CN105218097B - A kind of preparation method of nuclear reactor watch window crystalline ceramics - Google Patents
A kind of preparation method of nuclear reactor watch window crystalline ceramics Download PDFInfo
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- CN105218097B CN105218097B CN201510712301.1A CN201510712301A CN105218097B CN 105218097 B CN105218097 B CN 105218097B CN 201510712301 A CN201510712301 A CN 201510712301A CN 105218097 B CN105218097 B CN 105218097B
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Abstract
The present invention relates to a kind of preparation method of nuclear reactor watch window crystalline ceramics.This method includes:(1) by yttrium nitrate and yttrium acetate in molar ratio 1:(0.4~0.6) added water after mixing, the precursor solution of obtained clarification is placed in micro-wave oven, heat 5 25min;Through boiling, evaporation, self-propagating combustion, 10~35nm of particle diameter Y is obtained2O3Nano-powder;(2) by obtained Y2O3Nano-powder ball milling, drying, dry-pressing formed, Vacuum Package, isostatic cool pressing, obtain Y2O3Ceramic body, then by Y2O3Ceramic body is placed in 1300~1500 DEG C of sintering in microwave agglomerating furnace, produces.The inventive method firing rate is fast, the time is short, can make ceramic densifying rapidly in atmospheric conditions, and the ceramics of preparation can be used as nuclear reactor watch window material.
Description
Technical field
The present invention relates to a kind of preparation method of nuclear reactor watch window crystalline ceramics, and in particular to a kind of consistency
The good Y of high, light transmission2O3The preparation method of crystalline ceramics, belongs to field of inorganic nonmetallic material.
Background technology
Yttrium oxide transparent ceramic has fusing point height, good chemical and photochemical stability, transparent optical region field width, thermal conductivity high
The advantages of, there is preferable transmitance in 0.23~8.0 mu m waveband, be a kind of excellent high-temperature infrared material, electronic material and
Refractory material, has important application value in industries such as high temperature window, infrared acquisition, luminescence medium, semiconductors.
Coprecipitation synthesis Y is used in the prior art2O3Nano-powder, the vacuum-sintering 4h at 1700 DEG C, can be obtained
To yttrium oxide transparent ceramic;Referring to Lin Wen etc., Synthesis of yttria nanopowders for
transparent yttria ceramics.Optical Materials,2006,29(2):239-245.This method later stage
1700 DEG C of high-temperature calcinations are handled so that longer the time required to preparing powder, and equipment investment is big, and energy waste is big, low production efficiency.
Chinese patent document CN1594208A provides the sintering method of a yttrium oxide base transparent ceramic, using ammoniacal liquor and
The mixed solution of ammonium hydrogen carbonate is precipitating reagent, and the yttria-base powder of high sintering activity is prepared using coprecipitation technology, will be above-mentioned
Pressureless sintering of the powder after shaping under the conditions of the nitrogen atmosphere of flowing obtains transparent yttria-base ceramic material.What is obtained is saturating
Bright material reaches more than 70% in the transmitance of visible region (470nm-800nm), and near infrared region, (800nm-2500nm) reaches
To more than 76%.Rare earth ion doped sample has strong luminous under the irradiation of ultraviolet light and X-ray, can be used as transparent flickering
Ceramics, transparent laser ceramic and optical window material.This method is also to be sintered under 1700-1900 DEG C of high temperature, agglomerating plant
It is expensive.Yao G etc. use solution synthesis by self-combustion Eu:Y2O3Nano-powder, saves the energy;Referring to Eu:Y2O3nano-
phosphor prepared by novel energy-saving solution combustion method.Jour nal
of Alloys and Compounds,2008,462(1):381-385。
The above method comes with some shortcomings, for example:During synthetic powder, prepared using chemical coprecipitation process
High-temperature calcination processing (~1100 DEG C) is carried out after presoma, longer the time required to preparing powder, energy waste is big, production efficiency
It is low;Ordinary combustion synthetic reaction uses Electric heating, and material is heated uneven, causes final product local grain roughening occur
With crystal grain it is inter-adhesive, reunite etc. phenomenon.For another example:In sintering process, temperature needed for traditional vacuum sintering or normal atmosphere sintering
Degree is in 1700 DEG C of even more highs, and this requires that equipment investment is big, and energy demand is more, and production cost is high, and time-consuming.
