CN109053182A - A method of YAG base multi-layer compound structure crystalline ceramics is prepared using Isobam gel injection-moulding - Google Patents
A method of YAG base multi-layer compound structure crystalline ceramics is prepared using Isobam gel injection-moulding Download PDFInfo
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Abstract
The invention discloses a kind of method for preparing YAG base multi-layer compound structure crystalline ceramics using Isobam gel injection-moulding, prepared multi-layer ceramics meets structure shown in following formula: YAG/Re:YAG/YAG or YAG/Re:YAG/Re:YAG, and wherein YAG layers by Y3A15O12Composition, Re:YAG layers by (Y1‑xRex)3A15O12Composition, 0.02≤x≤0.2；Re is one of rare-earth element cerium, praseodymium, neodymium, samarium, europium, terbium, dysprosium, holmium, erbium, thulium or ytterbium；Isobam gel casting forming slurry is prepared first, is poured into mold after slurry is then carried out de-bubble processing, is poured other layer of slurry again after the solidification of first layer pulp gel, is dried after complete gelation, dumping；By the biscuit vacuum-sintering annealing after dumping, up to multi-layer compound structure crystalline ceramics after twin polishing.Method provided by the invention is based on water-based slurry, it is environmentally protective, ceramics obtained have the characteristics that high density, structure is complicated, optical quality is good, transmitance is high, interface ion range of scatter is small, are very suitable for the preparation of large scale and composite construction YAG base transparent ceramic material.
Description
Technical field
The invention belongs to advanced ceramics fields, are related to a kind of preparation method of multi-layer compound structure crystalline ceramics, especially relate to
A kind of and method that YAG base multi-layer compound structure crystalline ceramics is prepared using Isobam gel injection-moulding.
Background technique
Operation material of the Nd:YAG laser ceramics as laser has foreign atom coefficient height, optical property excellent, hot
Conductance is high, damage threshold is high, laser delivery efficiency is high, thermal shock resistance is good, easy manufacture, at low cost, size is big, can in high volume give birth to
It produces, easily obtain the advantages that multilayer and multifunctional ceramic structure, played an important role in high power solid state laser field.Other
Rare earth ion such as Yb, Er, Ho, the YAG crystalline ceramics of the doping such as Tm and transition metal ions Cr generate different optical maser wavelengths,
PWM Pulse Width Modulated (picosecond, femtosecond etc.) etc. also results in extensive concern.
However, since not flexible by its preparation process and structure unification is influenced, the especially single increasing of structure
Beneficial dielectric material will lead to the problem of fatal fuel factor in laser system operation: thermal stress, heating power is birefringent and heat penetration
Mirror effect etc. causes solid state laser to be difficult to develop towards large scale and high-power direction.And traditional solid phase reaction sintering
The YAG crystalline ceramics structure of method preparation is single, cannot effectively control fuel factor, and more in the past few years prepares sandwich
Method, such as plasma spraying method, hot molding, laser cladding, magnetron sputtering method, there are preparation costs high, light
Learn a series of problems, such as of poor quality, transmitance is low, structural integrity is poor, fuel factor control ability is general.In recent years, slip casting at
Type, tape casting prepare multi-functional composite construction crystalline ceramics and have achieved greater advance, obtain the properties of laser
Very big raising and improvement, but the static pressure such as cold/temperature are needed in preparation process, multilayer could be allowed closely to be bonded, increased
Manufacturing cost, while being also unfavorable for the preparation of the crystalline ceramics of multilayer labyrinth and shape.
Summary of the invention
YAG base multi-layer compound structure crystalline ceramics is prepared using Isobam gel injection-moulding the object of the present invention is to provide a kind of
Method, simple process environmental protection, ceramic dense obtained is high, and uniformity is good, and transmitance is high.
