CN101306942B - Fine-crystal high transparency ruby ceramic materials and low-temperature preparation thereof - Google Patents
Fine-crystal high transparency ruby ceramic materials and low-temperature preparation thereof Download PDFInfo
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- CN101306942B CN101306942B CN200810062629A CN200810062629A CN101306942B CN 101306942 B CN101306942 B CN 101306942B CN 200810062629 A CN200810062629 A CN 200810062629A CN 200810062629 A CN200810062629 A CN 200810062629A CN 101306942 B CN101306942 B CN 101306942B
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Abstract
The invention discloses a fine crystalline transparent ruby ceramic material with high-linear light transmittance and a technology for making the same under the condition of a pulse electric field. The transparent ruby ceramics made by the invention is sintered within a temperature range of between 1,200 and 1,400 DEG C with the sintering time of the entire process less than 30 minutes; moreover, the material has a relative density higher than 99.5 percent and the average grain size of between 0.5 and 1 micron, the Vickers hardness more than 19 GPa, the bending strength of between 600 and 800MPa, the fracture toughness of between 4 and 5 MPam<1/2> and the linear light transmittance at 640 nm wavelength more than 30 percent; and the color of the made ruby changes along with the variation in the doping quantity of Cr in the material. The transparent ruby ceramics made by the technology contains MgO with the weight ratio of between 0.01 and 0.5 percent and Cr2O3 with the weight ratio of between 0.01 and 2 percent. The method for making the transparent ruby ceramics disclosed by the invention has the characteristics of low temperature and quickness; moreover, the method has high reliability, and the deviation between the mechanical property and the optical performance of transparent ruby alumina ceramics made in different batches is not more than 2 percent.
Description
Technical field
The present invention relates to the preparation method of transparent ceramic material, specifically relate to a kind of fine-crystal transparent ruby ceramic materials of high straight-line luminous transmittance and the technology of preparing under the pulsed electrical field existence condition is arranged.
Background technology
As a kind of natural gemstone of preciousness, ruby obtains doting on of common people always.And since nineteen sixty had been invented ruby laser, ruby began really to be applied in the middle of the industrial production.Until now, the preparation method of synthetic ruby is main with the high-temperature fusion reaction method still still, and cost is still higher, and is difficult to make high-quality large size synthetic ruby crystal.Expensive with respect to monocrystalline prepares the direction that high-quality polycrystalline ruby becomes a development.Before the present invention, about the document of this respect and patent report all seldom, but quite similar with the realization approach of transparent alumina ceramics, a kind of method be exactly the preparation grain-size very big contain Cr
3+Thereby alumina transparent ceramic reduce the crystal boundary scattering realize transparent, another kind of method then be the preparation sub-micron crystal Cr
3+: Al
2O
3Thereby prepare transparent ruby ceramic materials.The sintering temperature of using among the patent CN1778758 all is higher than 1650 ℃, therefore can affirm the scope of grain-size greater than submicron, does not have the concrete numeral report of straight-line luminous transmittance in the patent.K.HAYASHI (Journal of theCeramic Society of Japan; 1989) made the transparent red jewel pottery of submicrometer structure through the method that adopts high pure raw material and 1250 ℃ of static pressure such as presintering heating; But the light transmission rate that is shown in the article obviously is the contribution that has comprised scattered light greater than 70% result, therefore is difficult to confirm the level of straight-line luminous transmittance.MiYoungSeo (Journal of Korean Ceramic Society, 2006) adopts the technology of static pressure such as identical and sintering heating to obtain transparent red jewel kapillary, but does not have the report of light transmission rate in the literary composition.Though patent WO2005068392 has still adopted identical and sintering to add the method for HIP sintering, has reported accurate believable straight-line luminous transmittance data for the first time, straight-line luminous transmittance can reach 30% when the 640nm wavelength.The most successful heat and other static pressuring processes still needs a prefabricated stage of very long relatively sample, comprises forming of green body and low temperature presintering, adds the flow process that last hip treatment often will experience at least 24 hours but all in all.The complicated flow process of heat and other static pressuring processes has determined should technology in actually operating, to be difficult to repeatability, and cost is higher.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, simple fine-crystal high transparency ruby ceramic materials of a kind of preparation technology and low temperature Fast Sintering preparation method thereof are provided.
