CN110054490A - A method of YAG crystalline ceramics is prepared using core-shell structured powder - Google Patents
A method of YAG crystalline ceramics is prepared using core-shell structured powder Download PDFInfo
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Abstract
The invention discloses a kind of method for preparing YAG crystalline ceramics using core-shell structured powder, specific steps are as follows: by Y (NO3)3Solution is added to Al2O3In suspension, precipitating reagent is urea, and the stoichiometric ratio that ionic weight meets Y:Al=3:5 is added, and reaction temperature is 50-80 DEG C；Urea adjusts slurry pH=8.8-9.1, solid content 35-60vol.%；Slurry directly filters, and arrives core-shell structured powder without washing；Powder freeze-day with constant temperature, and by the powder calcination after drying；It is dry by calcined powder ball milling, sieving；Biscuit, is then placed in Muffle furnace and calcines by cold isostatic compaction after first dry-pressing；Biscuit of ceramics vacuum-sintering；Annealing, grinding and polishing obtain YAG crystalline ceramics.The present invention prepares core-shell structure precursor powder using the precipitation method+without mode of washing, and without discarding ion in product, powder yield is high, purity is high, and partial size is tiny；Preparation process is simple to operation, and sintering temperature is low, at low cost.
Description
Technical field
The invention belongs to field of ceramic preparation technology, are related to the preparation of YAG crystalline ceramics, and in particular to a kind of to use nucleocapsid
The method that structure powder prepares YAG crystalline ceramics.
Background technique
Crystalline ceramics is since the 1960s occurs, with its high temperature resistant, corrosion-resistant, excellent mechanics and optical property
The advantages that, it is widely used in the Scientific And Technicals such as laser, illumination, medical instrument, military affairs and national defence field.Currently, various transparent
Ceramic material emerges one after another, such as YAG, sesquichloride, spinelle, fluoride system, obtains in many key areas
Obtain Preliminary Applications.In existing all transparent ceramic materials, YAG crystalline ceramics is with its easily prepared and good physical chemistry
The advantages such as performance have become the focus and emphasis of transparent ceramic material research field.
Currently, prepared by the main YAG material powder by vacuum-sintering high activity of high quality YAG crystalline ceramics；Make
The temperature of vacuum-sintering can just obtain the YAG crystalline ceramics of high quality, to vacuum-sintering equipment generally at 1760 DEG C or more
It is more demanding.Therefore, it in order to further decrease sintering temperature, needs using the higher YAG powder of activity as raw material.Currently, high living
The YAG material powder of property is mainly prepared by coprecipitation.
During coprecipitation prepares high activity YAG material powder, need to wash aqueous precursor gel repeatedly,
To remove extra discarded ion, impurity and other by-products, cause presoma partial size larger, activity is lower；It needs 1000
DEG C or more carry out high-temperature calcination processing, can just obtain the YAG material powder of high-purity.In addition, the YAG that this method is prepared is former
Feed powder body yield is lower, complex process, at high cost, is insufficient for industrialization production demand.
Summary of the invention
The object of the present invention is to provide a kind of methods for preparing YAG crystalline ceramics using core-shell structured powder.
To achieve the above object, The technical solution adopted by the invention is as follows: it is a kind of saturating using core-shell structured powder preparation YAG
The method of bright ceramics, specific steps are as follows:
(1) by the Y (NO of 0.5-0.8mol/L3)3Solution is added to Al with the speed of 0.5-3ml/min2O3In suspension,
Precipitating reagent is urea, and the stoichiometric ratio that ionic weight meets Y:Al=3:5 is added, and reaction temperature is 50-80 DEG C；
(2) urea that step (1) uses is added to Al as pH adjusting agent2O3In slurry, slurry pH=8.8- is kept
9.1, solid content 35-60vol.%；
(3) step (2) resulting slurry is directly filtered, arrives core-shell structured powder without washing；
(4) by the resulting core-shell structured powder freeze-day with constant temperature of step (3), and the powder after drying is forged in 300-500 DEG C
Burn 1-2h；
(5) alkaline solution of sintering aid and pH=7-12, ball milling mixing 6-16h are added into calcined powder；It will
Slurry freeze-day with constant temperature after ball milling, and the powder after drying is sieved；
(6) powder after step (5) sieving is placed in mold, cold isostatic compaction after first dry-pressing then sets biscuit
In Muffle furnace, in 300-500 DEG C of calcining 2-15h；
(7) step (6) calcined biscuit of ceramics is placed in vacuum sintering furnace, in 1680 DEG C of -1700 DEG C of vacuum-sinterings
4-10h；
(8) ceramics sample of above-mentioned vacuum-sintering is placed in air atmosphere or oxygen atmosphere in 800-1350 DEG C of annealing 2-
10h, the YAG ceramics after annealing are polished directly, and obtain YAG crystalline ceramics.