To achieve the above object, The technical solution adopted by the invention is as follows: a kind of prepare YAG using Isobam gel injection-moulding
The method of base multi-layer compound structure crystalline ceramics, prepared multi-layer ceramics meet structure shown in following formula: YAG/Re:YAG/
YAG or YAG/Re:YAG/Re:YAG, wherein YAG layers by Y3A15O12Composition, Re:YAG layers by (Y1-xRex)3A15O12Composition,
0.02≤x≤0.2；Re is rare-earth element cerium (Ce), praseodymium (Pr), neodymium (Nd), samarium (Sm), europium (Eu), terbium (Tb), dysprosium (Dy), holmium
(Ho), one of erbium (Er), thulium (Tm) or ytterbium (Yb) adulterate YAG ceramic powder to be formed；Specific step is as follows:
(1) gel casting forming slurry preparation: pure YAG layers is pressed Y3A15O12, Re:YAG layers are pressed (Y1-xRex)3A15O12,
0.02≤x≤0.2 composition needed for metallic element molar ratio weigh material powder respectively, by abrading-ball, organic solvent, dispersant A,
Sintering aid and load weighted material powder are put into ball grinder, carry out ball milling mixing, and rotational speed of ball-mill is 120r/min~160r/
Min, Ball-milling Time are 15~24 hours, obtain mixed slurry A；It takes out the mixed slurry A to be dried, crosses 100~200
Powder after sieving is placed in Muffle furnace and calcines by mesh, the raw material powder as gel casting forming；It is added and goes in ball grinder
Ionized water, Isobam104 solution, dispersant B, abrading-ball are eventually adding the raw material powder, with pH adjusting agent regulation system pH value
It is 9~11, carries out ball milling mixing again after tentatively 10~30min of stirring, rotational speed of ball-mill is 250~350r/min, and Ball-milling Time is
20~60min obtains the mixed slurry B that solid content is 70~80%, the as slurry of gel casting forming；
(2) gel casting forming: YAG the and Re:YAG gel slurry that step (1) is obtained carries out de-bubble processing, and condition is equal
Are as follows: 2~5min of degasification under vacuum environment -50~-70kpa；Then it by YAG slurry cast into mold, is being obtained after gel solidification
To biscuit on be poured Re:YAG slurry again, after the solidification of Re:YAG pulp gel, be finally poured YAG slurry or other components
Re:YAG slurry is dried, dumping after complete gelation；
(3) it forms and is sintered: the biscuit after dumping is sintered 16~24 hours for 1650~1780 DEG C in vacuum environment,
Annealing, up to multilayer YAG/Re:YAG/YAG (Re:YAG) composite construction crystalline ceramics after twin polishing.
Material powder described in step (1) is high-purity Y2O3Powder, Al2O3Powder and Re2O3Powder.
Abrading-ball described in step (1) is high purity aluminium oxide abrading-ball, and the abrading-ball and material powder total mass ratio are 1~3:
1；The organic solvent is dehydrated alcohol, and the organic solvent and material powder total mass ratio are 1:1~1.5；The dispersing agent
A be polyethyleneimine (PEI) solution, the additional amount of the dispersant A account for material powder gross mass percentage by volume be 0.1~
0.8%；The sintering aid is magnesia (MgO) and ethyl orthosilicate (TEOS), and the additional amount of the sintering aid is raw material
The 0.1~0.5% of powder gross mass.
Drying temperature described in step (1) is 50~60 DEG C, and drying time is 24~48 hours.
The detailed process of calcining described in step (1) are as follows: from room temperature to 700~900 DEG C, heating rate is 2~3
DEG C/min, 6~8 hours are kept the temperature, room temperature~100 DEG C are then cooled to, rate of temperature fall is 1~3 DEG C/min.
PH adjusting agent described in step (1) is ammonium hydroxide or tetramethylammonium hydroxide (TMAH)；The dispersant B is lemon
One of aqueous-based ceramics dispersing agent such as sour ammonium, ammonium polyacrylate, polyethylene glycol is a variety of, and the additional amount of dispersant B is described
The 0.2~0.5% of raw material powder gross mass；The additional amount of the Isobam104 solution be the raw material powder gross mass 2.5~
5%.
Step is dried process described in (2) are as follows: under room temperature after gel solidification 0.5~2 hour, is put into baking oven
In, 24~72 hours are kept the temperature at a temperature of 25~35 DEG C；It is warming up to 55~80 DEG C again, keeps the temperature 24~72 hours.
The detailed process of dumping described in step (2) are as follows: 400 are warming up at room temperature with the rate of 0.5~2 DEG C/min~
500 DEG C, 4~8 hours are kept the temperature, then is warming up to 800~900 DEG C with 0.5~2 DEG C/min, and keep the temperature 4~8 hours.
