CN106242577A - The nano oxidized terbium of a kind of MgALON is combined the preparation method of magneto-optic crystalline ceramics - Google Patents
The nano oxidized terbium of a kind of MgALON is combined the preparation method of magneto-optic crystalline ceramics Download PDFInfo
- Publication number
- CN106242577A CN106242577A CN201610647339.XA CN201610647339A CN106242577A CN 106242577 A CN106242577 A CN 106242577A CN 201610647339 A CN201610647339 A CN 201610647339A CN 106242577 A CN106242577 A CN 106242577A
- Authority
- CN
- China
- Prior art keywords
- terbium
- mgalon
- nano
- magneto
- terbia
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/30—Producing shaped prefabricated articles from the material by applying the material on to a core or other moulding surface to form a layer thereon
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63416—Polyvinylalcohols [PVA]; Polyvinylacetates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63424—Polyacrylates; Polymethacrylates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63488—Polyethers, e.g. alkylphenol polyglycolether, polyethylene glycol [PEG], polyethylene oxide [PEO]
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9646—Optical properties
- C04B2235/9653—Translucent or transparent ceramics other than alumina
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses the nano oxidized terbium of a kind of MgALON and be combined the preparation method of magneto-optic crystalline ceramics, with MgALON powder body as main component, composite Nano terbia. Diterbium trioxide, by batch mixing, sieve, vacuum outgas, carry out flow casting molding, binder removal, isostatic cool pressing, sintering, grinding and polishing, obtain the crystalline ceramics with magneto-optical property, this pottery transparency is good, and Verdet constant is high；This nano oxidized terbium uses extensive alcohol hot preparation, and the method is simple and practical, can prepare on a large scale, and prepared terbia. Diterbium trioxide nano-particle has the monodispersity in preferable dimensional homogeneity and alcoholic solution.
Description
Technical field
The invention belongs to magneto-optic transparent ceramic material field, be combined magneto-optic particularly to a kind of nano oxidized terbium of MgALON-
The preparation method of crystalline ceramics.
Background technology
Terbia. Diterbium trioxide be recent years by wide variety of rare earth oxide, relative to other common rare-earth oxidation
Thing, during terbium belongs in 15 kinds of rare earth elements, heavy rare earth, in the earth's crust, content is the lowest, even if at the high yttrium the highest containing terbium
In ion-type heavy rare earth ore deposit, the content of terbium the most only accounts for the 1.1-1.2% of total rare earth (TRE).In general middle yttrium richness europium material, the content of terbium exists
0.6-0.8%, as the content of terbium content in total rare earth (TRE) in the northern China ore deposit based on light rare earth less than 0.01%.
Rare and valuable just because of terbium, thus its application is quite limited to, but, along with electronics and information industry
Fast development, the new function material of terbio rare earth arises at the historic moment, and many excellent specific properties of terbium become new function material
In indispensable a member, and in some field, be in the irreplaceable status of other material.Owing to terbium is rare, so valency
Lattice are expensive, and preparation high-grade terbium is the most difficult, therefore, and the highly desirable a kind of method finding preparation cost low of people.
The research worker such as the Dong Yuming of nearest Southern Yangtze University use short-cut method to obtain oxygen in CN201310260729.8
Change terbium nano material, and establish the organic using method of oxygen catalytic oxidation, implement in accordance with the following steps: (1) terbia. Diterbium trioxide
The preparation method of nano material: added by 2.0g terbia. Diterbium trioxide (common rare-earth products) in concentrated hydrochloric acid (37%), the lower stirring of heating is molten
Xie Hou, vapors away unnecessary hydrochloric acid and moisture, is dissolved in 200mL water by the terbium chloride obtained, with NaOH regulation to pH=7, transfer
In closed reactor, 180 DEG C are heated 12 hours, by the white precipitate washing obtained, dry, calcine 2 hours at 500 DEG C,
Obtain brown solid, for terbium oxide nano material.(2) terbium oxide nano material is as the using method of analogue enztme: by synthesis
Nano material adds in the acidic buffer containing substrate, fully vibration or stirring, the dioxygen oxidation substrate in catalytic solution.No
Crossing due to coprecipitation method, the distribution of sizes of prepared terbium oxide nano material there is also certain room for improvement.
