CN101628811A - Transparent ceramic and preparation method thereof - Google Patents
Transparent ceramic and preparation method thereof Download PDFInfo
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- CN101628811A CN101628811A CN200910056445A CN200910056445A CN101628811A CN 101628811 A CN101628811 A CN 101628811A CN 200910056445 A CN200910056445 A CN 200910056445A CN 200910056445 A CN200910056445 A CN 200910056445A CN 101628811 A CN101628811 A CN 101628811A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 44
- 239000002994 raw material Substances 0.000 claims abstract description 40
- 238000005245 sintering Methods 0.000 claims abstract description 26
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 11
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 5
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 5
- MMKQUGHLEMYQSG-UHFFFAOYSA-N oxygen(2-);praseodymium(3+) Chemical compound [O-2].[O-2].[O-2].[Pr+3].[Pr+3] MMKQUGHLEMYQSG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 4
- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims abstract 2
- 229940075624 ytterbium oxide Drugs 0.000 claims abstract 2
- 239000011222 crystalline ceramic Substances 0.000 claims description 145
- 229910002106 crystalline ceramic Inorganic materials 0.000 claims description 145
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 10
- 238000005469 granulation Methods 0.000 claims description 8
- 230000003179 granulation Effects 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 4
- GWYXTVGANSBRNB-UHFFFAOYSA-N terbium(iii) oxide Chemical compound O=[Tb]O[Tb]=O GWYXTVGANSBRNB-UHFFFAOYSA-N 0.000 claims description 4
- -1 trioxide Chemical compound 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 27
- 229910021420 polycrystalline silicon Inorganic materials 0.000 abstract description 9
- 229910021421 monocrystalline silicon Inorganic materials 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 229910052747 lanthanoid Inorganic materials 0.000 abstract description 2
- 150000002602 lanthanoids Chemical class 0.000 abstract description 2
- ZIKATJAYWZUJPY-UHFFFAOYSA-N thulium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Tm+3].[Tm+3] ZIKATJAYWZUJPY-UHFFFAOYSA-N 0.000 abstract 2
- 238000000498 ball milling Methods 0.000 abstract 1
- 238000009694 cold isostatic pressing Methods 0.000 abstract 1
- 229910003447 praseodymium oxide Inorganic materials 0.000 abstract 1
- 229910003451 terbium oxide Inorganic materials 0.000 abstract 1
- SCRZPWWVSXWCMC-UHFFFAOYSA-N terbium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Tb+3].[Tb+3] SCRZPWWVSXWCMC-UHFFFAOYSA-N 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 229920005591 polysilicon Polymers 0.000 description 8
- 229910052710 silicon Inorganic materials 0.000 description 8
- 239000010703 silicon Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 230000005281 excited state Effects 0.000 description 4
- 239000002241 glass-ceramic Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 230000009466 transformation Effects 0.000 description 4
- 230000010307 cell transformation Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000695 excitation spectrum Methods 0.000 description 3
- 238000002189 fluorescence spectrum Methods 0.000 description 3
- 230000005283 ground state Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- 238000007908 dry granulation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000002110 toxicologic effect Effects 0.000 description 2
- 231100000027 toxicology Toxicity 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- FRNOGLGSGLTDKL-UHFFFAOYSA-N thulium atom Chemical compound [Tm] FRNOGLGSGLTDKL-UHFFFAOYSA-N 0.000 description 1
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- Inorganic Insulating Materials (AREA)
Abstract
一种透明陶瓷及其制备方法，该透明陶瓷的结构式为：LnxYbyY(3－x－y)Al5O12或LnwYbzY(2－w－z)O3，其中，0.003≤x≤0.03，0.006≤y≤1.5，0.002≤w≤0.02，0.004≤z≤1，Ln代表Ce、Tm、Pr或Tb镧系元素。制备方法是：采用纯度不低于99.9％的氧化钇、氧化铝、氧化镱，再选取氧化铈、氧化铥、氧化镨或氧化铽的氧化物粉末中的一种为原料，按透明陶瓷的结构式的组成配置粉体原料，用湿法球磨以无水乙醇为介质制备陶瓷粉料，粉料烘干后造粒、压片，施以200MPa以上冷等静压成坯体；最后放入真空烧结炉中烧结获得LnxYbyY(3－x－y)Al5O12、LnwYbzY(2－w－z)O3透明陶瓷。可以提高单晶硅和多晶硅太阳能电池的转化效率。
A transparent ceramic and a preparation method thereof . The transparent ceramic has a structural formula of LnxYbyY (3-x-y) Al5O12 or LnwYbzY (2-w-z) O3 , wherein 0.003≤x≤0.03, 0.006≤y≤1.5, 0.002≤w≤0.02, 0.004≤z≤1, and Ln represents Ce, Tm, Pr or Tb lanthanide elements. The preparation method comprises: using yttrium oxide, aluminum oxide and ytterbium oxide with a purity of not less than 99.9%, and then selecting one of the oxide powders of cerium oxide, thulium oxide, praseodymium oxide or terbium oxide as raw materials, configuring the powder raw materials according to the composition of the transparent ceramic structure, preparing ceramic powder by wet ball milling with anhydrous ethanol as the medium, granulating and tableting the powder after drying, applying cold isostatic pressing at more than 200MPa to form a green body; finally, sintering in a vacuum sintering furnace to obtain LnxYbyY (3-x-y) Al5O12 , LnwYbzY (2-w- z ) O3 transparent ceramics. The conversion efficiency of single crystal silicon and polycrystalline silicon solar cells can be improved.