The detailed process of sintering described in step (3) are as follows: be warming up to 200 DEG C by 5~10 DEG C/min first at room temperature, protect
Secondly 10~30min of temperature is warming up to 1000 DEG C by 10~20 DEG C/min and keeps the temperature 10~30min, presses 3~10 DEG C/min liter again
Temperature is to 1300 DEG C and keeps the temperature 1~2 hour, is then warming up to 1650~1780 DEG C by 1~5 DEG C/min and keeps the temperature 6~20 hours,
Room temperature is finally cooled to 5~10 DEG C/min, vacuum degree is maintained at 1 × 10 in entire sintering process-2~1 × 10-5Pa。
The detailed process of annealing described in step (3) are as follows: be warming up to 200 DEG C by 2~5 DEG C/min first at room temperature, secondly
1200 DEG C are warming up to by 5~15 DEG C/min, is warming up to 1400~1500 DEG C of annealing temperature by 3~10 DEG C/min again, and keep the temperature
8~12 hours, room temperature is finally cooled to 5~10 DEG C/min.
Compared with prior art, the invention has the following beneficial effects:
1. method preparation multilayer (YAG/Re:YAG/YAG (Re:YAG)) composite construction crystalline ceramics tool provided by the invention
There is the features such as high density, structure is complicated, optical quality is good, transmitance is high, interface ion range of scatter is small, is very suitable for large scale
And the preparation of composite construction YAG base transparent ceramic material.
2. Isobam gel-casting method provided by the invention, preparation multilayer (YAG/Re:YAG/YAG (Re:
YAG)) during composite construction crystalline ceramics composite construction crystalline ceramics, high-purity and partial size meet demand material powder is selected,
The additive amount of organic matter in slurry preparation is few, and dumping effect is good, and biscuit consistency is high, and without static pressure such as cold/temperature, structure is complicated
And overall performance is good, preparation method is highly suitable for the YAG base transparent ceramic of high optical quality and composite construction, complicated shape
The preparation of material.
3. multilayer (YAG/Re:YAG/YAG (Re:YAG)) composite construction crystalline ceramics prepared by the present invention is with water-based slurry
Based on, it is environmentally protective, it is highly suitable for (partly) industrialization promotion of composite construction YAG base transparent ceramic material.
Detailed description of the invention
Fig. 1 is the pictorial diagram of multi-layer compound structure crystalline ceramics made from the embodiment of the present invention 1；A:YAG/1 at.%Nd:
YAG/2at.%Nd:YAG, B:YAG/2at.%Nd:YAG, C:YAG/1at.%Nd:YAG；
Fig. 2 is the transmittance curve of multi-layer compound structure crystalline ceramics made from the embodiment of the present invention 1；
Fig. 3 is the SEM of multi-layer compound structure crystalline ceramics made from the embodiment of the present invention 1.
Specific embodiment
Invention is further described in detail in the following with reference to the drawings and specific embodiments.
Using deionized water and 20~25wt.%Isobam mixed solution as solvent, dispersing agent is ammonium citrate, gathers the present invention
One of aqueous-based ceramics dispersing agent such as ammonium acrylate, polyethylene glycol, the additional amount of dispersant B are the raw material powder gross mass
0.2~0.5%.Prepare 3 specific embodiments slurry of multilayer (YAG/Re:YAG/YAG (Re:YAG)) composite construction crystalline ceramics
Component such as table 1 is expected, using theoretical yield 125g as standard.
Table 1
Embodiment 1:YAG/1at.%Nd:YAG/2at.%Nd:YAG
Pure YAG layers of composition is as shown in 0# in table 1, and 1at.%Nd:YAG layers of composition are as shown in 1# in table 1,2at.%Nd:
YAG is as shown in 3# in table 1.
Specific preparation method includes the following steps:
(1) raw material is weighed by the composition in table 1, oxide raw material powder is put into high-purity aluminium oxide ceramics ball milling first
In tank, 375g high purity aluminium oxide abrading-ball is added, and sintering aid MgO and TEOS, dispersing agent PEI, dehydrated alcohol is added with slurrying
Material；With revolving speed 160r/min on planetary ball mill, ball milling 15 hours；Obtained mixed slurry A is again dry 24 at 60 DEG C
It is sieved with 100 mesh sieve net 3 times after hour, the powder after sieving is placed in Muffle furnace and is calcined, calcination process is to be raised to 700 from room temperature
DEG C, 2 DEG C/min of heating rate keeps the temperature 6 hours, then Temperature fall to room temperature, and the powder made is the raw material powder of gel injection-moulding.