The research worker such as the Zhang Le of Jiangsu Normal University disclose a kind of magneto-optic terbia. Diterbium trioxide in CN201610104880.6
The preparation method of crystalline ceramics.First adding to dissolve in nitric acid by terbia. Diterbium trioxide micro-powder and form Tb (NO3) 3, dilute obtains Tb
(NO3) 3 solution；Again (NH4) 2SO4 is joined and Tb (NO3) 3 solution after dilution obtains mother solution；Then it is added drop-wise to precipitant
Stirring in mother solution, the pH value to mother solution is 7.5～8.5；Continue stirring, static ageing；The precipitate being filtrated to get, by precipitate
Rinsing, drying, grinding are sieved, are calcined；Molding；Vacuum heating-press sintering obtains magneto-optic terbia. Diterbium trioxide crystalline ceramics.The present invention be all
Preparing magneto-optic terbia. Diterbium trioxide pottery under relatively low sintering temperature, economical and energy saving effect is obvious.The method using vacuum heating-press sintering,
Well control the discharge of pore, be unlikely to sintering growth too fast, cause pore to be wrapping to the inside of crystal grain, vacuum reduction
The valence state well controlling Tb ion under state is unified, and ceramic dense degree is high, crystallite dimension is little, even size distribution, magneto-optic
Can be good.But relatively costly due to terbium, prepared magneto-optic crystalline ceramics cost is high.
MgALON, the research new direction of present crystalline ceramics；Such as Wuhan University of Technology's public affairs in CN201510133394.2
Open a kind of method that Direct Coagulation Casting prepares MgAlON crystalline ceramics biscuit.It comprises the steps: 1) preparation
MgAlON ceramic size；Adding the aqueous solution of the dispersant that pH preconditioning is 8-11 in MgAlON powder body to be formed, mixing is also
Stirring, in the aqueous solution of described dispersant, the addition of dispersant is the 0.1～0.5wt% of MgAlON powder quality to be formed,
Obtain MgAlON ceramic size；2) add additive: by step 1) in the MgAlON ceramic size of gained add under condition of ice bath
Enter coagulator, stirring so that it is dispersed in MgAlON ceramic size；3) de-bubble；4) injection molding solidification；5) body drying.Should
Method is simple, and condition is easily-controllable, and the MgAlON crystalline ceramics biscuit shape prepared is intact, uniform microstructure, and sintering obtains
MgAlON crystalline ceramics sample optical transmission good.Shenzhen Graduate School of Tsinghua University is disclosed in CN200510035304.2
Preparing method and the high-purity dense MgAlON ceramic of high-purity dense MgAlON ceramic, its method is former with MgO, Al2O3 and AlN
Material, ball milling becomes mixed powder, uses discharge plasma sintering technique, is prepared by suitable sintering process and have certain chemistry
The high-purity dense MgAlON ceramic of composition.It achieve the quick of the high purity high dense MgAlON pottery that traditional method is difficult to
Efficiently preparation, it is possible at a lower temperature, the supper-fast MgAlON pottery preparing high-purity or single-phase densification.Prepare is high-purity
In dense MgAlON ceramic, the content of MgAlON phase is 95～100%, and relative density is 92～99%, bulk density be 3.4～
3.8g/cm3, can be widely applied to refractory material and high-performance ceramics field.But multiple now concerning the nano oxidized terbium of MgALON-
The research of the preparation method closing magneto-optic crystalline ceramics is less.
Summary of the invention
It is an object of the invention to for the problems referred to above, develop a kind of nano oxidized terbium of MgALON-and be combined the transparent pottery of magneto-optic
The preparation method of porcelain, with MgALON powder body as main component, composite Nano terbia. Diterbium trioxide, by batch mixing, sieves, vacuum outgas, enters
Row flow casting molding, binder removal, isostatic cool pressing, sintering, grinding and polishing, obtain the crystalline ceramics with magneto-optical property, this pottery
Transparency is good, and Verdet constant is high；This nano oxidized terbium uses extensive alcohol hot preparation, and the method is simple and practical, can be extensive
Preparation, prepared terbia. Diterbium trioxide nano-particle has the monodispersity in preferable dimensional homogeneity and alcoholic solution.