At present, main nuclear reactor watch window material is lead glass, but lead glass fragility is big, resistance to elevated temperatures
Difference, and lead element can cause environmental pollution.Yttrium oxide transparent ceramic has higher mechanical strength and hardness, thermal shock resistance
And resistance to chemical corrosion, it is expected to be used as reactor watch window material.But nuclear reactor watch window material needs ceramic dense
Degree is high, transparency is good, the Y of prior art report2O3The method of nano-powder and crystalline ceramics sintering, products obtained therefrom can not be met
The special requirement of nuclear reactor watch window material.The present invention is proposed for this.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of preparation side of nuclear reactor watch window crystalline ceramics
Method.Products obtained therefrom is that consistency is high, light transmission is good, transparent yttria ceramics with certain neutron absorption capability.
Technical solution of the present invention is as follows:
A kind of preparation method of nuclear reactor watch window crystalline ceramics, comprises the following steps:
(1) Y is synthesized2O3Nano-powder:
By yttrium nitrate and yttrium acetate in molar ratio 1:(0.4~0.6) mix, obtain binary material system;
Add water into above-mentioned binary material system, the mass ratio of the binary material system total amount and water is 1:(2~
4), it is sufficiently stirred under 20~80 DEG C of constant temperatures, until forming the precursor solution of clarification;
The precursor solution of obtained clarification is placed in the micro-wave oven that frequency is 2.45GHz, in the constant work(of 200-1000W
5-25min is heated under rate;Through boiling, evaporation, self-propagating combustion, 10~35nm of particle diameter Y is obtained2O3Nano-powder;
(2) yttrium oxide transparent ceramic is prepared:
By Y made from step (1)2O3Nano-powder ball milling, drying, dry-pressing formed, Vacuum Package, isostatic cool pressing, are obtained
Y2O3Ceramic body, then by Y2O3Ceramic body is placed in microwave agglomerating furnace and sintered, 5~20 DEG C/min of heating rate, sintering temperature
1300~1500 DEG C of degree, 30~120min of soaking time.
Yttrium oxide transparent ceramic consistency produced by the present invention is in 4.7g/cm3More than;It is preferred that yttrium oxide transparent ceramic is fine and close
Spend for 4.7~5g/cm3。
According to the present invention, in the binary material system described in step (1), it is preferred that mole of yttrium nitrate and yttrium acetate
Than for 1:(0.45~0.55).
According to currently preferred, in step (1), after the precursor solution of clarification is formed, continue constant temperature stirring 1-3 small
When;Ensure that composition is uniform.
According to currently preferred, in step (1), the precursor solution is mounted in corundum crucible.Because step (1) is micro-
The maximum temperature that ripple induction spontaneous combustion reaches is at 550 DEG C or so, and corundum crucible refractoriness is high, good thermal shock, it can be ensured that peace
Entirely.
Y prepared by step (1) of the present invention2O3Particle diameter of nanometer powder is in the range of 15~25nm.
Heretofore described yttrium nitrate is six nitric hydrate yttriums;Described yttrium acetate is four acetate hydrate yttriums, also known as four
It is hydrated acetic acid yttrium;Purity is 99.99%.Described water is deionized water.
According to the present invention, Y described in step (2)2O3Nano-powder ball milling condition is preferred:Medium is deionized water or anhydrous
Ethanol, ball is 1~3mm of diameter ZrO2Ball;Wherein, further preferably, ball:Y2O3Nano-powder:The mass ratio of medium is (15
~25):1:(4~5), Ball-milling Time is 1h~3h.
According to currently preferred, dry and carried out in drying box described in step (2), drying temperature is 40~80 DEG C,
Drying time is 20~40h.
It is dry-pressing formed described in step (2) to be according to currently preferred:Dried powder is placed in mould, it is single
Axle applies 20~30MPa of pressure, is pressed into a diameter of 10~30mm, and thickness is 2~5mm disk;
According to currently preferred, the pressure of isostatic cool pressing described in step (2) is 180~240MPa, keeps pressure
Time is 120~180s.
According to currently preferred, the microwave source tranmitting frequency of microwave agglomerating furnace described in step (2) be 2.45GHz ±
50MH。
The Y that present invention sintering is obtained2O3Crystalline ceramics consistency is up to 4.96g/cm3, relative density is up to 99%.Meet
The requirement of nuclear reactor watch window material, available for making nuclear reactor watch window.