Preferably, in step (4), the temperature of freeze-day with constant temperature is 100-120 DEG C, time 12-24h.
Preferably, in step (5), the temperature of freeze-day with constant temperature is 55-75 DEG C, time 12-24h.
Preferably, in step (5), the mesh diameter of the sieving is 80-200 mesh.
Preferably, in step (6), the pressure of the dry-pressing is 2-6MPa, pressure maintaining 1-60s；The pressure of the isostatic cool pressing
For 150-250MPa, the cold equal times are 3-8min.
Preferably, in step (5), the revolving speed of the ball milling is 155-185r/min.
Preferably, in step (5), the sintering aid be one of silica, magnesia, calcium oxide or a variety of,
The alkaline solution is one of ammonium hydrogen carbonate, ammonium carbonate, urea, ammonium hydroxide or a variety of.
The present invention is first by yttrium oxide (Y2O3) presoma electroprecipitation is in aluminium oxide (Al2O3) powder surface, form core-shell structure
Presoma powder, and this sediment presoma without washing, it is subsequent directly to prepare crystalline ceramics.
Compared with prior art, the invention has the following beneficial effects:
1. the present invention prepares YAG precursor powder using no mode of washing, nothing discards ion in product, and powder yield is high, pure
Degree is high, and partial size is tiny；Preparation process is simple to operation, at low cost.
2. the present invention is using the core-shell structure precursor powder of precipitation method preparation, preparation process is simple, treatment temperature 300-
500 DEG C are significantly lower than current powder pretreatment temperature, and powdery components are uniform, meet stoichiometric ratio.
3. the present invention is prepared high-quality under low sintering temperature using vacuum sintering technique preparation YAG crystalline ceramics
Amount crystalline ceramics, 1680-1700 DEG C, hence it is evident that be lower than current firing temperature.
4. the present invention realizes the preparation of high quality YAG crystalline ceramics, preparation process is not necessarily to without atmosphere auxiliary and sintering process
Expensive pressure sintering equipment, it is economical and energy saving, environmental-friendly.
5. process flow is simple, short preparation period, cost requirement is advantageously reduced, realizes Technique Popularizing and business promotion.
Detailed description of the invention
Fig. 1 is the XRD spectrum according to the YAG crystalline ceramics of the preparation of embodiment 1,2,3,4；
Fig. 2 is the photo in kind according to the YAG crystalline ceramics of the preparation of embodiment 1,2,3,4；
Fig. 3 is schemed according to the surface SEM of the YAG crystalline ceramics of the preparation of embodiment 1,2,3,4；
Fig. 4 is the transmittance curve according to the YAG crystalline ceramics of the preparation of embodiment 1,2,3,4；
Fig. 5 is the pictorial diagram of the YAG crystalline ceramics of comparative example preparation；
Fig. 6 is the transmittance curve of the YAG crystalline ceramics of comparative example preparation.
Specific embodiment
Invention is further described in detail in the following with reference to the drawings and specific embodiments.
