CN106316381A - Preparation method of YAG-nano terbium oxide composite magneto-optical transparent ceramic - Google Patents
Preparation method of YAG-nano terbium oxide composite magneto-optical transparent ceramic Download PDFInfo
- Publication number
- CN106316381A CN106316381A CN201610648794.1A CN201610648794A CN106316381A CN 106316381 A CN106316381 A CN 106316381A CN 201610648794 A CN201610648794 A CN 201610648794A CN 106316381 A CN106316381 A CN 106316381A
- Authority
- CN
- China
- Prior art keywords
- terbium
- yag
- nano
- magneto
- preparation
- 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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
-
- 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
- C04B35/505—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 based on yttrium 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
- 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
- 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
- C04B2235/70—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
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a preparation method of a YAG-nano terbium oxide composite magneto-optical transparent ceramic. The transparent ceramic with the magneto-optical performance is prepared from YAG powder serving as a main component and composite nano terbium oxide through the steps of material mixing, screening, vacuum degassing, tape casting, adhesive discharging, isostatic cool pressing, sintering and grinding and polishing. The ceramic is good in transparency and high in Verdet constant; nano terbium oxide is prepared through large-scale alcohol heating, the method is simple and practical, large-scale preparation can be achieved, and the prepared terbium oxide nanoparticles have the good size uniformity and the monodispersity in an 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 YAG-transparent
The preparation method of pottery.
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.
YAG, is the abbreviation of yttrium-aluminium-garnet, and chemical formula is Y3Al5O12, is the one generated by Y2O3 and Al2O3 reaction
Composite oxides, belong to cubic system, have garnet structure.It it is a kind of common crystalline ceramics；Electric lighting is really won such as Jiangsu
Company limited discloses the YAG crystalline ceramics of a kind of improvement in CN201410458635.6, and described YAG crystalline ceramics is by being combined
Inorganic raw material composition is fired and is formed, and the purity of described raw material is all at more than 99.99wt%, and the thickness of crystalline ceramics is 0.2-
0.6mm.Compared with prior art, blue-ray LED is used to excite this crystalline ceramics, it is possible to produce the white light of high-quality, have colour developing
The feature that index is high and colour temperature is soft.Shaanxi Tech Univ discloses a kind of solid state reaction at CN200910021368.5 and prepares
The method of YAG transparent ceramic powder, first, by analytically pure α-al2o3powder body and Y2O3 powder body mix homogeneously and add positive silicon
Acetoacetic ester obtains powder as sintering aid；Secondly, powder put in the corundum ball grinder equipped with corundum material abrading-ball and add
By this ball grinder at planetary ball mill ball milling after dehydrated alcohol and Y2O3；The powder body material that ball milling is good is taken out and dries, so
After calcine in high-temperature electric resistance furnace and i.e. obtain pure YAG transparent ceramic powder.The mill of corundum material is directly used due to mechanical ball milling
Ball and ball grinder, need not use high-purity heterogeneous material of lapping or high cost to make abrading-ball, and therefore, its process equipment is simple,
Gained powder purity is higher, i.e. can get the good YAG crystalline ceramics of printing opacity by and high temperature sintering compressing to it.But present
The research of the preparation method being combined magneto-optic crystalline ceramics about the nano oxidized terbium of YAG-is less.
Summary of the invention
It is an object of the invention to for the problems referred to above, develop the nano oxidized terbium of a kind of YAG-and be combined magneto-optic crystalline ceramics
Preparation method, with YAG powder body as main component, composite Nano terbia. Diterbium trioxide, by batch mixing, sieves, vacuum outgas, is cast into
Type, binder removal, isostatic cool pressing, sintering, grinding and polishing, obtain the crystalline ceramics with magneto-optical property, and this pottery transparency is good,
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, made
Standby terbia. Diterbium trioxide nano-particle has the monodispersity in preferable dimensional homogeneity and alcoholic solution.
The nano oxidized terbium of a kind of YAG-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The YAG of 100-150 weight portion, YAG are commercialization YAG powder body, and particle diameter is 1-3 μm；
The nano oxidized terbium of 10-15 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 150 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 YAG powder body and nano oxidized terbium so that two kinds of raw materials are sufficiently mixed,
Ball-milling medium is ethanol；It is subsequently added the PAA ethanol solution of solid gross mass 10-15%, the PVA of solid gross mass 10-15%
The PEG-1000 ethanol solution of ethanol solution and solid gross mass 10-15%, ball milling 20h subsequently, obtain mixed slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body binder removal at 850 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, YAG-nanometer can be obtained
Terbia. Diterbium trioxide 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 1700 degrees Celsius.
Beneficial effects of the present invention:
(1) YAG and nano oxidized terbium are organically combined by the present invention, and formation the most still can be prepared on a large scale
The nano oxidized terbium of YAG-is combined magneto-optic crystalline ceramics；Due to being combined of YAG so that compound magneto-optic crystalline ceramics is compared to common
The light transmittance of single terbia. Diterbium trioxide pottery has had and has been substantially improved, and the ceramic thick for the 1mm light transmittance in visible region reaches
More than 96%, and Verdet constant is also greater than 110rad/ (T m), Verdet constant is to obtain, by method measured by conventional method
Draw rotor to be installed on permanent magnet known to flux density magnitude, measure the Verdet constant under wavelength 1.06 μm, measure bar
Part 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 terbia. Diterbium trioxide nanometer base
Open another fan window.