The nano oxidized terbium of a kind of MgALON-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The MgALON of 100-170 weight portion, MgALON are the MgALON powder body prepared by reaction sintering, and particle diameter is 1-3 μ
m；
The nano oxidized terbium of 10-20 weight portion, nano oxidized terbium is the terbia. Diterbium trioxide nano-particle prepared by following methods, grain
Footpath is 5-50nm；Terbia. Diterbium trioxide nano-particle is prepared by extensive alcohol full-boiled process, including following preparation process:
1) benzyl alcohol of the solubility terbium salt of 10 weight portions Yu 100-200 weight portion is added in agitator tank, at 40-50 DEG C
Lower mechanical agitation 30-60min so that solubility terbium salt is completely dissolved, obtains the solution of transparent and homogeneous, standby；
2) stock solution is delivered to pre-reaction room, under 160 DEG C of atmosphere of inert gases, reacts 3h, obtain pre-reaction molten
Liquid；
3) pre-reaction solution is inputted to reative cell, surfactant is inputted to reative cell simultaneously, lazy at 180-210 DEG C
Property atmosphere under react 3-5h, obtain reactant liquor；
4) reactant liquor is delivered to separation chamber by condensing tube, is separated by high speed centrifugation, obtain upper strata benzyl alcohol and under
The terbia. Diterbium trioxide nano-particle that layer concentrates；
5) upper strata benzyl alcohol is delivered to waste reclaimation in agitator tank after treatment, the terbia. Diterbium trioxide that lower floor concentrates is received
Rice grain is scrubbed, be dried, pack, and can obtain terbia. Diterbium trioxide nano-particle；
(2) batch mixing, is positioned over ball milling in ball mill by MgALON powder body and nano oxidized terbium so that two kinds of raw materials are the most mixed
Closing, ball-milling medium is dimethylbenzene；It is subsequently added the PAA xylene solution of solid gross mass 10-20%, solid gross mass 10-
The PVA xylene solution of 20% and the PEG-1000 xylene solution of solid gross mass 10-20%, ball milling 7h subsequently, mixed
Close slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body binder removal at 910 DEG C, carry out isostatic cool pressing process subsequently, obtain the base substrate of uniform compact；
(5) base substrate is sintered 1-2 hour under 1650-1800 degree Celsius, after ground polishing, MgALON-can be obtained
Nano oxidized terbium is combined magneto-optic crystalline ceramics.
As preferably, described solubility terbium salt be Terbium nitrate (Tb(NO3)3), terbium chloride, sulphuric acid terbium one or more.
As preferably, step 3) in reaction temperature be 200 DEG C, the response time is 4h.
As preferably, described surfactant is one or more in oleic acid, Polyethylene Glycol, PVP.
As preferably, base substrate is sintered 1.5 hours under 1750 degrees Celsius.
Beneficial effects of the present invention:
(1) but MgALON and nano oxidized terbium are organically combined by the present invention, are formed cheap can prepare on a large scale
The nano oxidized terbium of MgALON-be combined magneto-optic crystalline ceramics；Due to being combined of MgALON so that compound magneto-optic crystalline ceramics is compared
Have in the light transmittance that common single terbia. Diterbium trioxide is ceramic and be substantially improved, the ceramic thick for the 1mm light transmittance in visible region
Having reached more than 95%, and Verdet constant is also greater than 115rad/ (T m), Verdet constant is that conventional method is measured to be obtained
Arrive, Faraday rotor be installed on permanent magnet known to flux density magnitude, measure the Verdet constant under wavelength 1.06 μm,
Condition determination is to carry out under room temperature air.
(2) compared to the preparation method of terbium oxide nano material of the prior art, the application uses alcohol pyrolysismethod to enter
The extensive preparation of row, through the alcohol thermal crystallisation of high temperature, prepared terbia. Diterbium trioxide nano is good, and this is for the physical and chemical performance of pottery
Having a major impact, the method is simple and practical simultaneously, can prepare on a large scale, and prepared terbia. Diterbium trioxide nano-particle has preferable chi
Monodispersity in very little homogeneity and alcoholic solution.This also makes the industrialized production of magneto-optic crystalline ceramics of nano oxidized terbio
Open another fan window.Prepared nano-particle and the tape casting are combined by the present invention, and selection slurry solvent is diformazan
Benzene, it has the good compatibility with by terbia. Diterbium trioxide nano-particle, meanwhile, in the selection of curtain coating system, present invention selection
Add the PAA xylene solution of solid gross mass 10-20%, the PVA xylene solution of solid gross mass 10-20% and solid
The PEG-1000 xylene solution of gross mass 10-20%, and after binder removal, carry out isostatic cool pressing process, improve system from entirety
The performance such as consistency, then improve the magneto-optical property of composite ceramics.
(3) present invention is in preparation technology, on the premise of optimizing for function ceramics performance, optimizes preparation work
Skill, is especially combined the nano material of alcohol full-boiled process by alcohol radical the tape casting, more suitably adds raw material by selection, preparation
Obtain high-compactness, highly purified magneto-optic crystalline ceramics.