Embodiment 1
(1) by the Y (NO of 0.5mol/L3)3Solution is added to Al with the speed of 0.5ml/min2O3In suspension, precipitating reagent
For urea, the stoichiometric ratio that ionic weight meets Y:Al=3:5 is added, reaction temperature is 50 DEG C；
(2) urea that step (1) uses is added to Al as pH adjusting agent2O3In slurry, slurry pH=8.8 is kept, Gu
Content is 35vol.%；
(3) step (2) resulting slurry is directly filtered, without washing, core-shell structured powder can be obtained；
(4) by step (3) resulting powder in 100 DEG C of constant temperature ovens it is dry for 24 hours, and by resulting powder low temperature 300
DEG C calcining 1h；
(5) ammonium bicarbonate soln of sintering aid silica and pH=9, ball milling mixing are added into calcined powder
10h, the revolving speed of ball milling are 165r/min；Obtained slurry is dried into 12h in 55 DEG C of constant temperature oven, by gained powder mistake
200 meshes；
(6) powder after step (5) sieving is placed in mold, first dry-pressing (5MPa, pressure maintaining 30s) isostatic cool pressing afterwards
Biscuit, is then placed in Muffle furnace, using 300 DEG C of calcining 2h by (200MPa, the cold equal times are 6min) molding；
(7) the calcined biscuit of ceramics that step (6) obtains is placed in vacuum sintering furnace, using 1680 DEG C of vacuum-sinterings
4h。
(8) ceramics sample of above-mentioned vacuum-sintering is used to air atmosphere or oxygen atmosphere annealing 2h in 800 DEG C.After annealing
YAG ceramics be polished directly, obtain YAG crystalline ceramics.
Embodiment 2
(1) by the Y (NO of 0.8mol/L3)3Solution is added to Al with the speed of 3ml/min2O3In suspension, precipitating reagent is
Urea, is added the stoichiometric ratio that ionic weight meets Y:Al=3:5, and reaction temperature is 80 DEG C；
(2) urea that step (1) uses is added to Al as pH adjusting agent2O3In slurry, slurry pH=9.1 is kept, Gu
Content is 60vol.%；
(3) step (2) resulting slurry is directly filtered, without washing, core-shell structured powder can be obtained；
(4) by step (3) resulting powder in 120 DEG C of constant temperature ovens it is dry for 24 hours, and by resulting powder low temperature 500
DEG C calcining 2h；
(5) into calcined powder be added sintering aid magnesia and pH=8 sal volatile, ball milling mixing 16h,
The revolving speed of ball milling is 155r/min；By obtained slurry, gained powder for 24 hours, is crossed 100 by drying in 75 DEG C of constant temperature oven
Mesh；
(6) powder after step (5) sieving is placed in mold, first dry-pressing (4MPa, pressure maintaining 30s) isostatic cool pressing afterwards
(200MPa, the cold equal times are 5min) molding；Then biscuit is placed in Muffle furnace, using 500 DEG C of calcining 15h.
(7) the calcined biscuit of ceramics that step (6) obtains is placed in vacuum sintering furnace, using 1700 DEG C of vacuum-sinterings
10h；
(8) ceramics sample of above-mentioned vacuum-sintering is used to air atmosphere or oxygen atmosphere annealing 10h in 1350 DEG C.Annealing
YAG ceramics afterwards are polished directly, and obtain YAG crystalline ceramics.
Embodiment 3
(1) by the Y (NO of 0.6mol/L3)3Solution is added to Al with the speed of 2ml/min2O3In suspension, precipitating reagent is
Urea, is added the stoichiometric ratio that ionic weight meets Y:Al=3:5, and reaction temperature is 65 DEG C；
(2) urea that step (1) uses is added to Al as pH adjusting agent2O3In slurry, slurry pH=9 is kept, admittedly contain
Amount is 50vol.%；
(3) step (2) resulting slurry is directly filtered, without washing, core-shell structured powder can be obtained；
(4) by step (3) resulting powder in 110 DEG C of constant temperature ovens dry 18h, and by resulting powder low temperature 400
DEG C calcining 1.5h；
(5) into calcined powder be added sintering aid calcium oxide and pH=7.2 urea liquid, ball milling mixing 16h,
The revolving speed of ball milling is 155r/min；Obtained slurry is dried into 18h in 65 DEG C of constant temperature oven, gained powder is crossed into 80 mesh
Sieve；
(6) powder after step (5) sieving is placed in mold, first dry-pressing (6MPa, pressure maintaining 1s) isostatic cool pressing afterwards
(250MPa, the cold equal times are 3min) molding；Then biscuit is placed in Muffle furnace, using 400 DEG C of calcining 8h.