Description
Technical field
The present invention relates to crystalline ceramics, particularly a kind of crystalline ceramics and preparation method thereof.
Background technology
The electricity conversion that improves solar cell is the target that people are pursued all the time.A major reason of restriction silicon single crystal and polysilicon solar cell transformation efficiency is exactly that its corresponding wave band of strong spectral is near infrared region, and the high-amplitude wave section of solar radiation is positioned at visible-range, silicon single crystal and polysilicon solar cell can produce the thermalization effect of current carrier and cause the reduction of transformation efficiency after absorbing the higher light photon of energy.At the problems referred to above, the mode that people have proposed to adopt cooperation to change down is converted into two near infrared light photons with a light photon, improves the transformation efficiency of silicon single crystal and polysilicon solar cell with this.That research is maximum at present is Yb
3+Ion and other lanthanide metal ion (trivalent cerium (Ce
3+), thulium (Tm
3+), praseodymium (Pr
3+), terbium (Tb
3+) etc., be designated as Ln
3+) mix in a certain matrix Ln altogether
3+(400～500nm) energy is delivered to two Yb by the mode of cooperating down conversion to the optical photon that ion absorbed
3+Ionic
2F
5/2Excited state, and then realize Yb
3+Ionic is efficiently luminous, Yb
3+The ionoluminescence wavelength is in 970～1100nm scope, just corresponding to the strongest response of the spectrum district of silicon single crystal and polysilicon solar cell.The concrete mechanism that above-mentioned energy shifts has play-by-play in reference 1,2.(document 1, Q.Y.Zhang, G.F.Yang and Z.H.Jiang, Applied Physics Letters 91,051903 (2007); Document 2, Daqin Chen, Yuansheng Wang, Yunlong Yu, Ping Huang andFangyi Weng, Journal of Applied Physics 104,116105 (2008)).
Why select Yb
3+And Ln
3+Mix altogether be because:
(1) Yb
3+Ion only has two atomic states, ground state
2F
7/2And excited state
2F
5/2, it is about 10 to be separated by, 000cm
-1(=1000nm), higher excited state in the 5d configuration, with ground state at a distance of about 100,000cm
-1, this simple level structure makes Yb
3+Ion itself does not exist excited state absorption and up-conversion luminescence.In addition, Yb
3+Ion has very high fluorescence quantum efficiency (being about 0.91).
(2) above-mentioned several Ln
3+The energy of ionic absorption visible light is approximately Yb
3+The twice of energy gap between ion ground state and excited state makes cooperation down-conversion luminescence to realize.
The cooperation energy transfer process of conversion down is the process that a light photon is converted into two infrared light photons, thereby can effectively improve the transformation efficiency of silicon single crystal and polysilicon solar cell.But present design is based on fluorescent material, oxyfluoride glass ceramic mostly, also produced corresponding problem thus in use: fluorescent material itself has stronger scattering to light, it can be converted into two near infrared photons with an optical photon on the one hand, but greatly reduce the transmitance of sunlight but then, so actual effect loses more than gain probably.Though it is oxyfluoride glass ceramic can obtain higher transmittance, harmful to human body and environment in its component because of containing fluorochemical.In addition, the uvioresistant Radiation Characteristics of fluorescent material and oxyfluoride glass ceramic is relative relatively poor, and is easily aging.
As the development of material science in recent years branch faster, crystalline ceramics can have very high transmitance (＞80%) in ultraviolet-visible-infrared light scope, and has good physical and chemical stability and machining property preferably.Therefore, crystalline ceramics probably becomes the Applied Materials that is used to improve silicon single crystal and polysilicon solar cell transformation efficiency.
Summary of the invention
The objective of the invention is in order to improve silicon single crystal and the polysilicon solar cell transformation efficiency provides a kind of crystalline ceramics and preparation method thereof, this crystalline ceramics has low cost, to the human body toxicological harmless, the advantage of environmentally safe, in addition, compare fluorescent material and oxyfluoride glass ceramic, the uvioresistant Radiation Characteristics of crystalline ceramics also will be got well a lot.
Technical solution of the present invention is as follows:
A kind of crystalline ceramics, the structural formula of this crystalline ceramics is: Ln
xYb
yY
(3-x-y)Al
5O
12Or Ln
wYb
zY
(2-w-z)O
3, wherein, 0.003≤x≤0.03,0.006≤y≤1.5,0.002≤w≤0.02,0.004≤z≤1, Ln represents Ce, Tm, Pr or Tb lanthanon.