Accompanying drawing explanation
Hereinafter, describe embodiment of the present invention in detail in conjunction with accompanying drawing, wherein:
Fig. 1 is the TEM figure of the terbia. Diterbium trioxide nano-particle prepared by the embodiment of the present invention 1；
Detailed description of the invention
Below in conjunction with specific embodiment, and with reference to data, the present invention is described in further detail.Should be understood that these embodiments
The present invention solely for the purpose of illustration, rather than limit the scope of the present invention by any way.
Embodiment 1:
The nano oxidized terbium of a kind of MgALON-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The MgALON of 125 weight portions, MgALON are the MgALON powder body prepared by reaction sintering, and particle diameter is 1.5 μm；
The nano oxidized terbium of 12 weight portions, nano oxidized terbium is the terbia. Diterbium trioxide nano-particle prepared by following methods, particle diameter
For 10nm；Terbia. Diterbium trioxide nano-particle is prepared by extensive alcohol full-boiled process, including following preparation process:
1) the solubility terbium salt of 10 weight portions and the benzyl alcohol of 170 weight portions are added in agitator tank, machinery at 45 DEG C
Stirring 45min so that solubility terbium salt is completely dissolved, and obtains the solution of transparent and homogeneous, standby；
2) stock solution is delivered to pre-reaction room, under 160 DEG C of atmosphere of inert gases, reacts 3h, obtain pre-reaction molten
Liquid；
3) pre-reaction solution is inputted to reative cell, surfactant is inputted to reative cell, at 200 DEG C of indifferent gas simultaneously
React 4h under body atmosphere, obtain reactant liquor；
4) reactant liquor is delivered to separation chamber by condensing tube, is separated by high speed centrifugation, obtain upper strata benzyl alcohol and under
The terbia. Diterbium trioxide nano-particle that layer concentrates；
5) upper strata benzyl alcohol is delivered to waste reclaimation in agitator tank after treatment, the terbia. Diterbium trioxide that lower floor concentrates is received
Rice grain is scrubbed, be dried, pack, and can obtain terbia. Diterbium trioxide nano-particle；
(2) batch mixing, is positioned over ball milling in ball mill by MgALON powder body and nano oxidized terbium so that two kinds of raw materials are the most mixed
Closing, ball-milling medium is dimethylbenzene；It is subsequently added the PAA xylene solution of solid gross mass 15%, the PVA of solid gross mass 15%
The PEG-1000 xylene solution of xylene solution and solid gross mass 15%, ball milling 7h subsequently, obtain mixed slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body binder removal at 910 DEG C, carry out isostatic cool pressing process subsequently, obtain the base substrate of uniform compact；
(5) base substrate is sintered 1.5 hours under 1750 degrees Celsius, after ground polishing, MgALON-nano oxygen can be obtained
Change terbium and be combined magneto-optic crystalline ceramics.
Described solubility terbium salt is Terbium nitrate (Tb(NO3)3).
Described surfactant is oleic acid.
The ceramic thick for the 1mm light transmittance in visible region has reached 97.5%, and Verdet constant is 119rad/ (T
m)。
Embodiment 2:
The nano oxidized terbium of a kind of MgALON-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The MgALON of 100 weight portions, MgALON are the MgALON powder body prepared by reaction sintering, and particle diameter is 1.5 μm；
The nano oxidized terbium of 10 weight portions, nano oxidized terbium is the terbia. Diterbium trioxide nano-particle prepared by following methods, particle diameter
For 10nm；Terbia. Diterbium trioxide nano-particle is prepared by extensive alcohol full-boiled process, including following preparation process:
1) the solubility terbium salt of 10 weight portions and the benzyl alcohol of 170 weight portions are added in agitator tank, machinery at 45 DEG C
Stirring 45min so that solubility terbium salt is completely dissolved, and obtains the solution of transparent and homogeneous, standby；
2) stock solution is delivered to pre-reaction room, under 160 DEG C of atmosphere of inert gases, reacts 3h, obtain pre-reaction molten
Liquid；
3) pre-reaction solution is inputted to reative cell, surfactant is inputted to reative cell, at 200 DEG C of indifferent gas simultaneously
React 4h under body atmosphere, obtain reactant liquor；
4) reactant liquor is delivered to separation chamber by condensing tube, is separated by high speed centrifugation, obtain upper strata benzyl alcohol and under
The terbia. Diterbium trioxide nano-particle that layer concentrates；
5) upper strata benzyl alcohol is delivered to waste reclaimation in agitator tank after treatment, the terbia. Diterbium trioxide that lower floor concentrates is received
Rice grain is scrubbed, be dried, pack, and can obtain terbia. Diterbium trioxide nano-particle；
(2) batch mixing, is positioned over ball milling in ball mill by MgALON powder body and nano oxidized terbium so that two kinds of raw materials are the most mixed
Closing, ball-milling medium is dimethylbenzene；It is subsequently added the PAA xylene solution of solid gross mass 15%, the PVA of solid gross mass 15%
The PEG-1000 xylene solution of xylene solution and solid gross mass 15%, ball milling 7h subsequently, obtain mixed slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body binder removal at 910 DEG C, carry out isostatic cool pressing process subsequently, obtain the base substrate of uniform compact；
(5) base substrate is sintered 1.5 hours under 1750 degrees Celsius, after ground polishing, MgALON-nano oxygen can be obtained
Change terbium and be combined magneto-optic crystalline ceramics.