Because yittrium oxide has certain neutron absorption capability and shielding property, yttrium oxide transparent ceramic removes known applications
Outside, it is alternatively arranged as nuclear reactor watch window material.Want to obtain the transparent yttria ceramics that consistency is high, light transmission is good,
There are two essential processes:One is with the small Y of purity height, granularity2O3Powder is used as raw material;Two be sintering process densification.
For existing synthesis Y2O3The deficiency of powder technology, the present invention is by oxidant of yttrium nitrate, yttrium acetate is reducing agent, using microwave
Inducing combustion method synthesizes nano yttrium oxide powder, and particle diameter is less than 30 nanometers, and powder even size distribution is made pottery as yttrium oxide transparent
The raw material of porcelain;Step (2) of the present invention prepares yttrium oxide transparent ceramic using microwave sintering method, and this method technique is simple, be produced into
This low, short preparation period, the ceramic dense degree sintered out is high.Nuclear reactor watch window material can be used as.
Beneficial effects of the present invention:
1st, Y is prepared in the present invention2O3Microwave induced combustion synthesis method is used during powder, directly precursor solution is carried out micro-
Wave heating, without gel process, technique is simple, aggregate velocity is fast, production cost is low;
According to propulsion chemical theory (i.e. total oxidation valency principle equal with total also original cost), the chemical combination of yttrium nitrate and yttrium acetate
Valency is respectively -15 ,+24, therefore, and the mol ratio of yttrium nitrate and yttrium acetate is 24 in theory:15, i.e., 1:0.625.But, this hair
A person of good sense has been surprisingly found that the ratio of appropriate reduction reducing agent limits the mol ratio of yttrium nitrate and yttrium acetate as 1:After (0.4~0.6),
Combustion reaction is more abundant, is more beneficial for the generation of reaction, and obtained product purity is higher, and dispersiveness is more preferably.
2nd, present invention sintering Y2O3Microwave heating, compared with traditional sintering processing, microwave sintering are used when ceramic
Firing rate is fast, the time is short, can make ceramic densifying rapidly in atmospheric conditions, prevents crystal grain from growing up.
3rd, in the present invention prepared by powder and sintering process uses microwave technology, compared with conventional sintering mode, sintering temperature
Degree is substantially reduced, and reduces energy consumption, environmental protection.
Brief description of the drawings
Fig. 1 is the Y obtained by the step of embodiment 1 (1)2O3The X ray diffracting spectrum of powder;Abscissa is 2 θ (°), indulges and sits
Mark is intensity (arbitrary unit).
Fig. 2 is the Y obtained by the step of embodiment 1 (1)2O3The scanning electron microscope image of powder.
Fig. 3 is Y prepared by embodiment 12O3The X ray diffracting spectrum of crystalline ceramics;Abscissa is 2 θ (°), and ordinate is strong
Spend (arbitrary unit).
Fig. 4 is the Y prepared by embodiment 12O3The sample surfaces scanning electron microscope image of crystalline ceramics.
Fig. 5 is the Y prepared by embodiment 12O3The strong light of crystalline ceramics sample passes through photo.
Embodiment
Technical scheme is described further with reference to embodiment, but institute's protection domain of the present invention is not limited to
This.
Raw material explanation:
Six nitric hydrate yttriums in embodiment:Purity 99.99%, four acetate hydrate yttriums:Purity 99.99%;The thin promise in Nanjing
Chemical Industry Science Co., Ltd is on sale.
Y2O3The density of ceramic material is tested with Archimedes's drainage, and step is as follows:
1. testing sample is placed in 50 DEG C of baking ovens and dried after 24h, in weighing testing sample at room temperature on assay balance
Dry weight (W1), it is accurate to 0.001g;
2. the testing sample after 1. step is weighed, which is put into boiling water, boils 2h, after room temperature is cooled to, and weighs saturation and treats
Buoyant weight (W of the test sample product in water2), it is accurate to 0.001g;
3. the testing sample after 2. step is weighed takes out from water, is gently wiped the unnecessary moisture of surface of test piece with gauze
It is rapid to weigh the aerial weight in wet base (W of saturation testing sample after falling3), it is accurate to 0.001g;
4. repeat above steps and take average 3 times, then according to formula:ρ=W1/(W3-W2) calculate testing sample volume
Density.