The chemical constitution of fine-crystal transparent ruby pottery is that to contain weight percent be 0.01%～0.5% MgO and 0.01%～2% Cr
2O
3Al
2O
3, the median size of fine-crystal transparent ruby pottery is 0.5～1 micron, the straight-line luminous transmittance of material is greater than 30% when optical wavelength is 640nm.
The specific density of described fine-crystal transparent ruby pottery is higher than 99.5%, and Vickers' hardness is 19～21GPa, and bending strength is 600～800MPa, and fracture toughness property is 4～5MPam
1/2
The preparation method of fine-crystal transparent ruby pottery comprises the steps:
1) MgO of 100 weight part aluminum oxide, 0.01～0.5 weight part being put into ball grinder is medium ball milling 1～2 hour with water and high purity aluminium oxide ball; Salpeter solution with 0.1M before the ball milling is adjusted into 3～4 with the pH value; 80～100 ℃ of vacuum-drying 4～5 hours is crossed 60 mesh sieves and is obtained powder;
2) powder that sieves is pressed into biscuit through isostatic cool pressing 120～250MPa after with punching block 40～70MPa dry-pressing again, biscuit is put into 750～900 ℃ of pre-burnings of box retort furnace, putting into concentration then respectively is the Cr (NO of 0.05～2M
3)
39H
2Soaked in the O solution 2～3 hours, solution is placed in the airtight Glass Containers that air pressure is 150～200Pa during immersion, takes out the biscuit that soaked and puts into slowly drying of baking oven;
3) dried biscuit is put into graphite jig with discharge plasma sintering stove sintering; Keep the vacuum of 3～6Pa in the stove, furnace temperature is warming up to 600 ℃ at 3～4 minutes internal heating, is warming up to 1200～1400 ℃ and this temperature insulation 1～10 minute at 3～10 minutes internal heating then; 10～200MPa keep-ups pressure; Cooling is taken out sample, 900～1100 ℃ of thermal treatments 8～12 hours when furnace temperature drops to 200～300 ℃.
The preparation method of fine-crystal transparent ruby pottery comprises the steps:
1) with 100 weight part aluminum oxide, be equivalent to the Mg (NO of 0.01～0.5 weight part MgO
3)
26H
2O be equivalent to 0.01～2 weight part Cr
2O
3Cr (NO
3)
39H
2It is medium ball milling 1～2 hour with water and high purity aluminium oxide ball that O puts into ball grinder, and slurry sprays into liquid nitrogen freezing, and the freeze drier inner drying obtained powder in 30～90 hours, and the salpeter solution with 0.1M before the ball milling is adjusted into 3～4 with the pH value;
2) powder that makes is directly put into graphite jig with discharge plasma sintering stove sintering; Keep the vacuum of 3～6Pa in the stove, furnace temperature is warming up to 600 ℃ at 3～4 minutes internal heating, is warming up to 1200～1400 ℃ and this temperature insulation 1～10 minute at 3～10 minutes internal heating then; 10～200MPa keep-ups pressure; Cooling is taken out sample, 900～1100 ℃ of thermal treatments 8～12 hours when furnace temperature drops to 200～300 ℃.
Described aluminum oxide powder purity is greater than 99.99%, and the particle diameter of powder is 100～500nm, and specific surface area is 4～15m
2/ g.
The average grain size of the prepared fine-crystal transparent ruby of the present invention pottery is between 0.5 to 1 micron, and its exemplary microstructure is as shown in Figure 2, and grain size distribution is even, the no crystal grain phenomenon of growing up unusually.
The present invention can reach above-mentioned optics and mechanical performance index in very wide material compositing range, can come the material component of designing optimal according to the concrete application approach of transparent red jewel aluminum oxide.Used aluminum oxide is purity greater than 99.99% aluminum oxide in the technology of the present invention, but the powder granule size can be selected between the 500nm at 100nm.Contain weight ratio in its chemical constitution and be 0.01%～0.5% MgO and 0.01%～2% Cr
2O
3The depth of ruby color can be come through Cr as required
2O
3Content regulate.