Described solubility terbium salt is Terbium nitrate (Tb(NO3)3).
Described surfactant is oleic acid.
The ceramic thick for the 1mm light transmittance in visible region has reached 96.9%, and Verdet constant is 118rad/ (T
m)。
Embodiment 3:
The nano oxidized terbium of a kind of MgALON-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The MgALON of 170 weight portions, MgALON are the MgALON powder body prepared by reaction sintering, and particle diameter is 1.5 μm；
The nano oxidized terbium of 20 weight portions, nano oxidized terbium is the terbia. Diterbium trioxide nano-particle prepared by following methods, particle diameter
For 10nm；Terbia. Diterbium trioxide nano-particle is prepared by extensive alcohol full-boiled process, including following preparation process:
1) the solubility terbium salt of 10 weight portions and the benzyl alcohol of 170 weight portions are added in agitator tank, machinery at 45 DEG C
Stirring 45min so that solubility terbium salt is completely dissolved, and obtains the solution of transparent and homogeneous, standby；
2) stock solution is delivered to pre-reaction room, under 160 DEG C of atmosphere of inert gases, reacts 3h, obtain pre-reaction molten
Liquid；
3) pre-reaction solution is inputted to reative cell, surfactant is inputted to reative cell, at 200 DEG C of indifferent gas simultaneously
React 4h under body atmosphere, obtain reactant liquor；
4) reactant liquor is delivered to separation chamber by condensing tube, is separated by high speed centrifugation, obtain upper strata benzyl alcohol and under
The terbia. Diterbium trioxide nano-particle that layer concentrates；
5) upper strata benzyl alcohol is delivered to waste reclaimation in agitator tank after treatment, the terbia. Diterbium trioxide that lower floor concentrates is received
Rice grain is scrubbed, be dried, pack, and can obtain terbia. Diterbium trioxide nano-particle；
(2) batch mixing, is positioned over ball milling in ball mill by MgALON powder body and nano oxidized terbium so that two kinds of raw materials are the most mixed
Closing, ball-milling medium is dimethylbenzene；It is subsequently added the PAA xylene solution of solid gross mass 15%, the PVA of solid gross mass 15%
The PEG-1000 xylene solution of xylene solution and solid gross mass 15%, ball milling 7h subsequently, obtain mixed slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body binder removal at 910 DEG C, carry out isostatic cool pressing process subsequently, obtain the base substrate of uniform compact；
(5) base substrate is sintered 1.5 hours under 1750 degrees Celsius, after ground polishing, MgALON-nano oxygen can be obtained
Change terbium and be combined magneto-optic crystalline ceramics.
Described solubility terbium salt is Terbium nitrate (Tb(NO3)3).
Described surfactant is oleic acid.