(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 YAG-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The YAG of 125 weight portions, YAG are commercialization YAG powder body, and particle diameter is 2 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 150 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 150 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 YAG powder body and nano oxidized terbium so that two kinds of raw materials are sufficiently mixed,
Ball-milling medium is ethanol；Being subsequently added the PAA ethanol solution of solid gross mass 10%, the PVA ethanol of solid gross mass 10% is molten
The PEG-1000 ethanol solution of liquid and solid gross mass 10%, ball milling 20h subsequently, obtain mixed slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body binder removal at 850 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 1700 degrees Celsius, after ground polishing, YAG-can be obtained nano oxidized
Terbium is 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%, and Verdet constant is 115rad/ (T
m)。
Embodiment 2:
The nano oxidized terbium of a kind of YAG-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The YAG of 100 weight portions, YAG are commercialization YAG powder body, and particle diameter is 2 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 150 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 150 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 YAG powder body and nano oxidized terbium so that two kinds of raw materials are sufficiently mixed,
Ball-milling medium is ethanol；Being subsequently added the PAA ethanol solution of solid gross mass 10%, the PVA ethanol of solid gross mass 10% is molten
The PEG-1000 ethanol solution of liquid and solid gross mass 10%, ball milling 20h subsequently, obtain mixed slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body binder removal at 850 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 1700 degrees Celsius, after ground polishing, YAG-can be obtained nano oxidized
Terbium is 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 96.5%, and Verdet constant is 114rad/ (T
m)。
Embodiment 3:
The nano oxidized terbium of a kind of YAG-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The YAG of 150 weight portions, YAG are commercialization YAG powder body, and particle diameter is 2 μm；
The nano oxidized terbium of 15 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 150 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 150 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 YAG powder body and nano oxidized terbium so that two kinds of raw materials are sufficiently mixed,
Ball-milling medium is ethanol；Being subsequently added the PAA ethanol solution of solid gross mass 10%, the PVA ethanol of solid gross mass 10% is molten
The PEG-1000 ethanol solution of liquid and solid gross mass 10%, ball milling 20h subsequently, obtain mixed slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body binder removal at 850 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 1700 degrees Celsius, after ground polishing, YAG-can be obtained nano oxidized
Terbium is 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 115rad/ (T
m)。
Comparative example 1:
The nano oxidized terbium of a kind of YAG-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The YAG 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 150 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 150 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 ethanol；It is subsequently added the PAA ethanol solution of solid gross mass 10%, the PVA ethanol solution of solid gross mass 10% and solid
The PEG-1000 ethanol solution of gross mass 10%, ball milling 20h subsequently, obtain mixed slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body binder removal at 850 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 1700 degrees Celsius, after ground polishing, YAG-can be obtained nano oxidized
Terbium is 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 85%, and Verdet constant is 124rad/ (T
m)。
Comparative example 2:
The nano oxidized terbium of a kind of YAG-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The YAG of 125 weight portions, YAG are commercialization YAG powder body, and particle diameter is 2 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 YAG powder body and nano oxidized terbium so that two kinds of raw materials are sufficiently mixed,
Ball-milling medium is ethanol；Being subsequently added the PAA ethanol solution of solid gross mass 10%, the PVA ethanol of solid gross mass 10% is molten
The PEG-1000 ethanol solution of liquid and solid gross mass 10%, ball milling 20h subsequently, obtain mixed slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body binder removal at 850 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 1700 degrees Celsius, after ground polishing, YAG-can be obtained nano oxidized
Terbium is combined magneto-optic crystalline ceramics.
The ceramic thick for the 1mm light transmittance in visible region has reached 90%, and Verdet constant is 101rad/ (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 YAG-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The YAG of 100-150 weight portion, YAG are commercialization YAG powder body, and particle diameter is 1-3 μm；
The nano oxidized terbium of 10-15 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 150 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 YAG powder body and nano oxidized terbium so that two kinds of raw materials are sufficiently mixed, ball milling
Medium is ethanol；It is subsequently added the PAA ethanol solution of solid gross mass 10-15%, the PVA ethanol of solid gross mass 10-15%
The PEG-1000 ethanol solution of solution and solid gross mass 10-15%, ball milling 20h subsequently, obtain mixed slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body binder removal at 850 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, YAG-can be obtained nano oxidized
Terbium is combined magneto-optic crystalline ceramics.
2. the nano oxidized terbium of YAG-as claimed in claim 2 is combined a preparation method for magneto-optic crystalline ceramics, and its feature exists
In: described solubility terbium salt be Terbium nitrate (Tb(NO3)3), terbium chloride, sulphuric acid terbium one or more.
