casting
yag
sintering
green compact
prepare
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曹永革
郭旺
黄秋凤
唐飞
费斌杰
陈剑
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Fujian Institute of Research on the Structure of Matter of CAS
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Fujian Institute of Research on the Structure of Matter of CAS
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Abstract

The invention provides a method for preparing a Re:YAG polycrystal transparent ceramic through a gel casting molding technology, and belongs to the technical field of special optical ceramic manufacturing processes. The method comprises: after vacuum defoaming, casting into a mold to initiate a monomer polymerization reaction at a temperature of 50-100 DEG C; after green compact molding, carrying out green compact drying in stages from a room temperature to a temperature of 200 DEG C, discharging the glue under an oxygen atmosphere, and placing the glue-discharged green compact in a vacuum furnace to sinter to obtain a transparent polycrystal Nd:YAG ceramic sample, wherein a sintering temperature is 1500-1900 DEG C, and a sintering time is 5-120 h; and carrying out annealing on the obtained transparent polycrystal Nd:YAG ceramic sample for 10 h under an oxygen atmosphere with a temperature of 1500 DEG C, and carrying out double-sided polishing to achieve a thickness of 2 mm, wherein measurement results of an ultraviolet visible near infrared spectroscopy photometer are that: transmissivity at a wavelength of 400 nm is 80.6%, and transmissivity at a wavelength of 1064 nm is 83.6%.

Description

Gel casting forming prepares the Re:YAG crystalline ceramics
Technical field
The invention provides a kind of Re:YAG of preparation polycrystalline transparent ceramic forming method, belong to special optical forming process of ceramics and manufacturing process technology field.
Background technology
The Mark.A.Janny of initial stage nineties U.S.'s Oak Ridge National Laboratory and professor O.Omattete have invented gel-casting method [1-3], and this is the forming technique of a kind of novelty, near net-shape pottery.Its forming principle is different from the traditional injection forming that relies on the plaster mould midge, but forms macromolecular network structure or ceramic particle network structure by the chemical reaction of slurry inside, thereby make the ceramic size rapid solidification injected in mould, is ceramic body.Gel casting forming is divided into aqueous gel injection molding and non-aqueous solution gel injection.The former is a kind of current application molding mode more widely, and the latter mainly is applicable to the system of those and water generation chemical reaction.Gel injection molding and forming technology has been widely used since being disclosed, and gel injection technique has been used to moulding from single-phase to complex phase ceramic, shape from the bulk to the tubulose, the ceramic green sheet of the shape such as perforate, piston, blade.Wherein single component has Al usually 2o 3, ZrO 2, SiC, Si 3n 4, TiO 2deng; With the matrix material of gel casting forming, ZrO is arranged 2-Al 2o 3complex phase ceramic, fiber reinforcement reaction reinforcement sintering Si 3n 4matrix material, laminated ceramic composite, and be used for preparing nano heterogeneous ceramic etc. [4], but do not met the report that adopts gel casting forming to prepare the Re:YAG crystalline ceramics.The invention provides a kind of method of utilizing gel casting forming to prepare the Re:YAG ceramic body, adopt a certain amount of organic monomer and linking agent, both are dissolved in the water and the ceramic powder ball milling mixes 20～40 hours, add afterwards a certain amount of initiator and facilitate agent, directly inject the mould of definite shape after froth in vacuum, put into 50～100 ℃ of baking oven initiation reactions and be frozen into base substrate.This molding mode is because gelinite is the network macromolecular structure, ceramic particle is cured in network molecular structure, solute in drying process in solvent can not move with the displacement of solvent, gained base sheet composition and structure have very evenly been avoided the density gradient as injection forming, dry-pressing formed generation, be very beneficial for pore eliminating in base substrate in the vacuum sintering process, obtain high transparent, whole inhomogeneity good ceramic body.Slurry injects different mould structures can obtain difform ceramic body, for example ceramic rod, vitrified pipe, ceramic plate and other different in nature ceramic components.