The ceramic thick for the 1mm light transmittance in visible region has reached 97.9%, and Verdet constant is 118rad/ (T
m)。
Comparative example 1:
The nano oxidized terbium of a kind of MgALON-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The MgALON of 0 weight portion；
The nano oxidized terbium of 12 weight portions, nano oxidized terbium is the terbia. Diterbium trioxide nano-particle prepared by following methods, particle diameter
For 10nm；Terbia. Diterbium trioxide nano-particle is prepared by extensive alcohol full-boiled process, including following preparation process:
1) the solubility terbium salt of 10 weight portions and the benzyl alcohol of 170 weight portions are added in agitator tank, machinery at 45 DEG C
Stirring 45min so that solubility terbium salt is completely dissolved, and obtains the solution of transparent and homogeneous, standby；
2) stock solution is delivered to pre-reaction room, under 160 DEG C of atmosphere of inert gases, reacts 3h, obtain pre-reaction molten
Liquid；
3) pre-reaction solution is inputted to reative cell, surfactant is inputted to reative cell, at 200 DEG C of indifferent gas simultaneously
React 4h under body atmosphere, obtain reactant liquor；
4) reactant liquor is delivered to separation chamber by condensing tube, is separated by high speed centrifugation, obtain upper strata benzyl alcohol and under
The terbia. Diterbium trioxide nano-particle that layer concentrates；
5) upper strata benzyl alcohol is delivered to waste reclaimation in agitator tank after treatment, the terbia. Diterbium trioxide that lower floor concentrates is received
Rice grain is scrubbed, be dried, pack, and can obtain terbia. Diterbium trioxide nano-particle；
(2) batch mixing, is positioned over ball milling in ball mill by nano oxidized terbium so that two kinds of raw materials are sufficiently mixed, ball-milling medium
For dimethylbenzene；It is subsequently added the PAA xylene solution of solid gross mass 15%, the PVA xylene solution of solid gross mass 15%
With the PEG-1000 xylene solution of solid gross mass 15%, ball milling 7h subsequently, obtain mixed slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body binder removal at 910 DEG C, carry out isostatic cool pressing process subsequently, obtain the base substrate of uniform compact；
(5) base substrate is sintered 1.5 hours under 1750 degrees Celsius, after ground polishing, MgALON-nano oxygen can be obtained
Change terbium and be combined magneto-optic crystalline ceramics.
Described solubility terbium salt is Terbium nitrate (Tb(NO3)3).
Described surfactant is oleic acid.
The ceramic thick for the 1mm light transmittance in visible region has reached 82%, and Verdet constant is 123rad/ (T
m)。
Comparative example 2:
The nano oxidized terbium of a kind of MgALON-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The MgALON of 125 weight portions, MgALON are the MgALON powder body prepared by reaction sintering, and particle diameter is 1.5 μm；
The nano oxidized terbium of 12 weight portions, nano oxidized terbium is the terbia. Diterbium trioxide nano-particle prepared by following methods, particle diameter
For 10nm；Terbia. Diterbium trioxide nano-particle coprecipitation prepares gained；
(2) batch mixing, is positioned over ball milling in ball mill by MgALON powder body and nano oxidized terbium so that two kinds of raw materials are the most mixed
Closing, ball-milling medium is dimethylbenzene；It is subsequently added the PAA xylene solution of solid gross mass 15%, the PVA of solid gross mass 15%
The PEG-1000 xylene solution of xylene solution and solid gross mass 15%, ball milling 7h subsequently, obtain mixed slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body binder removal at 910 DEG C, carry out isostatic cool pressing process subsequently, obtain the base substrate of uniform compact；
(5) base substrate is sintered 1.5 hours under 1750 degrees Celsius, after ground polishing, MgALON-nano oxygen can be obtained
Change terbium and be combined magneto-optic crystalline ceramics.
The ceramic thick for the 1mm light transmittance in visible region has reached 90.5%, and Verdet constant is 100rad/ (T
m)。
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of the spirit or essential attributes of the present invention, it is possible to realize the present invention in other specific forms.Therefore, no matter
From the point of view of which point, all should regard embodiment as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all by fall in the implication of equivalency and scope of claim
Change is included in the present invention.
Although moreover, it will be appreciated that this specification is been described by according to embodiment, but the most each embodiment only wraps
Containing an independent technical scheme, this narrating mode of description is only that for clarity sake those skilled in the art should
Description can also be formed those skilled in the art through appropriately combined as an entirety, the technical scheme in each embodiment
May be appreciated other embodiments.