The preparation method of above-mentioned crystalline ceramics comprises the following steps:
1. select the structural formula Ln of crystalline ceramics to be prepared
xYb
yY
(3-x-y)Al
5O
12Or Ln
wYb
zY
(2-w-z)O
3And respective x, y, w, z and concrete Ln element;
2. adopt purity to be not less than 99.9% yttrium oxide (Y
2O
3), aluminum oxide (Al
2O
3), ytterbium oxide (Yb
2O
3), choose cerium oxide (CeO again
2), trioxide (Tm
2O
3), Praseodymium trioxide (Pr
6O
11) or terbium sesquioxide (Tb
4O
7) a kind of in the oxide powder be raw material, by the stoicheiometry configuration powder raw material of selected structural formula;
3. with the 2. the raw material in step put into ball grinder, be that medium prepares ceramic powder with the dehydrated alcohol with wet ball grinding, powder carries out granulation, compressing tablet after drying;
4. the isostatic cool pressing that compressing tablet is imposed more than the 200MPa becomes base substrate;
5. putting into vacuum sintering furnace at last carries out sintering and obtains to have Ln under following condition
xYb
yY
(3-x-y)Al
5O
12Or Ln
wYb
zY
(2-w-z)O
3The crystalline ceramics of structure:
(a) be Ln to structural formula
xYb
yY
(3-x-y)Al
5O
12Base substrate, the holding temperature during vacuum sintering is 1600～1750 ℃, soaking time is 5～30 hours, vacuum tightness is better than 3 * 10
-3Pa;
(b) be Ln to structural formula
wYb
zY
(2-w-z)O
3Ceramic body, the holding temperature during vacuum sintering is 1750～2150 ℃, soaking time is 5～30 hours, vacuum tightness is better than 3 * 10
-3Pa.
Technique effect of the present invention:
Experiment shows, crystalline ceramics of the present invention has good transmitance in ultraviolet-visible light-infra-red range, toxicological harmless is pollution-free, and can effectively the part light photon be converted into the near infrared photon of double amount, can improve the transformation efficiency of silicon single crystal and polysilicon solar cell, and its preparation technology is also fairly simple.
Description of drawings
Fig. 1 is the prepared Ce of the embodiment of the invention 1
0.03Yb
1.5Y
1.47Al
5O
12The transmittance curve of crystalline ceramics (thickness is 1mm).
Fig. 2 is embodiment of the invention 1Ce
0.03Yb
1.5Y
1.47Al
5O
12The excitation spectrum of crystalline ceramics and fluorescence spectrum.
Embodiment
The invention will be further described below in conjunction with embodiment and accompanying drawing, but should not limit protection scope of the present invention with this.
Embodiment 1
Employing purity is 99.9% yttrium oxide (Y
2O
3), aluminum oxide (Al
2O
3), ytterbium oxide (Yb
2O
3) and cerium oxide (CeO
2) powder is raw material, presses Ce
0.003Yb
0.006Y
2.991Al
5O
12Composition configuration powder raw material, the back is that medium prepares ceramic powder with the dehydrated alcohol with wet ball grinding, powder oven dry granulation afterwards, compressing tablet; Subsequently it is imposed the above isostatic cool pressing of 200MPa; Put into vacuum sintering furnace at last in 1600 ℃ of sintering 5 hours, the vacuum tightness in sintered heat insulating stage is 2.5 * 10
-3Pa obtains Ce
0.003Yb
0.006Y
2.991Al
5O
12Crystalline ceramics.
This crystalline ceramics experimentizes, and obtains the experimental result as Fig. 1 and Fig. 2: Fig. 1 and be the prepared Ce of the embodiment of the invention 1
0.03Yb
1.5Y
1.47Al
5O
12The transmittance curve of crystalline ceramics (thickness is 1mm), the absorption band that wherein is positioned at 200～350nm, 400～500nm place corresponds respectively to Ce
3+Ionic 4f → 5d
2, 4f → 5d
1Transition; The absorption band at 850～1040nm place is corresponding to Yb
3+Ionic
2F
7/2→
2F
5/2Transition.Except that absorption band, this crystalline ceramics is about 80% in the transmitance of ultraviolet-visible-infra-red range.
Fig. 2 is embodiment of the invention 1Ce
0.03Yb
1.5Y
1.47Al
5O
12The excitation spectrum of crystalline ceramics and fluorescence spectrum.In excitation spectrum, the monitoring wavelength is Yb
3+Ionic 1028nm's is luminous, can observe excitation peak at 400～500nm place, has illustrated by Ce
3+Ion is to Yb
3+Energy of ions shifts; In fluorescence spectrum, adopt blue-light excited this sample of 457nm can observe Yb
3+Ion is at the emission peak at 1028nm place, and this has also proved the existence of above-mentioned energy transfer process.
Embodiment 2
The sintered heat insulating temperature is 1750 ℃, and other conditions can obtain Ce equally with embodiment 1
0.003Yb
0.006Y
2.991Al
5O
12Crystalline ceramics.
Embodiment 3
The sintered heat insulating temperature is 1650 ℃, and other conditions can obtain Ce equally with embodiment 1
0.003Yb
0.006Y
2.991Al
5O
12Crystalline ceramics.
Embodiment 4
The sintered heat insulating time is 30 hours, and other conditions can obtain Ce equally with embodiment 1
0.003Yb
0.006Y
2.991Al
5O
12Crystalline ceramics.
Embodiment 5
The sintered heat insulating time is 20 hours, and other conditions can obtain Ce equally with embodiment 1
0.003Yb
0.006Y
2.991Al
5O
12Crystalline ceramics.
Embodiment 6
Press Ce
0.02Yb
0.04Y
2.94Al
5O
12Composition configuration raw material, other conditions obtain Ce with embodiment 1
0.02Yb
0.04Y
2.94Al
5O
12Crystalline ceramics.
Embodiment 7
The sintered heat insulating temperature is 1750 ℃, and other conditions can obtain Ce equally with embodiment 6
0.02Yb
0.04Y
2.94Al
5O
12Crystalline ceramics.