The ruby crystalline ceramics of the present invention's preparation is fit to be applied to, and protection is armoring, semi-conductor industry connecting device, precision measurement equipment wear part, wrist-watch bearing, watch chain and watchcase, laserable material, flawless finish and large size costume jewelry starting material.
The preparation method who the present invention relates to transparent red jewel alumina-ceramic has low temperature, fast characteristics.Sintering temperature is lower than 1450 ℃, and the time of sintering whole process is no more than 30 minutes.This technological safety is very high, and the transparent alumina mechanics and the optical property deviation of different batches production are no more than 2%.
Description of drawings
Fig. 1 is the test set synoptic diagram of cathetus transmittance of the present invention;
Fig. 2 is the typical microstructure of the prepared high straight-line luminous transmittance ruby of technology of preparing of the present invention crystalline ceramics;
Fig. 3 is that embodiment 1 gained sample is at 200 straight-line luminous transmittance and wavelength relationship curves to the 2000nm wavelength region;
Fig. 4 is that embodiment 2 gained samples are at 200 straight-line luminous transmittance and wavelength relationship curves to the 2000nm wavelength region;
Fig. 5 is that embodiment 3 gained samples are at 200 straight-line luminous transmittance and wavelength relationship curves to the 2000nm wavelength region;
Fig. 6 is that embodiment 4 gained samples are at 200 straight-line luminous transmittance and wavelength relationship curves to the 2000nm wavelength region.
Embodiment
Stupalith sintering among the present invention all is to utilize the discharge plasma sintering stove of being produced by Japanese Sumitomo Coal Mining Co. company (Dr.Sinter 2050) to come concrete the completion.
Following examples come the present invention is further described, but the present invention is not limited to these embodiment.
In aluminum oxide is 100%, takes by weighing the MgO of mass percent 0.01%, is 99.99% with purity then, and mean particle size is the Al of 250nm
2O
3It is medium ball milling 1 hour with water and high purity aluminium oxide ball that powder is put into ball grinder, and the salpeter solution with 0.1M before the ball milling is adjusted into 3 with the pH value.80 ℃ of vacuum-drying is 4 hours behind the ball milling, crosses 60 mesh sieves.Taking by weighing 1 powder that sieves of gram suppresses through isostatic cool pressing 120MPa after with punching block 70MPa dry-pressing again and obtains biscuit.Then biscuit is put into 800 ℃ of pre-burnings of box retort furnace, then the pre-burning biscuit being put into concentration respectively is 0.1M, the Cr (NO of 0.2M and 0.5M
3)
39H
2Soaked 2 hours in the O solution, solution is placed in the airtight Glass Containers that air pressure is 150Pa during immersion.Put into slowly drying of a conventional oven after taking out the biscuit that soaked.Treat promptly to put into graphite jig with discharge plasma sintering stove sintering after the biscuit drying; The control furnace temperature was raised to 600 ℃ in 3 minutes; Be heated to 1300 ℃ and then in 6 minutes this temperature insulation 3 minutes; The sintering process 80MPa that keep-ups pressure, the cooling of cutting off the electricity supply is then taken out graphite jig when furnace temperature drops to 200 ℃ with sample.And after 1000 ℃ of air conditionses of high temperature descend processing 10 hours, at last with ceramic plate twin polishing to 0.8 millimeter thickness measuring optical performance.
The specific density of three kinds of ceramics samples behind the sintering is all more than 99.8%, and according to the order that soaking solution concentration raises, the average grain size of material is respectively 1 micron; 0.7 the micron and 0.6 micron, the Vickers' hardness of material is respectively 19GPa, 20.4GPa and 20GPa; Bending strength then is respectively 610; 700 and 760MPa, fracture toughness property is respectively 3.7,4.1 and 4.6MPam
1/2The straight-line luminous transmittance result under the different wave length condition is as shown in Figure 3 for material: in the 640nm wavelength, raise with strength of solution, the straight-line luminous transmittance of material is respectively 38%, 36.8% and 30.6%.Reference material with the Cr that do not mix is compared, and the ruby pottery of three kinds of different Cr content all tangible photoabsorption occurred in identical wavelength region, and this is the major cause that causes ruby different depths red; And increase with wavelength, the straight-line luminous transmittance of three kinds of ruby crystalline ceramics moves closer to reference material, can reach 78%-81% during 2000nm.