Then in ball grinder be added deionized water, Isobam104 solution, dispersing agent ammonium citrate, high purity aluminium oxide abrading-ball, finally plus
Enter the raw material powder, be 9 with tetramethylammonium hydroxide tune pH value, carries out ball milling mixing, rotational speed of ball-mill again after preliminary stirring 10min
For 250r/min, Ball-milling Time 60min, the mixed slurry B of solid content 80% is obtained；As slurry used in gel injection-moulding；Institute
Slurry fluidity obtained is good, and solid content is high.
(2) YAG the and Re:YAG gel slurry for obtaining step (1) carries out de-bubble processing, and condition is equal are as follows: vacuum environment-
Degasification 2min under 50kpa；Then it by YAG slurry cast into mold, is poured again on obtained biscuit after gel solidification
1at.%Nd:YAG slurry is finally poured 2at.%Nd:YAG slurry after the solidification of 1at.%Nd:YAG pulp gel, completely solidifying
It is put into baking oven after gelatinization, keeps the temperature 24 hours at 25 DEG C；It is warming up to 55 DEG C again and keeps the temperature 24 hours.Dumping is carried out after the completion of dry,
400 DEG C are warming up to the rate of 0.5 DEG C/min at room temperature, keeps the temperature 4 hours, then be warming up to 800 DEG C with 0.5 DEG C/min, and keep the temperature
4 hours, effectively remove organic matter.The pattern of gel biscuit is intact, it is whole uniformly, flawless or fracture, and having certain strong
Degree.
(3) biscuit after dumping is warming up to 200 DEG C by 5 DEG C/min in vacuum environment, keeps the temperature 10min, secondly presses 10
DEG C/min is warming up to 1000 DEG C and keeps the temperature 10min, be warming up to 1300 DEG C by 3 DEG C/min again and keep the temperature 1 hour, then by 1 DEG C/
Min is warming up to 1780 DEG C and keeps the temperature 8 hours, finally cools to room temperature with 5 DEG C/min, vacuum degree is maintained in entire sintering process
1×10-2~1 × 10-5Pa.Then it anneals, is warming up to 200 DEG C by 2 DEG C/min first at room temperature, be secondly warming up to by 5 DEG C/min
1200 DEG C, 1400 DEG C of annealing temperature is warming up to by 3 DEG C/min again, and keep the temperature 8 hours, room is finally cooled to 5 DEG C/min
For temperature to get multilayer YAG/1at.%Nd:YAG/2at.%Nd:YAG, pattern photo is shown in that Figure 1A, Figure 1B, Fig. 1 C are YAG/ respectively
The pattern photo of 2at.%Nd:YAG, YAG/1at.%Nd:YAG composite construction crystalline ceramics.
After YAG/1at.%Nd:YAG/2at.%Nd:YAG composite construction crystalline ceramics twin polishing, optical quality is excellent,
Transmitance is shown in Fig. 2, and the transmitance at 1064nm is 84.2%.Its cross-section morphology picture is shown in Fig. 3 simultaneously, and grain size is closed
It is suitable, it can not find stomata and other miscellaneous phases in figure.Illustrate that Gel-casting process and vacuum sintering technology can prepare the more of high quality
Layer YAG/Re:YAG/YAG (Re:YAG) composite construction crystalline ceramics.
Embodiment 2:YAG/1.5at.%Nd:YAG/YAG
Pure YAG layers of composition is as shown in 0# in table 1, and 1.5at.%Nd:YAG layers of composition are as shown in 2# in table 1.
Specific preparation method includes the following steps:
(1) raw material is weighed by the composition in table 1, oxide raw material powder is put into high-purity aluminium oxide ceramics ball milling first
In tank, 125g high purity aluminium oxide abrading-ball is added, and sintering aid MgO and TEOS, dispersing agent PEI, dehydrated alcohol is added with slurrying
Material；With revolving speed 120r/min on planetary ball mill, ball milling 24 hours；Obtained mixed slurry A is again dry 48 at 50 DEG C
It is sieved with 100 mesh sieve net 3 times after hour, the powder after sieving is placed in Muffle furnace and is calcined, calcination process is to be raised to 900 from room temperature
DEG C, 3 DEG C/min of heating rate keeps the temperature 8 hours, and then for Temperature fall to 100 DEG C, the powder made is the raw material of gel injection-moulding
Powder.Then deionized water, Isobam104 solution, dispersing agent polyethylene glycol, high purity aluminium oxide abrading-ball are added in ball grinder, most
After the raw material powder is added, be 11 with tetramethylammonium hydroxide tune pH value, it is preliminary stir 30min after carry out ball milling mixing, ball again
Mill revolving speed is 350r/min, Ball-milling Time 20min, obtains the mixed slurry B of solid content 75%；As slurry used in gel injection-moulding
Material；Obtained slurry fluidity is good, and solid content is high.