Embodiment 8
The sintered heat insulating temperature is 1650 ℃, and other conditions can obtain Ce equally with embodiment 6
0.02Yb
0.04Y
2.94Al
5O
12Crystalline ceramics.
Embodiment 9
The sintered heat insulating time is 30 hours, and other conditions can obtain Ce equally with embodiment 6
0.02Yb
0.04Y
2.94Al
5O
12Crystalline ceramics.
Embodiment 10
The sintered heat insulating time is 20 hours, and other conditions can obtain Ce equally with embodiment 6
0.02Yb
0.04Y
2.94Al
5O
12Crystalline ceramics.
Embodiment 11
Press Ce
0.03Yb
1.5Y
1.47Al
5O
12Composition configure raw material, other conditions are with embodiment 1, obtain Ce
0.03Yb
1.5Y
1.47Al
5O
12Crystalline ceramics.
Embodiment 12
The sintered heat insulating temperature is 1750 ℃, and other conditions can obtain Ce equally with embodiment 11
0.03Yb
1.5Y
1.47Al
5O
12Crystalline ceramics.
Embodiment 13
The sintered heat insulating temperature is 1650 ℃, and other conditions can obtain Ce equally with embodiment 11
0.03Yb
1.5Y
1.47Al
5O
12Crystalline ceramics.
Embodiment 14
The sintered heat insulating time is 30 hours, and other conditions can obtain Ce equally with embodiment 11
0.03Yb
1.5Y
1.47Al
5O
12Crystalline ceramics.
Embodiment 15
The sintered heat insulating time is 20 hours, and other conditions can obtain Ce equally with embodiment 11
0.03Yb
1.5Y
1.47Al
5O
12Crystalline ceramics.
Embodiment 16
Employing purity is 99.99% yttrium oxide (Y
2O
3), aluminum oxide (Al
2O
3), ytterbium oxide (Yb
2O
3) and trioxide (Tm
2O
3) powder is raw material, presses Tm
0.003Yb
0.03Y
2.967Al
5O
12Composition configuration powder raw material, the back is that medium prepares ceramic powder with the dehydrated alcohol with wet ball grinding, powder oven dry granulation afterwards, compressing tablet; Subsequently it is imposed the above isostatic cool pressing of 200MPa; Put into vacuum sintering furnace at last in 1600 ℃ of sintering 5 hours, the vacuum tightness in sintered heat insulating stage is 1 * 10
-3Pa obtains Tm
0.003Yb
0.03Y
2.967Al
5O
12Crystalline ceramics.
Embodiment 17
The sintered heat insulating temperature is 1750 ℃, and other conditions can obtain Tm equally with embodiment 16
0.003Yb
0.03Y
2.967Al
5O
12Crystalline ceramics.
Embodiment 18
The sintered heat insulating temperature is 1650 ℃, and other conditions can obtain Tm equally with embodiment 16
0.003Yb
0.03Y
2.967Al
5O
12Crystalline ceramics.
Embodiment 19
The sintered heat insulating time is 30 hours, and other conditions can obtain Tm equally with embodiment 16
0.003Yb
0.03Y
2.967Al
5O
12Crystalline ceramics.
Embodiment 20
The sintered heat insulating time is 20 hours, and other conditions can obtain Tm equally with embodiment 16
0.003Yb
0.03Y
2.967Al
5O
12Crystalline ceramics.
Embodiment 21
Press Tm
0.02Yb
0.2Y
2.78Al
5O
12Composition configure raw material, other conditions are with embodiment 16, obtain Tm
0.02Yb
0.2Y
2.78Al
5O
12Crystalline ceramics.
Embodiment 22
The sintered heat insulating temperature is 1750 ℃, and other conditions can obtain Tm equally with embodiment 21
0.02Yb
0.2Y
2.78Al
5O
12Crystalline ceramics.
Embodiment 23
The sintered heat insulating temperature is 1650 ℃, and other conditions can obtain Tm equally with embodiment 21
0.02Yb
0.2Y
2.78Al
5O
12Crystalline ceramics.
Embodiment 24
The sintered heat insulating time is 30 hours, and other conditions can obtain Tm equally with embodiment 21
0.02Yb
0.2Y
2.78Al
5O
12Crystalline ceramics.
Embodiment 25
The sintered heat insulating time is 20 hours, and other conditions can obtain Tm equally with embodiment 21
0.02Yb
0.2Y
2.78Al
5O
12Crystalline ceramics.
Embodiment 26
Press Tm
0.03Yb
1.5Y
1.47Al
5O
12Composition configure raw material, other conditions are with embodiment 16, obtain Tm
0.03Yb
1.5Y
1.47Al
5O
12Crystalline ceramics.
Embodiment 27
The sintered heat insulating temperature is 1750 ℃, and other conditions can obtain Tm equally with embodiment 26
0.03Yb
1.5Y
1.47Al
5O
12Crystalline ceramics.
Embodiment 28
The sintered heat insulating temperature is 1650 ℃, and other conditions can obtain Tm equally with embodiment 26
0.03Yb
1.5Y
1.47Al
5O
12Crystalline ceramics.
Embodiment 29
The sintered heat insulating time is 30 hours, and other conditions can obtain Tm equally with embodiment 26
0.03Yb
1.5Y
1.47Al
5O
12Crystalline ceramics.