3. the nano oxidized terbium of YAG-as claimed in claim 1 is combined a preparation method for magneto-optic crystalline ceramics, and its feature exists
In: in step (3), reaction temperature is 200 DEG C, and the response time is 4h.
4. the nano oxidized terbium of YAG-as claimed in claim 1 is combined a preparation method for magneto-optic crystalline ceramics, and its feature exists
In: described surfactant is one or more in oleic acid, Polyethylene Glycol, PVP.
5. the nano oxidized terbium of YAG-as claimed in claim 1 is combined a preparation method for magneto-optic crystalline ceramics, and its feature exists
In: base substrate is sintered 1.5 hours under 1700 degrees Celsius.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610648794.1A CN106316381A (en) | 2016-08-08 | 2016-08-08 | Preparation method of YAG-nano terbium oxide composite magneto-optical transparent ceramic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610648794.1A CN106316381A (en) | 2016-08-08 | 2016-08-08 | Preparation method of YAG-nano terbium oxide composite magneto-optical transparent ceramic |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106316381A true CN106316381A (en) | 2017-01-11 |
Family
ID=57739806
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610648794.1A Pending CN106316381A (en) | 2016-08-08 | 2016-08-08 | Preparation method of YAG-nano terbium oxide composite magneto-optical transparent ceramic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106316381A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| US20100032623A1 (en) * | 2008-07-09 | 2010-02-11 | OSRAM Gesellschaft Mit beschrankkter Haftung | Method for producing a garnet phosphor |
| CN102173774A (en) * | 2011-01-28 | 2011-09-07 | 中国科学院上海光学精密机械研究所 | Cerium, terbium and yttrium doped garnet transparent ceramic fluorescent material and preparation method thereof |
| 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 |
| 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 CN201610648794.1A patent/CN106316381A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100032623A1 (en) * | 2008-07-09 | 2010-02-11 | OSRAM Gesellschaft Mit beschrankkter Haftung | Method for producing a garnet phosphor |
| 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 |
| CN102173774A (en) * | 2011-01-28 | 2011-09-07 | 中国科学院上海光学精密机械研究所 | Cerium, terbium and yttrium doped garnet transparent ceramic fluorescent material and preparation method thereof |
| 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 |
| 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 |
|---|
| CHEN CHONG ET AL.: "Preparation of (Tb0.8Y0.2)3Al5O12 transparent ceramic as novel magneto-optical isolator material", 《CHINESE OPTICS LETTERS》 * |
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 | |
| CN102126857A (en) | Method for preparing transparent calcium fluoride ceramic | |
| CN105294138A (en) | Doublet aluminum oxide micropowder and preparation method thereof | |
| CN105272269A (en) | Preparation method of Si3N4/h-BN nano-composite ceramics | |
| CN111285380A (en) | Preparation method and application of multi-rare earth co-doped boride and nano heat insulation powder thereof | |
| CN102815941B (en) | Rare-earth-ion-doped lanthanum gadolinium zirconate transparent ceramic material and preparation method thereof | |
| CN102531606B (en) | Low-temperature manufacturing method of high-strength and toughness silicon carbide ceramics | |
| CN102093038B (en) | Method for manufacturing transparent alumina ceramic and application thereof | |
| CN109678506A (en) | A kind of preparation method of erbium oxide crystalline ceramics | |
| CN107880884A (en) | A kind of preparation method of cerium dopping rare earth silicate polycrystal powder | |
| CN102815945B (en) | Lanthanum gadolinium zirconate transparent ceramic material and preparation method thereof | |
| CN108609652A (en) | A method of preparing Zirconium dioxide nano powder using fused salt | |
| CN110550945B (en) | Preparation method of LuAG Ce transparent ceramic and LuAG Ce transparent ceramic | |
| CN106316381A (en) | Preparation method of YAG-nano terbium oxide composite magneto-optical transparent ceramic | |
| CN106145955A (en) | The nano oxidized terbium of a kind of ALON is combined the preparation method of magneto-optic crystalline ceramics | |
| CN114538920B (en) | Preparation method of high-toughness high-hardness zirconium lanthanum aluminum composite grinding medium | |
| CN114524440B (en) | High-entropy rare earth co-doped nano low-heat-transfer powder material and preparation method thereof | |
| CN106278198A (en) | A kind of oxidized alumina nano terbium is combined the preparation method of magneto-optic crystalline ceramics | |
| CN106242583A (en) | The nano oxidized terbium of a kind of SiALON is combined the preparation method of magneto-optic crystalline ceramics | |
| CN106242577A (en) | The nano oxidized terbium of a kind of MgALON is combined the preparation method of magneto-optic crystalline ceramics | |
| CN115925408B (en) | Transparent scintillating ceramic material and preparation method and application thereof | |
| CN104774608A (en) | Rare earth-doped alpha'-phase Sr2SiO4 nano-powder and preparation method thereof | |
| CN109970090A (en) | The ultra-fine ytterbium oxide chemical preparation process that a kind of D50 is 1.5-2um |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | 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: 20170111 |
|
| WD01 | Invention patent application deemed withdrawn after publication |