(2) YAG the and Re:YAG gel slurry for obtaining step (1) carries out de-bubble processing, and condition is equal are as follows: vacuum environment-
Degasification 5min under 70kpa；Then it by YAG slurry cast into mold, is poured again on obtained biscuit after gel solidification
1.5at.%Nd:YAG slurry is finally poured YAG slurry, complete gelation after the solidification of 1.5at.%Nd:YAG pulp gel
After be put into baking oven, keep the temperature 72 hours at 35 DEG C；It is warming up to 80 DEG C again and keeps the temperature 72 hours.Dumping, room temperature are carried out after the completion of dry
Under with the rate of 2 DEG C/min be warming up to 500 DEG C, keep the temperature 8 hours, then be warming up to 900 DEG C with 2 DEG C/min, and keep the temperature 8 hours, have
The removal organic matter of effect.The pattern of gel biscuit is intact, and has certain intensity.
(3) biscuit after dumping is warming up to 200 DEG C by 10 DEG C/min in vacuum environment, keeps the temperature 30min, secondly presses 20
DEG C/min is warming up to 1000 DEG C and keeps the temperature 30min, 1300 DEG C are warming up to by 10 DEG C/min again and keeps the temperature 2 hours, then press 5
DEG C/min be warming up to 1780 DEG C and keep the temperature 20 hours, room temperature, vacuum degree in entire sintering process are finally cooled to 10 DEG C/min
It is maintained at 1 × 10-2~1 × 10-5Pa.Then anneal, be warming up to 200 DEG C by 5 DEG C/min first at room temperature, secondly by 15 DEG C/
Min is warming up to 1200 DEG C, is warming up to 1500 DEG C of annealing temperature by 10 DEG C/min again, and keeps the temperature 12 hours, finally with 10 DEG C/
Min cools to room temperature.Up to multilayer YAG/Re:YAG/YAG composite construction crystalline ceramics after twin polishing.
Embodiment 3:YAG/2at.%Nd:YAG/YAG
Pure YAG layers of composition is as shown in 0# in table 1, and 2at.%Nd:YAG is as shown in 3# in table 1.
Specific preparation method includes the following steps:
(1) raw material is weighed by the composition in table 1, oxide raw material powder is put into high-purity aluminium oxide ceramics ball milling first
In tank, 250g high purity aluminium oxide abrading-ball is added, and sintering aid MgO and TEOS, dispersing agent PEI, dehydrated alcohol is added with slurrying
Material；With revolving speed 150r/min on planetary ball mill, ball milling 20 hours；Obtained mixed slurry A is again dry 36 at 55 DEG C
It is crossed 200 mesh screen 3 times after hour, the powder after sieving is placed in Muffle furnace and is calcined, calcination process is to be raised to 800 from room temperature
DEG C, 2 DEG C/min of heating rate keeps the temperature 7 hours, and then for Temperature fall to 50 DEG C, the powder made is the raw material powder of gel injection-moulding.
Then deionized water, Isobam104 solution, dispersants ammonium polyacrylate, high purity aluminium oxide abrading-ball are added in ball grinder, finally
The raw material powder is added, is 10 with ammonium hydroxide tune pH value, carries out ball milling mixing, rotational speed of ball-mill 350r/ again after preliminary stirring 20min
Min, Ball-milling Time 40min obtain the mixed slurry B of solid content 70%；As slurry used in gel injection-moulding；Obtained slurry
Expect that mobility is fine, viscosity is small.
(2) YAG the and Re:YAG gel slurry for obtaining step (1) carries out de-bubble processing, and condition is equal are as follows: vacuum environment-
Degasification 3min under 60kpa；Then it by YAG slurry cast into mold, is poured again on obtained biscuit after gel solidification
2at.%Nd:YAG slurry is finally poured YAG slurry, puts after complete gelation after the solidification of 2at.%Nd:YAG pulp gel
Enter in baking oven, keeps the temperature 48 hours at 30 DEG C；It is warming up to 70 DEG C again and keeps the temperature 48 hours.Dumping is carried out after the completion of dry, at room temperature with 1
DEG C/rate of min is warming up to 450 DEG C, 6 hours are kept the temperature, then be warming up to 850 DEG C with 1 DEG C/min, and keep the temperature 6 hours, effectively gone
Except organic matter.The pattern of gel biscuit is intact, and has certain intensity.