Embodiment 30
The sintered heat insulating time is 20 hours, and other conditions can obtain Tm equally with embodiment 26
0.03Yb
1.5Y
1.47Al
5O
12Crystalline ceramics.
Embodiment 31
Employing purity is 99.999% yttrium oxide (Y
2O
3), aluminum oxide (Al
2O
3), ytterbium oxide (Yb
2O
3) and Praseodymium trioxide (Pr
6O
11) powder is raw material, presses Pr
0.003Yb
0.03Y
2.967Al
5O
12Composition configure powder raw material, the back is that medium prepares ceramic powder with the dehydrated alcohol with wet ball grinding, powder is dried after granulation, compressing tablet; The back imposes the above isostatic cool pressing of 200MPa to it and makes base substrate; Put into vacuum sintering furnace at last in 1600 ℃ of sintering 5 hours, the vacuum tightness in sintered heat insulating stage is 2 * 10
-3Pa obtains Pr
0.003Yb
0.03Y
2.967Al
5O
12Crystalline ceramics.
Embodiment 32
The sintered heat insulating temperature is 1750 ℃, and other conditions can obtain Pr equally with embodiment 31
0.003Yb
0.03Y
2.967Al
5O
12Crystalline ceramics.
Embodiment 33
The sintered heat insulating temperature is 1650 ℃, and other conditions can obtain Pr equally with embodiment 31
0.003Yb
0.03Y
2.967Al
5O
12Crystalline ceramics.
Embodiment 34
The sintered heat insulating time is 30 hours, and other conditions can obtain Pr equally with embodiment 31
0.003Yb
0.03Y
2.967Al
5O
12Crystalline ceramics.
Embodiment 35
The sintered heat insulating time is 20 hours, and other conditions can obtain Pr equally with embodiment 31
0.003Yb
0.03Y
2.967Al
5O
12Crystalline ceramics.
Embodiment 36
Press Pr
0.03Yb
1Y
2.97Al
5O
12Composition configure raw material, other conditions are with embodiment 31, obtain Pr
0.03Yb
1Y
2.97Al
5O
12Crystalline ceramics.
Embodiment 37
The sintered heat insulating temperature is 1750 ℃, and other conditions can obtain Pr equally with embodiment 36
0.03Yb
1Y
2.97Al
5O
12Crystalline ceramics.
Embodiment 38
The sintered heat insulating temperature is 1650 ℃, and other conditions can obtain Pr equally with embodiment 36
0.03Yb
1Y
2.97Al
5O
12Crystalline ceramics.
Embodiment 39
The sintered heat insulating time is 30 hours, and other conditions can obtain Pr equally with embodiment 36
0.03Yb
1Y
2.97Al
5O
12Crystalline ceramics.
Embodiment 40
The sintered heat insulating time is 20 hours, and other conditions can obtain Pr equally with embodiment 36
0.03Yb
1Y
2.97Al
5O
12Crystalline ceramics.
Embodiment 41
Press Pr
0.03Yb
1.5Y
1.47Al
5O
12Composition configure raw material, other conditions are with embodiment 31, obtain Pr
0.03Yb
1.5Y
1.47Al
5O
12Crystalline ceramics.
Embodiment 42
The sintered heat insulating temperature is 1750 ℃, and other conditions can obtain Pr equally with embodiment 41
0.03Yb
1Y
2.97Al
5O
12Crystalline ceramics.
Embodiment 43
The sintered heat insulating temperature is 1650 ℃, and other conditions can obtain Pr equally with embodiment 41
0.03Yb
1Y
2.97Al
5O
12Crystalline ceramics.
Embodiment 44
The sintered heat insulating time is 30 hours, and other conditions can obtain Pr equally with embodiment 41
0.03Yb
1Y
2.97Al
5O
12Crystalline ceramics.
Embodiment 45
The sintered heat insulating time is 20 hours, and other conditions can obtain Pr equally with embodiment 41
0.03Yb
1Y
2.97Al
5O
12Crystalline ceramics.
Embodiment 46
Employing purity is 99.9% yttrium oxide (Y
2O
3), aluminum oxide (Al
2O
3), ytterbium oxide (Yb
2O
3) and terbium sesquioxide (Tb
4O
7) powder is raw material, presses Tb
0.003Yb
0.03Y
2.967Al
5O
12Composition configure powder raw material, the back is that medium prepares ceramic powder with the dehydrated alcohol with wet ball grinding, powder is dried after granulation, compressing tablet; The back imposes the above isostatic cool pressing of 200MPa to it and makes base substrate; Put into vacuum sintering furnace at last in 1600 ℃ of sintering 5 hours, the vacuum tightness in sintered heat insulating stage is 3 * 10
-3Pa obtains Tb
0.003Yb
0.03Y
2.967Al
5O
12Crystalline ceramics.
Embodiment 47
The sintered heat insulating temperature is 1750 ℃, and other conditions can obtain Tb equally with embodiment 46
0.003Yb
0.03Y
2.967Al
5O
12Crystalline ceramics.
Embodiment 48
The sintered heat insulating temperature is 1650 ℃, and other conditions can obtain Tb equally with embodiment 46
0.003Yb
0.03Y
2.967Al
5O
12Crystalline ceramics.