Embodiment 2
In aluminum oxide is 100%, takes by weighing to be equivalent to mass percent 0.03%MgO and 1.5%Cr
2O
3CP Mg (NO
3)
26H
2O and Cr (NO
3)
39H
2O is 99.99% with purity then, and mean particle size is the Al of 150nm
2O
3It is medium ball milling 1 hour with water and high purity aluminium oxide ball that powder is put into ball grinder, and the salpeter solution with 0.1M before the ball milling is adjusted into 3 with the pH value.Directly slurry is sprayed into liquid nitrogen freezing behind the ball milling, then freeze drier inner drying 72 hours, 60 mesh sieves are crossed in dry back.Take by weighing in the direct graphite jig of the powder that sieves with discharge plasma sintering stove sintering; The control furnace temperature was raised to 600 ℃ in 3 minutes; Be heated to 1350 ℃ and then in 6 minutes this temperature insulation 5 minutes; The sintering process 150MPa that keep-ups pressure, the cooling of cutting off the electricity supply is then taken out graphite jig when furnace temperature drops to 200 ℃ with sample.And, at last ceramic plate twin polishing to 0.8 mm thick is come the measuring optical performance after 1000 ℃ of air conditionses of high temperature were handled 10 hours down.
The specific density of transparent red jewel ceramics sample is 99.9% behind the sintering, and the average grain size of material is respectively 0.7 micron, the Vickers' hardness 20GPa of material, and fracture toughness property is 5.2MPam
1/2The straight-line luminous transmittance of material is 29.1% when wavelength is 640nm, then reaches 58% during 2000nm.The straight-line luminous transmittance result under the different wave length condition is as shown in Figure 4 for material: the sample with among the embodiment 1 is compared, and the photoabsorption phenomenon in embodiment 2 samples is stronger, but absorption bands is very close.
Embodiment 3
In aluminum oxide is 100%, takes by weighing to be equivalent to mass percent 0.3%MgO and 0.1%Cr
2O
3CP Mg (NO
3)
26H
2O and Cr (NO
3)
39H
2O is 99.99% with purity then, and mean particle size is the Al of 350nm
2O
3It is medium ball milling 1 hour with water and high purity aluminium oxide ball that the ` powder is put into ball grinder, and the salpeter solution with 0.1M before the ball milling is adjusted into 3 with the pH value.Directly slurry is sprayed into liquid nitrogen freezing behind the ball milling, then freeze drier inner drying 72 hours, 60 mesh sieves are crossed in dry back.Take by weighing the powder that sieves and directly put into graphite jig with discharge plasma sintering stove sintering; The control furnace temperature was raised to 600 ℃ in 3 minutes; Be heated to 1250 ℃ and then in 6 minutes, the sintering process 50MPa that keep-ups pressure, the cooling of cutting off the electricity supply then this temperature insulation 2 minutes.When furnace temperature drops to 200 ℃ graphite jig is taken out with sample.And, at last ceramic plate twin polishing to 0.8 millimeter thickness is come the measuring optical performance after 1000 ℃ of air conditionses of high temperature were handled 10 hours down.
The specific density of transparent red jewel ceramics sample is 99.9% behind the sintering, and the average grain size of material is respectively 0.8 micron, the Vickers' hardness 20GPa of material, and fracture toughness property is 4.7MPam
1/2Material is as shown in Figure 5 in the straight-line luminous transmittance result under the different wave length condition: the straight-line luminous transmittance of material is 34.1% when wavelength is 640nm, then reaches 74% during 2000nm.