(7) the calcined biscuit of ceramics that step (6) obtains is placed in vacuum sintering furnace, using 1690 DEG C of vacuum-sinterings
7h；
(8) ceramics sample of above-mentioned vacuum-sintering is used to air atmosphere or oxygen atmosphere annealing 6h in 1050 DEG C.Annealing
YAG ceramics afterwards are polished directly, and obtain YAG crystalline ceramics.
Embodiment 4
(1) by the Y (NO of 0.6mol/L3)3Solution is added to Al with the speed of 1ml/min2O3In suspension, precipitating reagent is
Urea, is added the stoichiometric ratio that ionic weight meets Y:Al=3:5, and reaction temperature is 70 DEG C；
(2) urea that step (1) uses is added to Al as pH adjusting agent2O3In slurry, slurry pH=9.0 is kept, Gu
Content is 55vol.%；
(3) step (2) resulting slurry is directly filtered, without washing, core-shell structured powder can be obtained；
(4) by step (3) resulting powder in 110 DEG C of constant temperature ovens dry 18h, and by resulting powder low temperature 500
DEG C calcining 2h；
(5) ammonia spirit of sintering aid magnesia, calcium oxide and pH=12 is added into calcined powder, ball milling is mixed
6h is closed, the revolving speed of ball milling is 185r/min；Obtained slurry is dried into 18h in 55-75 DEG C of constant temperature oven, by gained powder
Body crosses 150 meshes；
(6) powder after step (5) sieving is placed in mold, first dry-pressing (2MPa, pressure maintaining 60s) isostatic cool pressing afterwards
(150MPa, the cold equal times are 8min) molding；Then biscuit is placed in Muffle furnace, using 400 DEG C of calcining 9h；
(7) the calcined biscuit of ceramics that step (6) obtains is placed in vacuum sintering furnace, using 1690 DEG C of vacuum-sinterings
7h。
(8) ceramics sample of above-mentioned vacuum-sintering is used to air atmosphere or oxygen atmosphere annealing 8h in 1200 DEG C.Annealing
YAG ceramics afterwards are polished directly, and obtain YAG crystalline ceramics.
Comparative example
This comparative example moulding process step and sintering processing are identical as above-described embodiment 1, unlike: primary raw material is
Y2O3、Al(NO3)·9H2O and HNO3Deng；It comprises the concrete steps that:
(1) by Y2O3、Al(NO3) 9H2O is dissolved in dilute nitric acid solution by n (Al): n (Y)=5:3, is configured to mix
Prepared metal-nitrate solutions are added in ammonium bicarbonate soln by metal-nitrate solutions with the speed of 1.5ml/min,
It stirs simultaneously, generates milky white precipitate, filtering；
(2) dry in 80 DEG C of baking ovens after using deionized water, dehydrated alcohol and acetone soln washing precipitate respectively
For 24 hours, presoma powder is obtained；
(3) it will be dried after presoma powder ball milling and cross 200 meshes, then by the presoma powder after sieving at 900 DEG C
Calcining 4h obtains YAG material powder,
(4) by material powder tabletting (tabletting parameter is same as Example 1), then biscuit is placed in Muffle furnace, is used
800 DEG C of calcining 6h；
(5) calcined biscuit of ceramics is placed in vacuum sintering furnace, keeps the temperature 8h in 1750 DEG C of vacuum-sinterings；
(6) ceramics sample of above-mentioned vacuum-sintering is annealed at 1450 DEG C, twin polishing to 1mm.
Fig. 1: according to the XRD spectrum of the YAG crystalline ceramics of the preparation of embodiment 1,2,3,4, all ceramics are pure YAG
Phase, no miscellaneous phase or secondary phase exist；
Fig. 2: according to the photo in kind of the YAG crystalline ceramics of the preparation of embodiment 1,2,3,4, the text below ceramics is clear
It is clear as it can be seen that show the ceramics have good light transmission, excellent in optical properties；
Fig. 3: scheme according to the surface SEM of the YAG crystalline ceramics of the preparation of embodiment 1,2,3,4, show the ceramic crystalline grain
It is of uniform size, exist without Residual Pores or secondary phase；
Fig. 4: according to the transmittance curve of the YAG crystalline ceramics of the preparation of embodiment 1,2,3,4, at 1064nm
Transmitance reach 84% or more, illustrate the ceramics have excellent optical quality.
