CN106145955A - The nano oxidized terbium of a kind of ALON is combined the preparation method of magneto-optic crystalline ceramics - Google Patents
The nano oxidized terbium of a kind of ALON is combined the preparation method of magneto-optic crystalline ceramics Download PDFInfo
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Abstract
The invention discloses the nano oxidized terbium of a kind of ALON and be combined the preparation method of magneto-optic crystalline ceramics, with ALON powder as main component, composite Nano terbium oxide, 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 terbium oxide 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 ALON-saturating
The preparation method of bright pottery.
Background technology
Terbium oxide 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 very low, even at the high yttrium the highest containing terbium
In ionic heavy rare earth ore deposit, the content of terbium also only accounts for the 1.1-1.2% of total rare earth (TRE).In the rich europium material of general middle yttrium, the content of terbium exists
0.6-0.8%, as content in total rare earth (TRE) for the content with terbium 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, with electronics and information industry
Fast development, the new function material of terbium base 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 materials.Owing to terbium is rare, so valency
Lattice are expensive, and preparation high-grade terbium is more difficult, therefore, and the highly desirable a kind of method finding preparation cost low of people.
The researchers 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 using method of oxygen catalytic oxidation organic matter, implement in accordance with the following steps: (1) terbium oxide
The preparation method of nano material: add 2.0g terbium oxide (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 the terbium chloride obtaining in 200mL water, with NaOH regulation to pH=7, transfer
In closed reactor, 180 DEG C are heated 12 hours, by the white precipitate washing obtaining, dry, calcine 2 hours at 500 DEG C,
Obtain brown solid, be 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
The reason that cross due to coprecipitation method, the Size Distribution of prepared terbium oxide nano material there is also certain room for improvement.
The researchers such as the Zhang Le of Jiangsu Normal University disclose a kind of magneto-optic terbium oxide in CN201610104880.6
The preparation method of crystalline ceramics.First terbium oxide micro-powder is added to dissolve in nitric acid and form Tb (NO3) 3, be diluted with water to obtain Tb
(NO3) 3 solution；Tb (NO3) 3 solution after again (NH4) 2SO4 being joined dilution obtains mother liquor；Then it is added drop-wise to precipitating reagent
Mother liquor stirs, is 7.5～8.5 to the pH value of mother liquor；Continue stirring, static ageing；The sediment being filtrated to get, by sediment
Rinsing, drying, grinding are sieved, are calcined；Shaping；Vacuum heating-press sintering obtains magneto-optic terbium oxide crystalline ceramics.The present invention be all
Preparing magneto-optic terbium oxide pottery under relatively low sintering temperature, economical and energy saving effect is obvious.Use the method for 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
Under state, well the valence state of control Tb ion 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.
ALON, the abbreviation of aluminum oxynitride, is to study now a lot of crystalline ceramics series；As the Maritime Affairs University Of Dalian exists
CN201210338387.2 discloses a kind of method of batch preparation of pure phase AlON transparent ceramic powder body；But now concerning
The research of the preparation method that the nano oxidized terbium of ALON-is combined magneto-optic crystalline ceramics is less.
Content 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 ALON-and be combined magneto-optic crystalline ceramics
Preparation method, with ALON powder as main component, composite Nano terbium oxide, by batch mixing, sieve, vacuum outgas, flow
Prolonging shaping, binder removal, isostatic cool pressing, sintering, grinding and polishing, obtaining the crystalline ceramics with magneto-optical property, this pottery is transparent
Spending, 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,
Prepared terbium oxide nano particle has the monodispersity in preferable dimensional homogeneity and alcoholic solution.
The nano oxidized terbium of a kind of ALON-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The ALON of 100-160 weight portion, ALON are the ALON powder prepared by carbothermic method, and particle diameter is 2.5 μm；
The nano oxidized terbium of 10-16 weight portion, nano oxidized terbium is the terbium oxide nano particle prepared by following methods, grain
Footpath is 5-50nm；Terbium oxide nano particle is prepared by the hot method of extensive alcohol, including following preparation process:
1) it is added to the phenmethylol of the solubility terbium salt of 10 weight portions and 100-200 weight portion 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) input pre-reaction solution to reative cell, input surfactant to reative cell simultaneously, lazy at 180-210 DEG C
Property atmosphere under reaction 3-5h, obtain reactant liquor；
4) reactant liquor is delivered to separation chamber by condenser pipe, is separated by high speed centrifugation, obtain upper strata phenmethylol and under
The terbium oxide nano particle that layer concentrates；
5) upper strata phenmethylol is delivered to waste reclamation in agitator tank after treatment, the terbium oxide that lower floor concentrates is received
Rice grain is scrubbed, dry, pack, and can obtain terbium oxide nano particle；
(2) ALON powder and nano oxidized terbium are positioned over ball milling in ball mill by batch mixing so that two kinds of raw materials are fully mixed
Closing, ball-milling medium is ethanol；It is subsequently added the PAA ethanol solution of solid gross mass 10-14%, solid gross mass 10-14%
The PEG-1000 ethanol solution of PVA ethanol solution and solid gross mass 10-14%, ball milling 11h subsequently, obtain mixed slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body at 890 DEG C binder removal, carry out isostatic cool pressing process subsequently, obtain the base substrate of uniform compact；
(5) base substrate is sintered under 1650-1800 degree Celsius 1-2 hour, after ground polishing, ALON-can be obtained and receive
Rice terbium oxide is combined magneto-optic crystalline ceramics.