(3) biscuit after dumping is warming up to 200 DEG C by 8 DEG C/min in vacuum environment, keeps the temperature 20min, secondly presses 15
DEG C/min is warming up to 1000 DEG C and keeps the temperature 20min, 1300 DEG C are warming up to by 6 DEG C/min again and keeps the temperature 1.5 hours, then press 3
DEG C/min be warming up to 1750 DEG C and keep the temperature 10 hours, room temperature, vacuum degree in entire sintering process are finally cooled to 8 DEG C/min
It is maintained at 1 × 10-2~1 × 10-5Pa.Then anneal, be warming up to 200 DEG C by 3 DEG C/min first at room temperature, secondly by 10 DEG C/
Min is warming up to 1200 DEG C, 1450 DEG C of annealing temperature is warming up to by 8 DEG C/min again, and keep the temperature 10 hours, finally with 8 DEG C/min
Cool to room temperature.Up to multilayer YAG/Re:YAG/YAG composite construction crystalline ceramics after twin polishing.
Claims (10)
1. a kind of method for preparing YAG base multi-layer compound structure crystalline ceramics using Isobam gel injection-moulding, which is characterized in that institute
The multi-layer ceramics of preparation meets structure shown in following formula: YAG/Re:YAG/YAG or YAG/Re:YAG/Re:YAG, and wherein YAG layers
By Y3A15O12Composition, Re:YAG layers by (Y1-xRex)3A15O12Composition, 0.02≤x≤0.2；Re be rare-earth element cerium, praseodymium, neodymium,
One of samarium, europium, terbium, dysprosium, holmium, erbium, thulium or ytterbium；Specific step is as follows:
(1) gel casting forming slurry preparation: pure YAG layers is pressed Y3A15O12, Re:YAG layers are pressed (Y1-xRex)3A15O12, 0.02≤
Metallic element molar ratio needed for the composition of x≤0.2 weighs material powder respectively, and abrading-ball, organic solvent, dispersant A, sintering are helped
Agent and load weighted material powder are put into ball grinder, carry out ball milling mixing, and rotational speed of ball-mill is 120r/min~160r/min, ball
Time consuming is 15~24 hours, obtains mixed slurry A；It takes out the mixed slurry A to be dried, crosses 100~200 meshes,
Powder after sieving is placed in Muffle furnace and is calcined, the raw material powder as gel casting forming；Deionization is added in ball grinder
Water, Isobam104 solution, dispersant B, abrading-ball are eventually adding the raw material powder, with pH adjusting agent regulation system pH value be 9~
Ball milling mixing is carried out again after 11, tentatively 10~30min of stirring, rotational speed of ball-mill is 250~350r/min, Ball-milling Time is 20~
60min obtains the mixed slurry B that solid content is 70~80%, the as slurry of gel casting forming；
(2) gel casting forming: YAG the and Re:YAG gel slurry that step (1) is obtained carries out de-bubble processing, and condition is equal are as follows:
2~5min of degasification under vacuum environment -50~-70kpa；Then it by YAG slurry cast into mold, is being obtained after gel solidification
Re:YAG slurry is poured on biscuit again, after the solidification of Re:YAG pulp gel, is finally poured the Re of YAG slurry or other components:
YAG slurry is dried, dumping after complete gelation；
(3) it forms and is sintered: the biscuit after dumping being sintered 16~24 hours for 1650~1780 DEG C in vacuum environment, annealing,
Up to multilayer YAG/Re:YAG/YAG (Re:YAG) composite construction crystalline ceramics after twin polishing.
2. according to claim 1 a kind of using Isobam gel injection-moulding preparation YAG base multi-layer compound structure crystalline ceramics
Method, which is characterized in that material powder described in step (1) be high-purity Y2O3Powder, Al2O3Powder and Re2O3Powder.