Embodiment 49
The sintered heat insulating time is 30 hours, and other conditions can obtain Tb equally with embodiment 46
0.003Yb
0.03Y
2.967Al
5O
12Crystalline ceramics.
Embodiment 50
The sintered heat insulating time is 20 hours, and other conditions can obtain Tb equally with embodiment 46
0.003Yb
0.03Y
2.967Al
5O
12Crystalline ceramics.
Embodiment 51
Press Tb
0.03Yb
1Y
2.97Al
5O
12Composition configure raw material, other conditions are with embodiment 46, obtain Tb
0.03Yb
1Y
2.97Al
5O
12Crystalline ceramics.
Embodiment 52
The sintered heat insulating temperature is 1750 ℃, and other conditions can obtain Tb equally with embodiment 51
0.03Yb
1Y
2.97Al
5O
12Crystalline ceramics.
Embodiment 53
The sintered heat insulating temperature is 1650 ℃, and other conditions can obtain Tb equally with embodiment 51
0.03Yb
1Y
2.97Al
5O
12Crystalline ceramics.
Embodiment 54
The sintered heat insulating time is 30 hours, and other conditions can obtain Tb equally with embodiment 51
0.03Yb
1Y
2.97Al
5O
12Crystalline ceramics.
Embodiment 55
The sintered heat insulating time is 20 hours, and other conditions can obtain Tb equally with embodiment 51
0.03Yb
1Y
2.97Al
5O
12Crystalline ceramics.
Embodiment 56
Press Tb
0.03Yb
1.5Y
1.47Al
5O
12Composition configure raw material, other conditions are with embodiment 46, obtain Tb
0.03Yb
1.5Y
1.47Al
5O
12Crystalline ceramics.
Embodiment 57
The sintered heat insulating temperature is 1750 ℃, and other conditions can obtain Tb equally with embodiment 56
0.03Yb
1.5Y
1.47Al
5O
12Crystalline ceramics.
Embodiment 58
The sintered heat insulating temperature is 1650 ℃, and other conditions can obtain Tb equally with embodiment 56
0.03Yb
1.5Y
1.47Al
5O
12Crystalline ceramics.
Embodiment 59
The sintered heat insulating time is 30 hours, and other conditions can obtain Tb equally with embodiment 56
0.03Yb
1.5Y
1.47Al
5O
12Crystalline ceramics.
Embodiment 60
The sintered heat insulating time is 20 hours, and other conditions can obtain Tb equally with embodiment 56
0.03Yb
1.5Y
1.47Al
5O
12Crystalline ceramics.
Embodiment 61
Employing purity is 99.99% yttrium oxide (Y
2O
3), ytterbium oxide (Yb
2O
3) and cerium oxide (CeO
2) powder is raw material, presses Ce
0.002Yb
0.004Y
1.994O
3Composition configure powder raw material, the back is that medium prepares ceramic powder with the dehydrated alcohol with wet ball grinding, the back granulation of powder oven dry, compressing tablet; Subsequently it is imposed the above isostatic cool pressing of 200MPa; Put into vacuum sintering furnace at last in 1750 ℃ of sintering 5 hours, the vacuum tightness in sintered heat insulating stage is 2.5 * 10
-3Pa obtains Ce
0.002Yb
0.004Y
1.994O
3Crystalline ceramics.
Embodiment 62
The sintered heat insulating temperature is 2150 ℃, and other conditions can obtain Ce equally with embodiment 61
0.002Yb
0.004Y
1.994O
3Crystalline ceramics.
Embodiment 63
The sintered heat insulating temperature is 1850 ℃, and other conditions can obtain Ce equally with embodiment 61
0.002Yb
0.004Y
1.994O
3Crystalline ceramics.
Embodiment 64
The sintered heat insulating time is 30 hours, and other conditions can obtain Ce equally with embodiment 61
0.002Yb
0.004Y
1.994O
3Crystalline ceramics.
Embodiment 65
The sintered heat insulating time is 20 hours, and other conditions can obtain Ce equally with embodiment 61
0.002Yb
0.004Y
1.994O
3Crystalline ceramics.
Embodiment 66
Press Ce
0.005Yb
0.25Y
1.745O
3Composition configure raw material, other conditions are with embodiment 46, obtain Ce
0.005Yb
0.25Y
1.745O
3Crystalline ceramics.
Embodiment 67
The sintered heat insulating temperature is 2150 ℃, and other conditions can obtain Ce equally with embodiment 66
0.005Yb
0.25Y
1.745O
3Crystalline ceramics.
Embodiment 68
The sintered heat insulating temperature is 1850 ℃, and other conditions can obtain Ce equally with embodiment 66
0.005Yb
0.25Y
1.745O
3Crystalline ceramics.
Embodiment 69
The sintered heat insulating time is 30 hours, and other conditions can obtain Ce equally with embodiment 66
0.005Yb
0.25Y
1.745O
3Crystalline ceramics.
Embodiment 70
The sintered heat insulating time is 20 hours, and other conditions can obtain Ce equally with embodiment 56
0.005Yb
0.25Y
1.745O
3Crystalline ceramics.
Embodiment 71
Press Ce
0.01Yb
1Y
0.99O
3Composition configure raw material, other conditions are with embodiment 66, obtain Ce
0.01Yb
1Y
0.99O
3Crystalline ceramics.