The present invention prepares YAG powder [number of patent application 200910112279.1] or commercial oxide powder is raw material certainly, adopts gel casting forming to prepare high-quality ceramic body, through vacuum sintering, prepares high transparent Re:YAG pottery, domestic genus reported first.
[1]MARK?A?JANNEY，OGBEMI?O?OMETETE.Gelcasting?of?ceramic?powders[P].U.S.Patent：5145908，1992209208.
[2]OMETETE?O?O，MARK?A?JANNEY，STREHLOW?R?A.Gelcasting?a?new?ceramic?forming?process[J].Ceram.Bull，1991，70(10)：1641.
[3]MARK?A?JANNEY.Method?for?molding?ceramic?powders[P].U.S.Patent：4894194，1990202216.
[4] Tong Jianfeng, Chen great Ming, Li Baowei, Liu Xiaoguang, the structure of gel injection alumina-ceramic base substrate and sign [J]. aeronautical material journal, 2004,24 (6): 42-46.
Summary of the invention
The objective of the invention is to utilize the gel casting forming mode to prepare the Re:YAG polycrystalline transparent ceramic in conjunction with vacuum sintering, the method is characterized in that technical process is followed successively by: the preparation of Re:YAG ceramic size, froth in vacuum, moulding, the demoulding, drying, binder removal, burn till.Specifically be implemented as follows step:
(1) according to Nd xy 3-xal 5o 12the commercially available high-purity Y of stoichiometric ratio weighing of (x is the material molar weight that part Nd atom replaces the Y atom, x=0～0.1) molecular formula 2o 3powder 0.0297～0.0288mol, Al 2o 3powder 0.025mol, Nd 2o 3powder 0.0003～0012mol or homemade Nd:YAG powder.Except Nd 2o 3beyond the powder doping, can also add all other rare earth oxides, or rare earth oxide codoped or single doping.For example: Yb 2o 3, Cr 2o 3, Er 2o 3, Ce 2o 3, Tm 2o 3, Sm 2o 3, Eu 2o 3deng rare earth oxide;
(2) sintering aid adopts commercially available high-purity MgO, CaO, wherein one or several of TEOS sintering agent.0～2at% of mole amount that the addition of sintering aid MgO is mixed oxide, 0～2wt% that the TEOS addition is mixed oxide weight;
(3) the ball milling liquid medium is comprised of deionized water system or pure system or water and pure mixed system, and the solid load 30～60wt% of slurry, regulate the pH value of slurry between 7～12;
(4) add a certain amount of and organic monomer, linking agent, softening agent and defrother ratio, mixing and ball milling ball milling mixed powder 0.5～150 hour; 0.2～3wt%, organic monomer addition that the dispersion agent addition is powder weight (following all take powder weight as standard) are 5～35wt%, and organic monomer and linking agent ratio are between 1: 5～1: 50, the softening agent addition is that 0.5～5wt%, defrother addition are 0.1～5wt%;
(5) by adding 0.1～1wt% initiator after the mixed slurry froth in vacuum, add 0.01～1wt% and facilitate agent, inject the mould of definite shape, put into the baking oven trigger monomer reaction of 50～100 ℃, wait the slurry original position to solidify base substrate and separate with mould, the demoulding.
(6) after the green compact moulding, from room temperature to 200 dried ℃ stage by stage, in order to prevent green compact distortion, cracking, 30 ℃ of initial setting temperature, humidity 90%, slowly increasing temperature, to reduce humidity dry stage by stage;
(7) give birth to biscuit after moulding and put into the alumina crucible tube furnace of packing into, heat up at a slow speed (0.1～10 ℃/min) to the organic substance decomposing temperature spot (200～1300 ℃) added, insulation for some time (size per sample determines soaking time length), carry out degreasing;
(8) green compact after binder removal are put into vacuum oven, carry out sintering under vacuum atmosphere, 1500 ℃～1900 ℃ of sintering ranges, and sintering time is 5～120 hours (size per sample).