Embodiment 4
In aluminum oxide is 100%, takes by weighing to be equivalent to mass percent 0.5%MgO and 0.3%Cr
2O
3CP Mg (NO
3)
26H
2O and Cr (NO
3)
39H
2O is 99.99% with purity then, and mean particle size is the Al of 200nm
2O
3It is medium ball milling 1 hour with water and high purity aluminium oxide ball that powder is put into ball grinder, and the salpeter solution with 0.1M before the ball milling is adjusted into 3 with the pH value.Directly slurry is sprayed into liquid nitrogen freezing behind the ball milling, then freeze drier inner drying 54 hours, 60 mesh sieves are crossed in dry back.Take by weighing the powder that sieves and directly put into graphite jig with discharge plasma sintering stove sintering; The control furnace temperature was raised to 600 ℃ in 3 minutes; Be heated to 1370 ℃ and then in 8 minutes, the sintering process 140MPa that keep-ups pressure, the cooling of cutting off the electricity supply then this temperature insulation 5 minutes.When furnace temperature drops to 200 ℃ graphite jig is taken out with sample.And, at last ceramic plate twin polishing to 0.8 mm thick is come the measuring optical performance after 1000 ℃ of air conditionses of high temperature were handled 10 hours down.
The specific density of the transparent red jewel ceramics sample behind the sintering is 99.8%, and the average grain size of material is respectively 0.6 micron, the Vickers' hardness 21GPa of material, and fracture toughness property is 4.9MPam
1/2Material is as shown in Figure 6 in the straight-line luminous transmittance result under the different wave length condition: the straight-line luminous transmittance of material is 45% when wavelength is 640nm, then reaches 79% during 2000nm.
Embodiment 5
In aluminum oxide is 100%, takes by weighing the MgO of mass percent 0.01%, is 99.99% with purity then, and mean particle size is the Al of 100nm
2O
3It is medium ball milling 1 hour with water and high purity aluminium oxide ball that powder is put into ball grinder, and the salpeter solution with 0.1M before the ball milling is adjusted into 3,80 ℃ of vacuum-dryings 4 hours with the pH value, crosses 60 mesh sieves and obtains powder.The powder that sieves is pressed into biscuit through isostatic cool pressing 120MPa after with punching block 40MPa dry-pressing again, biscuit is put into 750 ℃ of pre-burnings of box retort furnace, putting into concentration then is the Cr (NO of 0.05M
3)
39H
2Soaked 2 hours in the O solution, solution is placed in the airtight Glass Containers that air pressure is 150Pa during immersion, takes out the biscuit that soaked and puts into slowly drying of baking oven.Dried biscuit is put into graphite jig with discharge plasma sintering stove sintering; Keep the vacuum of 3Pa in the stove, furnace temperature is warming up to 600 ℃ at 3 minutes internal heating, is warming up to 1200 ℃ and this temperature insulation 1 minute at 3 minutes internal heating then; 10MPa keep-ups pressure; Cooling is taken out sample, 900 ℃ of thermal treatments 8 hours when furnace temperature drops to 200 ℃.Prepared ceramics sample is an incarnadine, and straight-line luminous transmittance is 34.7% when wavelength 640nm.
Embodiment 6
In aluminum oxide is 100%, takes by weighing the MgO of mass percent 0.5%, is 99.99% with purity then, and mean particle size is the Al of 500nm
2O
3It is medium ball milling 2 hours with water and high purity aluminium oxide ball that powder is put into ball grinder, and the salpeter solution with 0.1M before the ball milling is adjusted into 4,100 ℃ of vacuum-dryings 5 hours with the pH value, crosses 60 mesh sieves and obtains powder.The powder that sieves is pressed into biscuit through isostatic cool pressing 250MPa after with punching block 70MPa dry-pressing again, biscuit is put into 900 ℃ of pre-burnings of box retort furnace, putting into concentration then is the Cr (NO of 2M
3)
39H
2Soaked 3 hours in the O solution, solution is placed in the airtight Glass Containers that air pressure is 200Pa during immersion, takes out the biscuit that soaked and puts into slowly drying of baking oven.Dried biscuit is put into graphite jig with discharge plasma sintering stove sintering; Keep the vacuum of 6Pa in the stove, furnace temperature is warming up to 600 ℃ at 4 minutes internal heating, is warming up to 1400 ℃ and this temperature insulation 10 minutes at 10 minutes internal heating then; 200MPa keep-ups pressure; Cooling is taken out sample, 1100 ℃ of thermal treatments 12 hours when furnace temperature drops to 300 ℃.Prepared crystalline ceramics sample is a scarlet, and straight-line luminous transmittance is 32.5% when wavelength 640nm.