Fig. 5: the pictorial diagram of the YAG crystalline ceramics of comparative example preparation, the text under the ceramics are slightly fuzzy；
Fig. 6: comparative example preparation YAG crystalline ceramics and its transmittance curve, transmitance of the sample at 1064nm is only
It is 68.2%.
Claims (7)
1. a kind of method for preparing YAG crystalline ceramics using core-shell structured powder, which is characterized in that specific steps are as follows:
(1) by the Y (NO of 0.5-0.8mol/L3)3Solution is added to Al with the speed of 0.5-3ml/min2O3In suspension, precipitating reagent
For urea, the stoichiometric ratio that ionic weight meets Y:Al=3:5 is added, reaction temperature is 50-80 DEG C；
(2) urea that step (1) uses is added to Al as pH adjusting agent2O3In slurry, slurry pH=8.8-9.1 is kept, Gu
Content is 35-60vol.%；
(3) step (2) resulting slurry is directly filtered, arrives core-shell structured powder without washing；
(4) by the resulting core-shell structured powder freeze-day with constant temperature of step (3), and by the powder after drying in 300-500 DEG C of calcining 1-
2h；
(5) alkaline solution of sintering aid and pH=7-12, ball milling mixing 6-16h are added into calcined powder；By ball milling
Slurry freeze-day with constant temperature afterwards, and the powder after drying is sieved；
(6) powder after step (5) sieving is placed in mold, biscuit is then placed in horse by cold isostatic compaction after first dry-pressing
Not in furnace, in 300-500 DEG C of calcining 2-15h；
(7) step (6) calcined biscuit of ceramics is placed in vacuum sintering furnace, in 1680 DEG C of -1700 DEG C of vacuum-sintering 4-
10h；
(8) ceramics sample of above-mentioned vacuum-sintering is placed in air atmosphere or oxygen atmosphere in 800-1350 DEG C of annealing 2-10h,
YAG ceramics after annealing are polished directly, and obtain YAG crystalline ceramics.
2. a kind of method for preparing YAG crystalline ceramics using core-shell structured powder according to claim 1, feature exist
In in step (4), the temperature of freeze-day with constant temperature is 100-120 DEG C, time 12-24h.
3. a kind of method for preparing YAG crystalline ceramics using core-shell structured powder according to claim 1, feature exist
In in step (5), the temperature of freeze-day with constant temperature is 55-75 DEG C, time 12-24h.
4. a kind of method for preparing YAG crystalline ceramics using core-shell structured powder according to claim 1, feature exist
In in step (5), the mesh diameter of the sieving is 80-200 mesh.
5. a kind of method for preparing YAG crystalline ceramics using core-shell structured powder according to claim 1, feature exist
In in step (6), the pressure of the dry-pressing is 2-6MPa, pressure maintaining 1-60s；The pressure of the isostatic cool pressing is 150-250MPa,
The cold equal times are 3-8min.
6. a kind of method for preparing YAG crystalline ceramics using core-shell structured powder according to claim 1, feature exist
In in step (5), the revolving speed of the ball milling is 155-185r/min.
7. a kind of method for preparing YAG crystalline ceramics using core-shell structured powder according to claim 1, feature exist
In in step (5), the sintering aid is one of silica, magnesia, calcium oxide or a variety of, the alkaline solution
For one of ammonium hydrogen carbonate, ammonium carbonate, urea, ammonium hydroxide or a variety of.
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| CN111087235A (en) * | 2019-12-30 | 2020-05-01 | 江苏师范大学 | Method for preparing YAG transparent ceramic by adopting yttrium/auxiliary agent/aluminum triple core-shell structure powder |
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| CN115650721A (en) * | 2022-10-21 | 2023-01-31 | 江苏师范大学 | Method for preparing magnesia-alumina spinel transparent ceramic by using core-shell structure powder synthesized by low-temperature hydrothermal method |
| CN115650721B (en) * | 2022-10-21 | 2023-05-23 | 江苏师范大学 | Method for preparing magnesia-alumina spinel transparent ceramic by using core-shell structure powder synthesized by low-temperature hydrothermal method |
| CN115924875A (en) * | 2022-12-23 | 2023-04-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of high-compaction lithium manganese iron phosphate positive electrode material and product thereof |
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