The accompanying drawing explanation
Fig. 1 is 1830 ℃ of XRD crystal phase analysis that are incubated 20 hours ceramics samples after sintering, and the diffraction peak in figure, all corresponding to a cube YAG crystalline phase, does not have intermediate transisting phase YAP, YAM to occur as seen from the figure, has shown that the oxide compound in the raw material reacts completely.
Fig. 2 (a) is the dried pole green compact of Nd:YAG gel injection, is (b) photo in kind (sample size Φ 6.0mm * L48mm) of 1830 ℃ of sintering ceramic rod after 20 hours.(c) be YAG powder gel injection green compact at 10 hours ceramics samples of 1780 ℃ of sintering, the diagram sample 1450 ℃ annealing twin polishings in 10 hours.
The straight line transmittance curve that Fig. 3 is Fig. 2 (c) ceramics sample, at 400nm wavelength place, transmitance is 80.6%, in the transmitance of 1064nm wavelength, reaches 83.6%
Embodiment
Embodiment 1
(9) by the commercially available high-purity powder of stoichiometric ratio weighing: Y 2o 3: 10.0600g, Al 2o 3: 7.6470g, Nd 2o 3: 0.1516g (doping of 1at%Nd), add the MgO sintering aid of 0.5at%, the 0.5wt% dispersion agent gathers volatile salt, 15wt% Methacrylamide (MAM) organic monomer, 1: 20 times of (organic monomer: linking agent) N, N '-methylene-bisacrylamide (MBAM), 0.8wt% softening agent polyvinyl alcohol (PEG), 0.5wt% defrother propyl carbinol; Raw material, abrading-ball, additive are poured into to 36 gram deionized water ball millings and mix 24 hours, rotational speed of ball-mill 350r/m, material: ball=1: 5.The mixed slurry interpolation 0.5wt% initiator ammonium persulfate (APS) of ball milling and 0.1wt% catalyzer Tetramethyl Ethylene Diamine (TEMED) are put into to vacuum tank, vacuum-treat to vacuum tightness reaches-below 0.1Mpa, till not having bubble to overflow in slurry.Slurry after de-bubble injects the cylindrical plastic mould, puts into 60 ℃ of baking oven trigger monomer reactions, waits the slurry original position to solidify base substrate and separates with mould, the demoulding.The green compact of moulding are ℃ stage by stage dry from room temperature to 100, and 30 ℃ of initial setting temperature, humidity 90% slowly increase temperature and reduces humidity and slowly be raised to 100 ℃.Dried green compact are put into tube furnace and be warmed up to 700 ℃ with 1 ℃/min temperature rise rate under oxygen atmospheres, are incubated 2 hours, and oxygen flow is per minute 50～100ml, after insulation finishes with the stove naturally cooling.Green compact after degreasing are put into vacuum oven, (vacuum tightness 1.5 * 10 under vacuum atmosphere -4pa) carry out sintering, be raised to 1200 ℃ with 10 ℃/min temperature rise rate, then with 5 ℃/min temperature rise rate be warming up to 1830 ℃ and 1830 ℃ the insulation 20 hours, drop to 1200 ℃ with 5 ℃/min rate of temperature fall, naturally cool to room temperature, obtain transparent Nd:YAG ceramic rod.What X-ray diffraction analysis XRD figure spectrum recorded this ceramics sample is pure YAG phase mutually, do not have intermediate transisting phase YAP, YAM to occur, shown that the oxide compound in the raw material reacts completely as figure (1), figure (2) a is unsintered green compact, and b is unpolished crystalline ceramics rod after sintering.