Embodiment 72
The sintered heat insulating temperature is 2150 ℃, and other conditions can obtain Ce equally with embodiment 71
0.01Yb
1Y
0.99O
3Crystalline ceramics.
Embodiment 73
The sintered heat insulating temperature is 1850 ℃, and other conditions can obtain Ce equally with embodiment 71
0.01Yb
1Y
0.99O
3Crystalline ceramics.
Embodiment 74
The sintered heat insulating time is 30 hours, and other conditions can obtain Ce equally with embodiment 71
0.01Yb
1Y
0.99O
3Crystalline ceramics.
Embodiment 75
The sintered heat insulating time is 20 hours, and other conditions can obtain Ce equally with embodiment 71
0.01Yb
1Y
0.99O
3Crystalline ceramics.
Embodiment 76
Employing purity is 99.999% yttrium oxide (Y
2O
3), ytterbium oxide (Yb
2O
3) and trioxide (Tm
2O
3) powder is raw material, presses Tm
0.002Yb
0.004Y
1.994O
3Composition configure powder raw material, the back is that medium prepares ceramic powder with the dehydrated alcohol with wet ball grinding, the back granulation of powder oven dry, compressing tablet; Subsequently it is imposed the above isostatic cool pressing of 200MPa; Put into vacuum sintering furnace at last in 1750 ℃ of sintering 5 hours, the vacuum tightness in sintered heat insulating stage is 1 * 10
-3Pa obtains Tm
0.002Yb
0.004Y
1.994O
3Crystalline ceramics.
Embodiment 77
The sintered heat insulating temperature is 2150 ℃, and other conditions can obtain Tm equally with embodiment 76
0.002Yb
0.004Y
1.994O
3Crystalline ceramics.
Embodiment 78
The sintered heat insulating temperature is 1850 ℃, and other conditions can obtain Tm equally with embodiment 76
0.002Yb
0.004Y
1.994O
3Crystalline ceramics.
Embodiment 79
The sintered heat insulating time is 30 hours, and other conditions can obtain Tm equally with embodiment 76
0.002Yb
0.004Y
1.994O
3Crystalline ceramics.
Embodiment 80
The sintered heat insulating time is 20 hours, and other conditions can obtain Tm equally with embodiment 76
0.002Yb
0.004Y
1.994O
3Crystalline ceramics.
Embodiment 81
Press Tm
0.0025Yb
0.05Y
1.925O
3Composition configure raw material, other conditions are with embodiment 76, obtain Tm
0.0025Yb
0.05Y
1.925O
3Crystalline ceramics.
Embodiment 82
The sintered heat insulating temperature is 2150 ℃, and other conditions can obtain Tm equally with embodiment 81
0.0025Yb
0.05Y
1.925O
3Crystalline ceramics.
Embodiment 83
The sintered heat insulating temperature is 1850 ℃, and other conditions can obtain Tm equally with embodiment 81
0.0025Yb
0.05Y
1.925O
3Crystalline ceramics.
Embodiment 84
The sintered heat insulating time is 30 hours, and other conditions can obtain Tm equally with embodiment 81
0.0025Yb
0.05Y
1.925O
3Crystalline ceramics.
Embodiment 85
The sintered heat insulating time is 20 hours, and other conditions can obtain Tm equally with embodiment 81
0.0025Yb
0.05Y
1.925O
3Crystalline ceramics.
Embodiment 86
Press Tm
0.01Yb
1Y
0.99O
3Composition configure raw material, other conditions are with embodiment 76, obtain Tm
0.01Yb
1Y
0.99O
3Crystalline ceramics.
Embodiment 87
The sintered heat insulating temperature is 2150 ℃, and other conditions can obtain Tm equally with embodiment 86
0.01Yb
1Y
0.99O
3Crystalline ceramics.
Embodiment 88
The sintered heat insulating temperature is 1850 ℃, and other conditions can obtain Tm equally with embodiment 86
0.01Yb
1Y
0.99O
3Crystalline ceramics.
Embodiment 89
The sintered heat insulating time is 30 hours, and other conditions can obtain Tm equally with embodiment 86
0.01Yb
1Y
0.99O
3Crystalline ceramics.
Embodiment 90
The sintered heat insulating time is 20 hours, and other conditions can obtain Tm equally with embodiment 86
0.01Yb
1Y
0.99O
3Crystalline ceramics.
Embodiment 91
Employing purity is 99.99% yttrium oxide (Y
2O
3), ytterbium oxide (Yb
2O
3) and Praseodymium trioxide (Pr
6O
11) powder is raw material, presses Pr
0.002Yb
0.004Y
1.994O
3Composition configure powder raw material, the back is that medium prepares ceramic powder with the dehydrated alcohol with wet ball grinding, powder is dried after granulation, compressing tablet; Subsequently it is imposed the above isostatic cool pressing of 200MPa; Put into vacuum sintering furnace at last in 1750 ℃ of sintering 5 hours, the vacuum tightness in sintered heat insulating stage is 2 * 10
-3Pa obtains Pr
0.002Yb
0.004Y
1.994O
3Crystalline ceramics.
Embodiment 92
The sintered heat insulating temperature is 2150 ℃, and other conditions can obtain Pr equally with embodiment 91
0.002Yb
0.004Y
1.994O
3Crystalline ceramics.
Embodiment 93
The sintered heat insulating temperature is 1850 ℃, and other conditions can obtain Pr equally with embodiment 91
0.002Yb
0.004Y
1.994O
3Crystalline ceramics.