As preferably, described solubility terbium salt be terbium nitrate, terbium chloride, sulfuric acid terbium one or more.
As preferably, step 3) in reaction temperature be 200 DEG C, the reaction time is 4h.
As preferably, described surfactant is oleic acid, polyethylene glycol, one or more in PVP.
As preferably, base substrate is sintered 1.5 hours under 1750 degrees Celsius.
Beneficial effects of the present invention:
(1) ALON and nano oxidized terbium are organically combined by the present invention, and formation inexpensively still can be prepared on a large scale
The nano oxidized terbium of ALON-is combined magneto-optic crystalline ceramics；Due to being combined of ALON so that compound magneto-optic crystalline ceramics is compared to commonly
The light transmittance of single terbium oxide pottery had and be substantially improved, the thick ceramic of 1mm reaches at the light transmittance of visible region
More than 93%, and Verdet constant is also greater than 125rad/ (T m), Verdet constant is to obtain measured by conventional method, by 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 normal temperature air.
(2) preparation method compared to 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 terbium oxide nano is good, and this is for ceramic physical and chemical performance
Having a major impact, the method is simple and practical simultaneously, can prepare on a large scale, and prepared terbium oxide nano particle has preferable chi
Monodispersity in very little homogeneity and alcoholic solution.This also makes the industrialized production of the magneto-optic crystalline ceramics of nano oxidized terbium base
Open another fan window.Meanwhile, in the preparation process of composite ceramics, have employed organic solvent base the tape casting and prepare, benzene
Dispersion in ethanol solution for the nano particle prepared by methyl alcohol is also especially good so that have preferable slurry in casting processes
Homogeneity and dispersiveness, and the addO-on therapy in casting processes is such as subsequently added the PAA ethanol solution of solid gross mass 14%,
The PVA ethanol solution of solid gross mass 14% and the PEG-1000 ethanol solution of solid gross mass 14%, together with raw material so that
Compound magneto-optic pottery can be prepared by the tape casting；And the compactness of pottery and its magneto-optical property are closely bound up, the present invention exists
Flow casting molding, binder removal at 890 DEG C, carry out isostatic cool pressing process subsequently, obtain the base substrate of uniform compact.
(3) present invention is in preparation technology, based on the premise of optimization for function ceramics performance, optimizes preparation work
The nano material of hot for alcohol method is especially combined by skill by alcohol radical the tape casting, then by selecting the suitable raw material that adds, preparation
Obtain high-compactness, highly purified magneto-optic crystalline ceramics.
Brief description
Hereinafter, embodiment of the present invention are described in detail in conjunction with accompanying drawing, wherein:
Fig. 1 is the TEM figure of the terbium oxide 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 ALON-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The ALON of 125 weight portions, ALON are the ALON powder prepared by carbothermic method, and particle diameter is 1.6 μm；
The nano oxidized terbium of 12 weight portions, nano oxidized terbium is the terbium oxide nano particle prepared by following methods, particle diameter
For 10nm；Terbium oxide nano particle is prepared by the hot method of extensive alcohol, including following preparation process:
1) it is added to the solubility terbium salt of 10 weight portions and the phenmethylol of 160 weight portions 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) input pre-reaction solution to reative cell, input surfactant 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 condenser pipe, is separated by high speed centrifugation, obtain upper strata phenmethylol and under
The terbium oxide nano particle that layer concentrates；
5) upper strata phenmethylol is delivered to waste reclamation in agitator tank after treatment, the terbium oxide that lower floor concentrates is received
Rice grain is scrubbed, dry, pack, and can obtain terbium oxide nano particle；
(2) ALON powder and nano oxidized terbium are positioned over ball milling in ball mill by batch mixing so that two kinds of raw materials are fully mixed
Closing, ball-milling medium is ethanol；It is subsequently added the PAA ethanol solution of solid gross mass 10%, the PVA ethanol of solid gross mass 10%
The PEG-1000 ethanol solution of solution and solid gross mass 10%, ball milling 11h subsequently, obtain mixed slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body at 890 DEG C binder removal, 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, ALON-can be obtained nano oxidized
Terbium is combined magneto-optic crystalline ceramics.