Y2O3The phase structure of powder and ceramics is by X-ray diffraction (XRD) atlas analysis, and diameter of particle passes through Scherrer formula
Estimation.
Embodiment 1:A kind of Y2O3The preparation method of crystalline ceramics, step is as follows:
(1) the nitric hydrate yttriums of 47.88g six, the acetate hydrate yttriums of 19.12g tetra- are weighed, mol ratio is 1:0.45, mix, add
250g deionized waters, the stirring at 70 DEG C are until form the precursor solution of clarification, and continuation afterwards stirs 1 hour to ensure solution
Middle composition is uniform;
The precursor solution of obtained clarification is weighed into 30g in corundum crucible, the microwave that frequency is 2.45GHz is placed in
In stove, 15min is heated under 300W power, through solution fast boiling, evaporation and self-propagating combustion, obtaining average grain diameter is
17.2nm Y2O3Powder;
(2) gained nano-powder 10g, ZrO in step (1) is weighed2Ball 200g, absolute ethyl alcohol 45g, are placed in ball grinder,
Ball grinder is placed in planetary ball mill, with 200r/min speed ball milling 2h;
The slurry that ball milling is obtained is placed in 50 DEG C of drying bakers and dried after 24h, grinding, takes 3g to be placed in mould, applies 30MPa
Pressure, pressurize 1min obtains diameter 30mm disk.By disk under 200MPa pressure isostatic cool pressing, pressurize 3min, obtain
Y2O3Green compact;By obtained Y2O3Green compact are placed in the furnace chamber of microwave agglomerating furnace, and programming rate is about 12 DEG C/min, when temperature reaches
During to 1400 DEG C, 2h is incubated, microwave source is then shut off, normal temperature is cooled to air, Y is made2O3Crystalline ceramics.
Y obtained by the present embodiment step (1)2The principal crystalline phase of O ground rice bodies is cube Y2O3Phase, as shown in figure 1, according to thanking
The average grain diameter of happy formula estimation is 17.2nm.The Y of gained2O3The electron scanning micrograph of nano-powder as shown in Fig. 2
There is slight agglomeration, slight reunion can increase powder active, improve sintering character.
The finally obtained Y of the present embodiment2O3Crystalline ceramics principal crystalline phase is cube Y2O3Phase, such as Fig. 3.By Archimedes method
Measure Y2O3Ceramic density is 4.96g/cm3, relative density is 99%.
Y prepared by the present embodiment2O3Sample surfaces scanning electron microscope image such as Fig. 4 of ceramics, ceramic average crystal grain
Size is 1 μm, and crystal grain distribution is uniform, and intercrystalline is without visible stomata, and the ceramic dense of preparation is preferable.
Embodiment 2:One kind prepares Y2O3The method of crystalline ceramics, step is as follows:
(1) the nitric hydrate yttriums of 47.88g six, the acetate hydrate yttriums of 21.13g tetra- are weighed, mol ratio is 1:0.5, mix, add
200g deionized waters, the stirring at 50 DEG C are until form the precursor solution of clarification, and continuation afterwards stirs 2 hours to ensure solution
Middle composition is uniform;
The precursor solution of obtained clarification is weighed into 20g in corundum crucible, the microwave that frequency is 2.45GHz is placed in
In stove, 10min is heated under 400W power, through solution fast boiling, evaporation and self-propagating combustion, average grain diameter is obtained for 20nm
Y2O3Powder;
(2) gained Y in step (1) is weighed2O3Powder 10g, ZrO2Ball 160g, absolute ethyl alcohol 40g, are placed in ball grinder, will
Ball grinder is placed in planetary ball mill, with 200r/min speed ball milling 3h;Slurry is placed in 40 DEG C of drying bakers and dries 30h
Afterwards, grind, take 3g to be placed in mould, apply 30Mpa pressure, pressurize 1min obtains diameter 30mm disk.Disk is existed
Isostatic cool pressing under 180Mpa pressure, pressurize 3min, obtains Y2O3Green compact;
By above-mentioned Y2O3Green compact are placed in the furnace chamber of microwave agglomerating furnace, and programming rate is about 16 DEG C/min, when temperature reaches
At 1450 DEG C, 1h is incubated, microwave source is then shut off, normal temperature is cooled to air, Y is made2O3Crystalline ceramics.After testing, it is prepared
Sintering after gained Y2O3Crystalline ceramics density is 4.92g/cm3, relative density is 98%.