3. according to claim 1 a kind of using Isobam gel injection-moulding preparation YAG base multi-layer compound structure crystalline ceramics
Method, which is characterized in that abrading-ball described in step (1) is high purity aluminium oxide abrading-ball, the abrading-ball and material powder gross mass
Than for 1~3:1；The organic solvent is dehydrated alcohol, and the organic solvent and material powder total mass ratio are 1:1~1.5；Institute
Stating dispersant A is polyethyleneimine (PEI) solution, and the additional amount of the dispersant A accounts for the volume basis of material powder gross mass
Number is 0.1~0.8%；The sintering aid is magnesia and ethyl orthosilicate, and the additional amount of the sintering aid is raw material powder
The 0.1~0.5% of body gross mass.
4. according to claim 1 a kind of using Isobam gel injection-moulding preparation YAG base multi-layer compound structure crystalline ceramics
Method, which is characterized in that drying temperature described in step (1) be 50~60 DEG C, drying time be 24~48 hours.
5. according to claim 1 a kind of using Isobam gel injection-moulding preparation YAG base multi-layer compound structure crystalline ceramics
Method, which is characterized in that the detailed process of calcining described in step (1) are as follows: from room temperature to 700~900 DEG C, heating speed
Rate is 2~3 DEG C/min, keeps the temperature 6~8 hours, then cools to room temperature~100 DEG C, and rate of temperature fall is 1~3 DEG C/min.
6. according to claim 1 a kind of using Isobam gel injection-moulding preparation YAG base multi-layer compound structure crystalline ceramics
Method, which is characterized in that pH adjusting agent described in step (1) be ammonium hydroxide or tetramethylammonium hydroxide；The dispersant B is
One of ammonium citrate, ammonium polyacrylate, polyethylene glycol are a variety of, and the additional amount of dispersant B is the raw material powder gross mass
0.2~0.5%；The additional amount of the Isobam104 solution is the 2.5~5% of the raw material powder gross mass.
7. according to claim 1 a kind of using Isobam gel injection-moulding preparation YAG base multi-layer compound structure crystalline ceramics
Method, which is characterized in that step is dried process described in (2) are as follows: under room temperature after gel solidification 0.5~2 hour,
It is put into baking oven, keeps the temperature 24~72 hours at a temperature of 25~35 DEG C；It is warming up to 55~80 DEG C again, keeps the temperature 24~72 hours.
8. according to claim 1 a kind of using Isobam gel injection-moulding preparation YAG base multi-layer compound structure crystalline ceramics
Method, which is characterized in that the detailed process of dumping described in step (2) are as follows: at room temperature with the rate liter of 0.5~2 DEG C/min
Temperature keeps the temperature 4~8 hours to 400~500 DEG C, then is warming up to 800~900 DEG C with 0.5~2 DEG C/min, and keep the temperature 4~8 hours.
9. according to claim 1 a kind of using Isobam gel injection-moulding preparation YAG base multi-layer compound structure crystalline ceramics
Method, which is characterized in that the detailed process of sintering described in step (3) are as follows: be warming up to first by 5~10 DEG C/min at room temperature
200 DEG C, 10~30min is kept the temperature, secondly 1000 DEG C is warming up to by 10~20 DEG C/min and keeps the temperature 10~30min, press 3~10 again
DEG C/min be warming up to 1300 DEG C and keep the temperature 1~2 hour, then by 1~5 DEG C/min be warming up to 1650~1780 DEG C and heat preservation 6~
20 hours, room temperature is finally cooled to 5~10 DEG C/min, vacuum degree is maintained at 1 × 10 in entire sintering process-2~1 × 10- 5Pa。
10. according to claim 1 a kind of using Isobam gel injection-moulding preparation YAG base multi-layer compound structure crystalline ceramics
Method, which is characterized in that the detailed process of annealing described in step (3) are as follows: be warming up to first by 2~5 DEG C/min at room temperature
200 DEG C, 1200 DEG C secondly are warming up to by 5~15 DEG C/min, is warming up to annealing temperature 1400~1500 by 3~10 DEG C/min again
DEG C, and 8~12 hours are kept the temperature, room temperature is finally cooled to 5~10 DEG C/min.
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Effective date of registration: 20200306 Address after: 221000 Xinzhuang village and mailou village, New District Office, Tongshan District, Xuzhou City, Jiangsu Province Applicant after: Xuzhou attapulgite Photoelectric Technology Co., Ltd Address before: 221000 57 Heping Road, No. 4, west campus, Yunlong campus, Jiangsu Normal University, Xuzhou, Jiangsu. Applicant before: XUZHOU JIANGSU NORMAL UNIVERSITY LASER TECHNOLOGY CO., LTD. |
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