Described solubility terbium salt is terbium nitrate.
Described surfactant is oleic acid.
The thick ceramic of 1mm has reached 96.5% at the light transmittance of visible region, and Verdet constant is 129rad/ (T
m)。
Embodiment 2:
The nano oxidized terbium of a kind of ALON-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The ALON of 100 weight portions, ALON are the ALON powder prepared by carbothermic method, and particle diameter is 1.6 μm；
The nano oxidized terbium of 10 weight portions, nano oxidized terbium is the terbium oxide nano particle prepared by following methods, particle diameter
For 10nm；Terbium oxide nano particle is prepared by the hot method of extensive alcohol, including following preparation process:
1) it is added to the solubility terbium salt of 10 weight portions and the phenmethylol of 160 weight portions 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) input pre-reaction solution to reative cell, input surfactant 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 condenser pipe, is separated by high speed centrifugation, obtain upper strata phenmethylol and under
The terbium oxide nano particle that layer concentrates；
5) upper strata phenmethylol is delivered to waste reclamation in agitator tank after treatment, the terbium oxide that lower floor concentrates is received
Rice grain is scrubbed, dry, pack, and can obtain terbium oxide nano particle；
(2) ALON powder and nano oxidized terbium are positioned over ball milling in ball mill by batch mixing so that two kinds of raw materials are fully mixed
Closing, ball-milling medium is ethanol；It is subsequently added the PAA ethanol solution of solid gross mass 10%, the PVA ethanol of solid gross mass 10%
The PEG-1000 ethanol solution of solution and solid gross mass 10%, ball milling 11h subsequently, obtain mixed slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body at 890 DEG C binder removal, 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, ALON-can be obtained nano oxidized
Terbium is combined magneto-optic crystalline ceramics.
Described solubility terbium salt is terbium nitrate.
Described surfactant is oleic acid.
The thick ceramic of 1mm has reached 97.9% at the light transmittance of visible region, and Verdet constant is 138rad/ (T
m)。
Embodiment 3:
The nano oxidized terbium of a kind of ALON-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The ALON of 160 weight portions, ALON are the ALON powder prepared by carbothermic method, and particle diameter is 1.6 μm；
The nano oxidized terbium of 15 weight portions, nano oxidized terbium is the terbium oxide nano particle prepared by following methods, particle diameter
For 10nm；Terbium oxide nano particle is prepared by the hot method of extensive alcohol, including following preparation process:
1) it is added to the solubility terbium salt of 10 weight portions and the phenmethylol of 160 weight portions 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) input pre-reaction solution to reative cell, input surfactant 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 condenser pipe, is separated by high speed centrifugation, obtain upper strata phenmethylol and under
The terbium oxide nano particle that layer concentrates；
5) upper strata phenmethylol is delivered to waste reclamation in agitator tank after treatment, the terbium oxide that lower floor concentrates is received
Rice grain is scrubbed, dry, pack, and can obtain terbium oxide nano particle；
(2) ALON powder and nano oxidized terbium are positioned over ball milling in ball mill by batch mixing so that two kinds of raw materials are fully mixed
Closing, ball-milling medium is ethanol；It is subsequently added the PAA ethanol solution of solid gross mass 10%, the PVA ethanol of solid gross mass 10%
The PEG-1000 ethanol solution of solution and solid gross mass 10%, ball milling 11h subsequently, obtain mixed slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body at 890 DEG C binder removal, 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, ALON-can be obtained nano oxidized
Terbium is combined magneto-optic crystalline ceramics.
Described solubility terbium salt is terbium nitrate.
Described surfactant is oleic acid.
The thick ceramic of 1mm has reached 96.9% at the light transmittance of visible region, and Verdet constant is 133rad/ (T
m)。
Comparative example 1:
The nano oxidized terbium of a kind of ALON-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The ALON of 0 weight portion；
The nano oxidized terbium of 12 weight portions, nano oxidized terbium is the terbium oxide nano particle prepared by following methods, particle diameter
For 10nm；Terbium oxide nano particle is prepared by the hot method of extensive alcohol, including following preparation process:
1) it is added to the solubility terbium salt of 10 weight portions and the phenmethylol of 160 weight portions 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) input pre-reaction solution to reative cell, input surfactant 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 condenser pipe, is separated by high speed centrifugation, obtain upper strata phenmethylol and under
The terbium oxide nano particle that layer concentrates；
5) upper strata phenmethylol is delivered to waste reclamation in agitator tank after treatment, the terbium oxide that lower floor concentrates is received
Rice grain is scrubbed, dry, pack, and can obtain terbium oxide nano particle；
(2) nano oxidized terbium is positioned over ball milling in ball mill by batch mixing 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 11h subsequently, obtain mixed slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body at 890 DEG C binder removal, 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, ALON-can be obtained nano oxidized
Terbium is combined magneto-optic crystalline ceramics.