Embodiment 3:One kind prepares Y2O3The method of crystalline ceramics, step is as follows:
(1) the nitric hydrate yttriums of 47.88g six, the acetate hydrate yttriums of 23.25g tetra- are weighed, mol ratio is 1:0.55, mix, add
230g deionized waters, at 50 DEG C stirring until formed clarification precursor solution, afterwards continue stir 1.5 hours it is molten to ensure
Composition is uniform in liquid;
The precursor solution of obtained clarification is weighed into 25g in corundum crucible, the microwave that frequency is 2.45GHz is placed in
In stove, 15min is heated under 4500W power, through solution fast boiling, evaporation and self-propagating combustion, Y is obtained2O3Nano-powder;
(2) gained Y in step (1) is weighed2O3Nano-powder 10g, ZrO2Ball 220g, absolute ethyl alcohol 50g, are placed in ball grinder
In, ball grinder is placed in planetary ball mill, with 200r/min speed ball milling 1h;Gained slurry is placed in 60 DEG C of drying bakers and done
After dry 20h, grinding takes 3g to be placed in mould, applies 20Mpa pressure, and pressurize 1min obtains diameter 30mm disk.By disk
The isostatic cool pressing under 200Mpa pressure, pressurize 2min, obtains Y2O3Green compact;
By Y2O3Green compact are placed in the furnace chamber of microwave agglomerating furnace, and programming rate is about 14 DEG C/min, when temperature reaches 1350 DEG C
When, 2h is incubated, microwave source is then shut off, normal temperature is cooled to air, Y is made2O3Crystalline ceramics.After testing, prepared Y2O3
The average grain diameter of nano-powder is 25nm, and gained ceramic density is 4.73g/cm after sintering3, relative density is 94.4%.
Embodiment 4:
(1) the nitric hydrate yttriums of 47.88g six, the acetate hydrate yttriums of 22g tetra- are weighed, mol ratio is 1:0.52, mix, add
150g deionized waters, the stirring at 80 DEG C are until form the precursor solution of clarification, and continuation afterwards stirs 1 hour so that in solution
Composition is uniform;The precursor solution of obtained clarification is weighed into 35g in corundum crucible, it is the micro- of 2.45GHz to be placed in frequency
In ripple stove, 18min is heated under 300W power, through solution fast boiling, evaporation and self-propagating combustion, Y is obtained2O3Nano-powder;
(2) gained Y in step (1) is weighed2O3Nano-powder 10g, ZrO2Ball 180g, absolute ethyl alcohol 40g, are placed in ball grinder
In, ball grinder is placed in planetary ball mill, with 200r/min speed ball milling 3h;Gained slurry is placed in 45 DEG C of drying bakers and done
After dry 24h, grinding takes 3.5g to be placed in mould, applies 30Mpa pressure, and pressurize 1min obtains diameter 30mm disk.Will circle
Piece isostatic cool pressing under 240Mpa pressure, pressurize 2min obtains Y2O3Green compact;By gained Y2O3Green compact are placed in microwave agglomerating furnace
In furnace chamber, programming rate is about 15 DEG C/min, when temperature reaches 1500 DEG C, is incubated 2h, is then shut off microwave source, cold with air
But to normal temperature, Y is made2O3Crystalline ceramics.After testing, prepared Y2O3The average grain diameter of nano-powder is institute after 23nm, sintering
It is 4.75g/cm to obtain ceramic density3, relative density is 94.8%.
It should be noted that listed above is only several specific embodiments of the invention, it is clear that the present invention is not only
It is limited to above example, there can also be other deformations.Those skilled in the art directly exported from the disclosure of invention or
All deformations of amplification are connect, protection scope of the present invention is considered as.