Embodiment 2
Weighing 20.0000g 2at%Nd:YAG powder, add the TEOS sintering aid of 0.5wt%, add 0.5wt% dispersion agent ammonium polyacrylate (NH4PAA), 10wt% acrylamide (AM) organic monomer, 1: 10 times of (organic monomer: linking agent) N, N '-methylene-bisacrylamide (MBAM), 1.5wt% fluidizer polyoxyethylene glycol (PEG), 0.5wt% defrother isooctyl alcohol, organic additive is added in 30 gram deionized waters, add ammoniacal liquor and regulate PH=9, raw material and deionized water mixing and ball milling, rotational speed of ball-mill 350r/m, material: ball=1: 5, the mixed slurry of ball milling is added to 0.2wt% initiator hydrogen peroxide (H 2o 2) and 0.05wt% catalyzer Tetramethyl Ethylene Diamine (TEMED) put into vacuum tank, vacuum-treat to vacuum tightness reaches-below 0.1Mpa, till not having bubble to overflow in slurry.In slurry implantation glass mould after de-bubble, put into 80 ℃ of baking oven trigger monomer reactions, wait the slurry original position to solidify base substrate and separate with mould, the demoulding.Dried green compact are put into tube furnace, and from room temperature to 500 ℃ with 2 ℃/min temperature rise rate, 500 ℃～800 ℃ with 1 ℃/min temperature rise rate, and in 800 ℃ of insulations degreasing in 10 hours, other process is identical with embodiment 1.The transparent polycrystalline Nd:YAG ceramics sample obtained is annealed 10 hours under 1500 ℃ of oxygen atmospheres, twin polishing is thick in Fig. 2 (c) to 2mm, by the UV, visible light near infrared spectrometer, recording in 400nm wavelength place transmitance is 80.6%, in the transmitance of 1064nm wavelength, reaches 83.6% as figure (3).

Claims (10)

1. gel casting forming prepares the method for Re:YAG crystalline ceramics, and the method comprises the steps:
(1) according to Re xy 3-xal 5o 12the array mode of (x is the material molar weight that part Re atom replaces the Y atom, x=0～0.1) molecular formula, by a certain amount of commercially available high-purity Y of molecular formula stoichiometric ratio weighing 2o 3powder, Al 2o 3powder, Re 2o 3powder (wherein Re is rare earth element) or different rear-earth-doped YAG powder;
(2) sintering aid adopts commercially available high-purity MgO, CaO, TEOS and wherein one or several of other sintering agent;
(3) the ball milling liquid medium is comprised of deionized water system or pure system or water and pure mixed system, and alcohols is as compositions such as methyl alcohol, ethanol, propyl alcohol, butanols, ethylene glycol, n-propyl alcohol, the trimethyl carbinols;
(4) add a certain amount of and organic monomer, linking agent, softening agent and defrother ratio, ball milling mixed powder 0.5～150 hour;
(5) will add initiator after the slurry froth in vacuum and facilitate the mould that definite shape is injected in agent, the medium slurry original position of baking oven of putting into 50～100 ℃ be solidified, and base substrate separates with mould, the demoulding.Mould can be plastics, glass or metal;
(6) after the green compact moulding, from room temperature to 200 dried ℃ stage by stage, in order to prevent the green compact distortion, 30 ℃ of initial setting drying temperatures, humidity 90% slowly increases temperature and reduces the humidity drying;
(7) give birth to biscuit after moulding and putting into tube furnace, binder removal under oxygen atmosphere;
(8) green compact after binder removal are put into vacuum oven, carry out sintering under vacuum atmosphere.
2. prepare the method for Re:YAG crystalline ceramics by gel casting forming claimed in claim 1, it is characterized in that: can add all rare earth oxides, or rare earth oxide codoped or single doping, for example: Nd 2o 3, Yb 2o 3, Cr 2o 3, Er 2o 3, Ce 2o 3, Sm 2o 3, Tm 2o 3, Eu 2o 3deng rare earth oxide.
3. prepare the method for Re:YAG crystalline ceramics by gel casting forming claimed in claim 1, it is characterized in that: 0～2at% of mole amount that the addition of described sintering aid MgO, CaO is oxide compound; 0～2wt% that the TEOS addition is mixed oxide weight; 0～2wt% that other silica-based and non-silica-based sintering aid is mixed oxide weight.
4. prepare the method for Re:YAG crystalline ceramics by gel casting forming claimed in claim 1, it is characterized in that: the solid load 30～60wt% of slurry, regulate the pH value of slurry between 7～12.