Embodiment 7
In aluminum oxide is 100%, takes by weighing the Mg (NO that is equivalent to 0.01%MgO
3)
26H
2O be equivalent to 0.01%Cr
2O
3Cr (NO
3)
39H
2O, with mean particle size be the Al of 100nm
2O
3It is medium ball milling 1 hour with water and high purity aluminium oxide ball that powder is put into ball grinder, and the salpeter solution with 0.1M before the ball milling is adjusted into 3 with the pH value, and the ball milling disposed slurry sprays into liquid nitrogen freezing, and the freeze drier inner drying obtained powder in 30 hours.The powder that makes is directly put into graphite jig with discharge plasma sintering stove sintering; Keep the vacuum of 3Pa in the stove, furnace temperature is warming up to 600 ℃ at 3 minutes internal heating, is warming up to 1200 ℃ and this temperature insulation 1 minute at 3 minutes internal heating then; 10MPa keep-ups pressure; Cooling is taken out sample, 900 ℃ of thermal treatments 8 hours when furnace temperature drops to 200 ℃.Prepared ceramics sample is an incarnadine, and straight-line luminous transmittance is 33.8% when wavelength 640nm.
Embodiment 8
In aluminum oxide is 100%, takes by weighing the Mg (NO that is equivalent to 0.5%MgO
3)
26H
2O be equivalent to 2%Cr
2O
3Cr (NO
3)
39H
2O, with mean particle size be the Al of 500nm
2O
3It is medium ball milling 2 hours with water and high purity aluminium oxide ball that powder is put into ball grinder, and the salpeter solution with 0.1M before the ball milling is adjusted into 4 with the pH value, and the ball milling disposed slurry sprays into liquid nitrogen freezing, and the freeze drier inner drying obtained powder in 90 hours.The powder that makes is directly put into graphite jig with discharge plasma sintering stove sintering; Keep the vacuum of 6Pa in the stove, furnace temperature is warming up to 600 ℃ at 4 minutes internal heating, is warming up to 1400 ℃ and this temperature insulation 10 minutes at 10 minutes internal heating then; 200MPa keep-ups pressure; Cooling is taken out sample, 1100 ℃ of thermal treatments 12 hours when furnace temperature drops to 300 ℃.Prepared crystalline ceramics sample is a scarlet, and straight-line luminous transmittance is 31.7% when wavelength 640nm.
Claims (6)
1. a fine-crystal transparent ruby pottery is characterized in that the raw material of fine-crystal transparent ruby pottery is with aluminum oxide 100 weight parts, adds 0.01-0.5 weight part MgO and 0.01-2 weight part Cr
2O3, the median size of fine-crystal transparent ruby pottery is 0.5～1 micron, the straight-line luminous transmittance of material is greater than 30% when optical wavelength is 640nm.