Claims (9)
1. a kind of preparation method of nuclear reactor watch window crystalline ceramics, comprises the following steps:
(1)Synthesize Y2O3Nano-powder:
By yttrium nitrate and yttrium acetate in molar ratio 1:(0.4 ~ 0.6) mix, obtain binary material system;
Add water into above-mentioned binary material system, the mass ratio of the binary material system total amount and water is 1:(2 ~ 4), 20
It is sufficiently stirred under ~ 80 DEG C of constant temperatures, until forming the precursor solution of clarification;
The precursor solution of obtained clarification is placed in the micro-wave oven that frequency is 2.45GHz, under 200-1000W firm powers
Heat 5-25min;Through boiling, evaporation, self-propagating combustion, 15 ~ 25nm of particle diameter Y is obtained2O3Nano-powder;
(2)Prepare yttrium oxide transparent ceramic:
By step(1)Obtained Y2O3Nano-powder ball milling, drying, dry-pressing formed, Vacuum Package, isostatic cool pressing, obtain Y2O3Pottery
Porcelain base substrate, then by Y2O3Ceramic body is placed in microwave agglomerating furnace and sintered, 5 ~ 20 DEG C/min of heating rate, and sintering temperature 1300 ~
1500 DEG C, 30 ~ 120min of soaking time;
Gained yttrium oxide transparent ceramic consistency is 4.7 ~ 5 g/cm3, for making nuclear reactor watch window.
2. the preparation method of nuclear reactor watch window crystalline ceramics as claimed in claim 1, it is characterised in that step(1)
In described binary material system, the mol ratio of yttrium nitrate and yttrium acetate is 1:(0.45~0.55).
3. the preparation method of nuclear reactor watch window crystalline ceramics as claimed in claim 1, it is characterised in that step(1)
In, after the precursor solution of clarification is formed, continue constant temperature and stir 1-3 hours.
4. the preparation method of nuclear reactor watch window crystalline ceramics as claimed in claim 1, it is characterised in that step(1)
In, the precursor solution is mounted in corundum crucible.
5. the preparation method of nuclear reactor watch window crystalline ceramics as claimed in claim 1, it is characterised in that step(2)
Described in Y2O3Nano-powder ball milling condition is:Medium is deionized water or absolute ethyl alcohol, and ball is 1 ~ 3mm of diameter ZrO2Ball;Its
In, ball:Y2O3Nano-powder:The mass ratio of medium is(15~25):1:(4~5), Ball-milling Time is 1h ~ 3h.
6. the preparation method of nuclear reactor watch window crystalline ceramics as claimed in claim 1, it is characterised in that step(2)
Described in drying temperature be 40 ~ 80 DEG C, drying time be 20 ~ 40h.
7. the preparation method of nuclear reactor watch window crystalline ceramics as claimed in claim 1, it is characterised in that step(2)
Described in dry-pressing formed be:Dried powder is placed in mould, single shaft applies 20 ~ 30MPa of pressure, is pressed into a diameter of 10
~ 30mm, thickness is 2 ~ 5mm disk.
8. the preparation method of nuclear reactor watch window crystalline ceramics as claimed in claim 1, it is characterised in that step(2)
Described in isostatic cool pressing pressure be 180 ~ 240MPa, keep pressure time be 120 ~ 180s.
9. a kind of preparation method of nuclear reactor watch window crystalline ceramics, it is characterised in that step is as follows:
(1)The nitric hydrate yttriums of 47.88g six, the acetate hydrate yttriums of 19.12g tetra- are weighed, mol ratio is 1:0.45, mixing adds 250g
Deionized water, at 70 DEG C stirring until formed clarification precursor solution, afterwards continue stir 1 hour with ensure in solution into
Divide uniform;
The precursor solution of obtained clarification is weighed into 30g in corundum crucible, the micro-wave oven that frequency is 2.45GHz is placed in
In, 15min is heated under 300W power, through solution fast boiling, evaporation and self-propagating combustion, average grain diameter is obtained for 17.2nm
Y2O3Powder;
(2) step is weighed(1)Middle gained nano-powder 10g, ZrO2Ball 200g, absolute ethyl alcohol 45g, are placed in ball grinder, by ball
Grinding jar is placed in planetary ball mill, with 200r/min speed ball milling 2h;
The slurry that ball milling is obtained is placed in 50 DEG C of drying bakers and dried after 24h, grinding, takes 3g to be placed in mould, applies 30MPa pressures
Power, pressurize 1min obtains diameter 30mm disk, by disk under 200MPa pressure isostatic cool pressing, pressurize 3min, obtain Y2O3
Green compact;By obtained Y2O3Green compact are placed in the furnace chamber of microwave agglomerating furnace, and programming rate is about 12 DEG C/min, when temperature reaches
At 1400 DEG C, 2h is incubated, microwave source is then shut off, normal temperature is cooled to air, Y is made2O3Crystalline ceramics.
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