5. prepare the method for Re:YAG crystalline ceramics by gel casting forming claimed in claim 1, it is characterized in that: the organic monomer of interpolation is acrylamide, Methacrylamide, N 2-n-methylolacrylamide, linking agent is N, N '-methylene-bisacrylamide, softening agent is polyoxyethylene glycol, PMAm, the kind of dispersion agent is polyelectrolyte class dispersion agent as polyacrylic acid, sodium polyacrylate, ammonium polyacrylate, polymethyl acrylic acid, ammonium polymethacrylate, ammonium acrylate and methyl acrylate copolymer; The non-ionic polyalcohol dispersion agent is as Sudan Gum-arabic, gelatin, menhaden fish oil, Viscotrol C, carboxymethyl cellulose; High price small molecules class dispersion agent is as citric acid, ammonium citrate, 2-phosphonic acids butane-1,2,4-tricarboxylic acid; Defrother can adopt lower alcohols as methyl alcohol, ethanol, Virahol, sec-butyl alcohol, propyl carbinol, n-propyl alcohol, isooctyl alcohol; Organic polar form compound is as amylalcohol, tributyl phosphate, oleic acid, polypropylene glycol, cithrol.Catalyzer is Tetramethyl Ethylene Diamine, and initiator is Potassium Persulphate, Potassium Persulphate, hydrogen peroxide; 5wt%～35wt% that 0.2wt%～3wt% that the dispersion agent addition is powder weight, organic monomer addition are powder weight, organic monomer and linking agent ratio are between 1: 5～1: 50, the softening agent addition is that 0.5wt%～5wt%, defrother addition are 0.1～5wt%, the initiator addition is 0.1～1wt%, facilitating the agent addition is 0.1mL～1mL, the trigger monomer reaction.
6. prepare the method for Re:YAG crystalline ceramics by gel casting forming claimed in claim 1, it is characterized in that: the mixed slurry of ball milling, vacuum-treat to vacuum tightness reaches-below 0.1Mpa or micro-negative pressure, till not having bubble to overflow in slurry, slurry after de-bubble injects the mould of definite shape after adding initiator and facilitating agent, putting into 60～90 ℃ of baking oven reactions solidifies, in order to prevent that oxygen in air from stoping poly-occur with reaction and the billet surface skin effect phenomenon has added and relatively take polyethylene that the powder weight ratio is 0.2wt%～5wt% and adjoin the polyoxyethylene of pyrrolidone (PVP) or 0.2～8wt% polyacrylamide or 0.2～10wt%, Deng the base substrate contraction, with mould, separate, slough mould.
7. prepare the method for Re:YAG crystalline ceramics by gel casting forming claimed in claim 1, it is characterized in that: after the green compact moulding, can take lyophilize mode and the dry mode of room temperature high humidity slow curing in order to avoid too fast rate of drying causes the defects such as biscuit cracking, distortion, tiny crack, cause waste product.
8. prepare the method for Re:YAG crystalline ceramics by gel casting forming claimed in claim 1, it is characterized in that: the green compact of moulding are put into alumina crucible, crucible and sample are packed in vacuum oven, heat up at a slow speed (0.1～10 ℃/min) to the organic substance decomposing temperature spot (200～1300 ℃) added, insulation for some time (size per sample determines soaking time length), carry out degreasing.Can utilize vacuum, oxygen atmosphere, nitrogen atmosphere protection binder removal or inert gas atmosphere binder removal.
9. prepare the method for Re:YAG crystalline ceramics by gel casting forming claimed in claim 1, it is characterized in that: the green compact after binder removal are put into vacuum oven, carry out sintering under vacuum atmosphere, 1500 ℃～1900 ℃ of sintering ranges, sintering time is 5～120 hours (size per sample).
10. prepare the method for Re:YAG crystalline ceramics by gel casting forming claimed in claim 1, it is characterized in that: the ceramic body prepared after sintering, after the mechanical workout polishing, can be realized the impurity of highly transparent and rare earth element at visible ray and near-infrared band.
CN201110353652XA 2011-11-10 2011-11-10 Re:YAG transparent ceramic prepared through gel casting molding Pending CN103102156A (en)

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Application publication date: 20130515