Claims (5)
1. the nano oxidized terbium of MgALON-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The MgALON of 100-170 weight portion, MgALON are the MgALON powder body prepared by reaction sintering, and particle diameter is 1-3 μm；
The nano oxidized terbium of 10-20 weight portion, nano oxidized terbium is the terbia. Diterbium trioxide nano-particle prepared by following methods, and particle diameter is
5-50nm；Terbia. Diterbium trioxide nano-particle is prepared by extensive alcohol full-boiled process, including following preparation process: 1) by 10 weight portions can
Dissolubility terbium salt is added in agitator tank with the benzyl alcohol of 100-200 weight portion, mechanical agitation 30-60min at 40-50 DEG C so that
Solubility terbium salt is completely dissolved, and obtains the solution of transparent and homogeneous, standby；
2) stock solution is delivered to pre-reaction room, under 160 DEG C of atmosphere of inert gases, reacts 3h, obtain pre-reaction solution；
3) pre-reaction solution is inputted to reative cell, surfactant is inputted to reative cell, at 180-210 DEG C of indifferent gas simultaneously
React 3-5h under body atmosphere, obtain reactant liquor；
4) reactant liquor is delivered to separation chamber by condensing tube, is separated by high speed centrifugation, obtain upper strata benzyl alcohol and lower floor is dense
The terbia. Diterbium trioxide nano-particle of contracting；
5) upper strata benzyl alcohol is delivered to waste reclaimation in agitator tank after treatment, the terbia. Diterbium trioxide nanometer lower floor concentrated
Grain is scrubbed, be dried, pack, and can obtain terbia. Diterbium trioxide nano-particle；
(2) batch mixing, is positioned over ball milling in ball mill by MgALON powder body and nano oxidized terbium so that two kinds of raw materials are sufficiently mixed,
Ball-milling medium is dimethylbenzene；It is subsequently added the PAA xylene solution of solid gross mass 10-20%, solid gross mass 10-20%
The PEG-1000 xylene solution of PVA xylene solution and solid gross mass 10-20%, ball milling 7h subsequently, obtain mixed slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body binder removal at 910 DEG C, carry out isostatic cool pressing process subsequently, obtain the base substrate of uniform compact；
(5) base substrate is sintered 1-2 hour under 1650-1800 degree Celsius, after ground polishing, MgALON-nanometer can be obtained
Terbia. Diterbium trioxide is combined magneto-optic crystalline ceramics.
2. the nano oxidized terbium of MgALON-as claimed in claim 2 is combined a preparation method for magneto-optic crystalline ceramics, its feature
Be: described solubility terbium salt be Terbium nitrate (Tb(NO3)3), terbium chloride, sulphuric acid terbium one or more.
3. the nano oxidized terbium of MgALON-as claimed in claim 1 is combined a preparation method for magneto-optic crystalline ceramics, its feature
Be: step 3) in reaction temperature be 200 DEG C, the response time is 4h.
4. the nano oxidized terbium of MgALON-as claimed in claim 1 is combined a preparation method for magneto-optic crystalline ceramics, its feature
It is: described surfactant is one or more in oleic acid, Polyethylene Glycol, PVP.
5. the nano oxidized terbium of MgALON-as claimed in claim 1 is combined a preparation method for magneto-optic crystalline ceramics, its feature
It is: base substrate is sintered 1.5 hours under 1750 degrees Celsius.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610647339.XA CN106242577A (en) | 2016-08-08 | 2016-08-08 | The nano oxidized terbium of a kind of MgALON is combined the preparation method of magneto-optic crystalline ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610647339.XA CN106242577A (en) | 2016-08-08 | 2016-08-08 | The nano oxidized terbium of a kind of MgALON is combined the preparation method of magneto-optic crystalline ceramics |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106242577A true CN106242577A (en) | 2016-12-21 |
Family
ID=58079145
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610647339.XA Pending CN106242577A (en) | 2016-08-08 | 2016-08-08 | The nano oxidized terbium of a kind of MgALON is combined the preparation method of magneto-optic crystalline ceramics |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106242577A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1709823A (en) * | 2005-06-21 | 2005-12-21 | 清华大学深圳研究生院 | Method for preparing transparent MgAlON ceramic and transparent MgAlON ceramic |
| CN101584981A (en) * | 2009-06-12 | 2009-11-25 | 华中师范大学 | Low-temperature preparation method of ceria nano-crystalline microsphere of graduation structure |
| CN104744045A (en) * | 2015-03-25 | 2015-07-01 | 武汉理工大学 | Method for preparing MgAlON transparent ceramic biscuit by direct coagulation casting |