Described solubility terbium salt is terbium nitrate.
Described surfactant is oleic acid.
The thick ceramic of 1mm has reached 84% at the light transmittance of visible region, and Verdet constant is 133rad/ (T
m)。
Comparative example 2:
The nano oxidized terbium of a kind of ALON-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The ALON of 125 weight portions, ALON are the ALON powder prepared by carbothermic method, and particle diameter is 1.6 μm；
The nano oxidized terbium of 12 weight portions, nano oxidized terbium is the terbium oxide nano particle prepared by following methods, particle diameter
For 10nm；Terbium oxide nano particle coprecipitation prepares gained；
(2) ALON powder and nano oxidized terbium are positioned over ball milling in ball mill by batch mixing so that two kinds of raw materials are fully mixed
Closing, ball-milling medium is ethanol；It is subsequently added the PAA ethanol solution of solid gross mass 10%, the PVA ethanol of solid gross mass 10%
The PEG-1000 ethanol solution of solution and solid gross mass 10%, ball milling 11h subsequently, obtain mixed slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body at 890 DEG C binder removal, 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, ALON-can be obtained nano oxidized
Terbium is combined magneto-optic crystalline ceramics.
The thick ceramic of 1mm has reached 90.1% at the light transmittance of visible region, 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 without departing substantially from the spirit or essential attributes of the present invention, the present invention can be realized 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 not each embodiment only wraps
Containing an independent technical scheme, this narrating mode of specification is only that for clarity sake those skilled in the art should
Using specification as an entirety, the technical scheme in each embodiment also can form those skilled in the art through appropriately combined
May be appreciated other embodiments.
Claims (5)
1. the nano oxidized terbium of an ALON-is combined the preparation method of magneto-optic crystalline ceramics: it is characterized in that:
(1) get the raw materials ready:
The ALON of 100-160 weight portion, ALON are the ALON powder prepared by carbothermic method, and particle diameter is 2.5 μm；
The nano oxidized terbium of 10-16 weight portion, nano oxidized terbium is the terbium oxide nano particle prepared by following methods, and particle diameter is
5-50nm；Terbium oxide nano particle is prepared by the hot method of extensive alcohol, including following preparation process:
1) it is added to the phenmethylol of the solubility terbium salt of 10 weight portions and 100-200 weight portion in agitator tank, machine at 40-50 DEG C
Tool stirs 30-60min 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) input pre-reaction solution to reative cell, input surfactant 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 condenser pipe, is separated by high speed centrifugation, obtain upper strata phenmethylol and lower floor is dense
The terbium oxide nano particle of contracting；
5) upper strata phenmethylol is delivered to waste reclamation in agitator tank after treatment, the terbium oxide nanometer that lower floor is concentrated
Grain scrubbed, dry, pack, terbium oxide nano particle can be obtained；
(2) ALON powder and nano oxidized terbium are positioned over ball milling in ball mill by batch mixing so that two kinds of raw materials are sufficiently mixed, ball
Grinding media is ethanol；It is subsequently added the PAA ethanol solution of solid gross mass 10-14%, the PVA second of solid gross mass 10-14%
The PEG-1000 ethanol solution of alcoholic solution and solid gross mass 10-14%, ball milling 11h subsequently, obtain mixed slurry；
(3) mixed slurry sieved, vacuum outgas, carry out flow casting molding；
(4) by flow casting molding body at 890 DEG C binder removal, carry out isostatic cool pressing process subsequently, obtain the base substrate of uniform compact；
(5) base substrate is sintered under 1650-1800 degree Celsius 1-2 hour, after ground polishing, ALON-nano oxygen can be obtained
Change terbium and be combined magneto-optic crystalline ceramics.
2. the nano oxidized terbium of ALON-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, terbium chloride, sulfuric acid terbium one or more.
3. the nano oxidized terbium of ALON-as claimed in claim 1 is combined a preparation method for magneto-optic crystalline ceramics, and its feature exists
In step 3) in reaction temperature be 200 DEG C, the reaction time is 4h.
4. the nano oxidized terbium of ALON-as claimed in claim 1 is combined a preparation method for magneto-optic crystalline ceramics, and its feature exists
It is oleic acid, polyethylene glycol, one or more in PVP in: described surfactant.
5. the nano oxidized terbium of ALON-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 1750 degrees Celsius.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109516813A (en) * | 2019-01-08 | 2019-03-26 | 大连海事大学 | A kind of method that direct water injection forming prepares high light transmittance AlON crystalline ceramics |
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