2. a kind of fine-crystal transparent ruby pottery according to claim 1 is characterized in that the specific density of described fine-crystal transparent ruby pottery is higher than 99.5%, and Vickers' hardness is 19～21GPa, and bending strength is 600～800MPa, and fracture toughness property is 4～5MPam
1/2
3. the preparation method of a fine-crystal transparent ruby pottery as claimed in claim 1 is characterized in that, comprises the steps:
1) MgO of 100 weight part aluminum oxide, 0.01～0.5 weight part being put into ball grinder is medium ball milling 1～2 hour with water and high purity aluminium oxide ball; Salpeter solution with 0.1M before the ball milling is adjusted into 3～4 with the pH value; 80～100 ℃ of vacuum-drying 4～5 hours is crossed 60 mesh sieves and is obtained powder;
2) powder that sieves is pressed into biscuit through isostatic cool pressing 120～250MPa after with punching block 40～70MPa dry-pressing again, biscuit is put into 750～900 ℃ of pre-burnings of box retort furnace, putting into concentration then respectively is the Cr (NO of 0.05～2M
3)
39H
2Soaked in the O solution 2～3 hours, solution is placed in the airtight Glass Containers that air pressure is 150～200Pa during immersion, takes out the biscuit that soaked and puts into slowly drying of baking oven;
3) dried biscuit is put into graphite jig with discharge plasma sintering stove sintering; Keep the vacuum of 3～6Pa in the stove, furnace temperature is warming up to 600 ℃ at 3～4 minutes internal heating, is warming up to 1200～1400 ℃ and this temperature insulation 1～10 minute at 3～10 minutes internal heating then; 10～200MPa keep-ups pressure; Cooling is taken out sample, 900～1100 ℃ of thermal treatments 8～12 hours when furnace temperature drops to 200～300 ℃.
4. the preparation method of a kind of fine-crystal transparent ruby pottery according to claim 3 is characterized in that described aluminum oxide powder purity greater than 99.99%, and the particle diameter of powder is 100～500nm, and specific surface area is 4～15m
2/ g.
5. the preparation method of a fine-crystal transparent ruby pottery as claimed in claim 1 is characterized in that, comprises the steps:
1) with 100 weight part aluminum oxide, be equivalent to the Mg (NO of 0.01～0.5 weight part MgO
3)
26H
2O be equivalent to 0.01～2 weight part Cr
2O
3Cr (NO
3)
39H
2It is medium ball milling 1～2 hour with water and high purity aluminium oxide ball that O puts into ball grinder, and slurry sprays into liquid nitrogen freezing, and the freeze drier inner drying obtained powder in 30～90 hours, and the salpeter solution with 0.1M before the ball milling is adjusted into 3～4 with the pH value;
2) powder that makes is directly put into graphite jig with discharge plasma sintering stove sintering; Keep the vacuum of 3～6Pa in the stove, furnace temperature is warming up to 600 ℃ at 3～4 minutes internal heating, is warming up to 1200～1400 ℃ and this temperature insulation 1～10 minute at 3～10 minutes internal heating then; 10～200MPa keep-ups pressure; Cooling is taken out sample, 900～1100 ℃ of thermal treatments 8～12 hours when furnace temperature drops to 200～300 ℃.
6. the preparation method of a kind of fine-crystal transparent ruby pottery according to claim 5 is characterized in that described aluminum oxide powder purity greater than 99.99%, and the particle diameter of powder is 100～500nm, and specific surface area is 4～15m
2/ g.
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| CN102581929B (en) * | 2012-02-16 | 2014-03-05 | 山东晶鑫晶体科技有限公司 | Cake forming method of high-purity alumina powder |
| CN105239161B (en) * | 2015-10-19 | 2018-06-26 | 中国科学院青海盐湖研究所 | The preparation method of ruby crystal |
| CN105645987B (en) * | 2016-01-20 | 2018-07-03 | 西北工业大学 | A kind of method of electric field-assisted low temperature Fast Sintering porous ceramics |
| CN107188543A (en) * | 2016-03-15 | 2017-09-22 | 中国科学院上海硅酸盐研究所 | Cr2O3/ ZTA composite granules and ceramics and preparation method thereof |
| CN106966704A (en) * | 2017-02-28 | 2017-07-21 | 梧州市东麟宝石机械有限公司 | One kind synthesis ruby preparation method of dove blood |
| CN112125661A (en) * | 2020-09-04 | 2020-12-25 | 临沂金成电子有限公司 | Low-temperature co-fired microwave ceramic dielectric material and preparation method thereof |
| CN116283240A (en) * | 2023-03-28 | 2023-06-23 | 苏州芯合半导体材料有限公司 | Ruby type high-strength Cr-ZTA ceramic material and preparation method thereof |
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