| CN104844217A (en) * | 2015-04-01 | 2015-08-19 | 苏州工业园区晶冠瓷材料科技有限公司 | Preparation method of AlON transparent ceramic phosphor for warm-color warm-white LED packaging light source |
| CN104961466A (en) * | 2015-06-10 | 2015-10-07 | 武汉理工大学 | Preparation method of rare earth ion-doped MgAlON transparent ceramic material with ultraviolet filtration ability |
| CN105753473A (en) * | 2016-02-25 | 2016-07-13 | 江苏师范大学 | Preparation method of magneto-optic terbium oxide transparent ceramic |
-
2016
- 2016-08-08 CN CN201610647339.XA patent/CN106242577A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1709823A (en) * | 2005-06-21 | 2005-12-21 | 清华大学深圳研究生院 | Method for preparing transparent MgAlON ceramic and transparent MgAlON ceramic |
| CN101584981A (en) * | 2009-06-12 | 2009-11-25 | 华中师范大学 | Low-temperature preparation method of ceria nano-crystalline microsphere of graduation structure |
| CN104744045A (en) * | 2015-03-25 | 2015-07-01 | 武汉理工大学 | Method for preparing MgAlON transparent ceramic biscuit by direct coagulation casting |
| CN104844217A (en) * | 2015-04-01 | 2015-08-19 | 苏州工业园区晶冠瓷材料科技有限公司 | Preparation method of AlON transparent ceramic phosphor for warm-color warm-white LED packaging light source |
| CN104961466A (en) * | 2015-06-10 | 2015-10-07 | 武汉理工大学 | Preparation method of rare earth ion-doped MgAlON transparent ceramic material with ultraviolet filtration ability |
| CN105753473A (en) * | 2016-02-25 | 2016-07-13 | 江苏师范大学 | Preparation method of magneto-optic terbium oxide transparent ceramic |
Non-Patent Citations (1)
| Title |
|---|
| XIN LIU，ET AL.: ""Characterization in activators’ distribution and photoluminescence properties of Ce3+ doped MgAlON transparent fluorescent ceramic"", 《JOURNAL OF THE EUROPEAN CERAMIC SOCIETY》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Li et al. | Microwave-assisted Sol− Gel synthesis and photoluminescence characterization of LaPO4: Eu3+, Li+ nanophosphors | |
| CN108689422B (en) | Preparation method of large-specific-surface-area nano gadolinium oxide powder | |
| CN103408062B (en) | Gallium aluminium mixes the preparation method of zinc oxide nano powder and high-density high conductance sputtering coating target thereof altogether | |
| CN111377737B (en) | Tetragonal phase nano-doped zirconia ceramic powder material and preparation method thereof | |
| CN102126857A (en) | Method for preparing transparent calcium fluoride ceramic | |
| CN111285380A (en) | Preparation method and application of multi-rare earth co-doped boride and nano heat insulation powder thereof | |
| CN113816379B (en) | Preparation method of nano hafnium boride powder | |
| CN111484050B (en) | Preparation method of spheroidal alpha-phase nano-alumina | |
| CN108300474B (en) | Method for preparing nano yttrium aluminum garnet fluorescent powder | |
| CN106966430B (en) | A kind of preparation method of metal vanadate nano material | |
| CN108609652A (en) | A method of preparing Zirconium dioxide nano powder using fused salt | |
| CN111470867B (en) | Zirconium carbide ceramic hollow microsphere and preparation method thereof | |
| CN106242577A (en) | The nano oxidized terbium of a kind of MgALON is combined the preparation method of magneto-optic crystalline ceramics | |
| CN111439778A (en) | Preparation method of nano-grade gallium oxide | |
| CN106145955A (en) | The nano oxidized terbium of a kind of ALON is combined the preparation method of magneto-optic crystalline ceramics | |
| CN108610048B (en) | Preparation of corundum type Mg with low sintering temperature4Ta2O9Method for preparing microwave dielectric ceramic material | |
| CN110550945B (en) | Preparation method of LuAG Ce transparent ceramic and LuAG Ce transparent ceramic | |
| CN106278198A (en) | A kind of oxidized alumina nano terbium is combined the preparation method of magneto-optic crystalline ceramics | |
| CN106316381A (en) | Preparation method of YAG-nano terbium oxide composite magneto-optical transparent ceramic | |
| CN106242583A (en) | The nano oxidized terbium of a kind of SiALON is combined the preparation method of magneto-optic crystalline ceramics | |
| CN106495194B (en) | A kind of method of low temperature preparation alpha-type aluminum oxide superfine powder | |
| CN101070175A (en) | Method for preparing nano Al2O3 adopting salt-melting calcination process | |
| CN114028966A (en) | Preparation method of novel nano tin oxide transparent dispersion liquid | |
| CN114291844A (en) | Preparation method of bismuth oxide coated YSZ powder | |
| CN110395908A (en) | Ceramic crystalline glaze seed slurry and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20161221 |
|
| WD01 | Invention patent application deemed withdrawn after publication |