Embodiment 94
The sintered heat insulating time is 30 hours, and other conditions can obtain Pr equally with embodiment 91
0.002Yb
0.004Y
1.994O
3Crystalline ceramics.
Embodiment 95
The sintered heat insulating time is 20 hours, and other conditions can obtain Pr equally with embodiment 91
0.002Yb
0.004Y
1.994O
3Crystalline ceramics.
Embodiment 96
Press Pr
0.006Yb
0.012Y
1.982O
3Composition configure raw material, other conditions are with embodiment 91, obtain Pr
0.006Yb
0.012Y
1.982O
3Crystalline ceramics.
Embodiment 97
The sintered heat insulating temperature is 2150 ℃, and other conditions can obtain Pr equally with embodiment 96
0.006Yb
0.012Y
1.982O
3Crystalline ceramics.
Embodiment 98
The sintered heat insulating temperature is 1850 ℃, and other conditions can obtain Pr equally with embodiment 96
0.006Yb
0.012Y
1.982O
3Crystalline ceramics.
Embodiment 99
The sintered heat insulating time is 30 hours, and other conditions can obtain Pr equally with embodiment 96
0.006Yb
0.012Y
1.982O
3Crystalline ceramics.
Embodiment 100
The sintered heat insulating time is 20 hours, and other conditions can obtain Pr equally with embodiment 96
0.006Yb
0.012Y
1.982O
3Crystalline ceramics.
Embodiment 101
Press Pr
0.01Yb
1Y
0.99O
3Composition configure raw material, other conditions are with embodiment 91, obtain Pr
0.01Yb
1Y
0.99O
3Crystalline ceramics.
Embodiment 102
The sintered heat insulating temperature is 2150 ℃, and other conditions can obtain Pr equally with embodiment 101
0.01Yb
1Y
0.99O
3Crystalline ceramics.
Embodiment 103
The sintered heat insulating temperature is 1850 ℃, and other conditions can obtain Pr equally with embodiment 101
0.01Yb
1Y
0.99O
3Crystalline ceramics.
Embodiment 104
The sintered heat insulating time is 30 hours, and other conditions can obtain Pr equally with embodiment 101
0.01Yb
1Y
0.99O
3Crystalline ceramics.
Embodiment 105
The sintered heat insulating time is 20 hours, and other conditions can obtain Pr equally with embodiment 101
0.01Yb
1Y
0.99O
3Crystalline ceramics.
Embodiment 106
Employing purity is 99.999% yttrium oxide (Y
2O
3), ytterbium oxide (Yb
2O
3) and terbium sesquioxide (Tb
4O
7) powder is raw material, presses Tb
0.002Yb
0.004Y
1.994O
3Composition configure powder raw material, the back is that medium prepares ceramic powder with the dehydrated alcohol with wet ball grinding, powder is dried after granulation, compressing tablet; Subsequently it is imposed the above isostatic cool pressing of 200MPa; Put into vacuum sintering furnace at last in 1750 ℃ of sintering 5 hours, the vacuum tightness in sintered heat insulating stage is 1 * 10
-3Pa obtains Tb
0.002Yb
0.004Y
1.994O
3Crystalline ceramics.
Embodiment 107
The sintered heat insulating temperature is 2150 ℃, and other conditions can obtain Tb equally with embodiment 106
0.002Yb
0.004Y
1.994O
3Crystalline ceramics.
Embodiment 108
The sintered heat insulating temperature is 1850 ℃, and other conditions can obtain Tb equally with embodiment 106
0.002Yb
0.004Y
1.994O
3Crystalline ceramics.
Embodiment 109
The sintered heat insulating time is 30 hours, and other conditions can obtain Tb equally with embodiment 106
0.002Yb
0.004Y
1.994O
3Crystalline ceramics.
Embodiment 110
The sintered heat insulating time is 20 hours, and other conditions can obtain Tb equally with embodiment 106
0.002Yb
0.004Y
1.994O
3Crystalline ceramics.
Embodiment 111
Press Tb
0.008Yb
0.75Y
1.242O
3Composition configure raw material, other conditions are with embodiment 106, obtain Tb
0.008Yb
0.75Y
1.242O
3Crystalline ceramics.
Embodiment 112
The sintered heat insulating temperature is 2150 ℃, and other conditions can obtain Tb equally with embodiment 111
0.008Yb
0.75Y
1.242O
3Crystalline ceramics.
Embodiment 113
The sintered heat insulating temperature is 1850 ℃, and other conditions can obtain Tb equally with embodiment 111
0.008Yb
0.75Y
1.242O
3Crystalline ceramics.
Embodiment 114
The sintered heat insulating time is 30 hours, and other conditions can obtain Tb equally with embodiment 111
0.008Yb
0.75Y
1.242O
3Crystalline ceramics.
Embodiment 115
The sintered heat insulating time is 20 hours, and other conditions can obtain Tb equally with embodiment 111
0.008Yb
0.75Y
1.242O
3Crystalline ceramics.
Embodiment 116
Press Pr
0.01Yb
1Y
0.99O
3Composition configure raw material, other conditions are with embodiment 106, obtain Pr
0.01Yb
1Y
0.99O
3Crystalline ceramics.
Embodiment 117
The sintered heat insulating temperature is 2150 ℃, and other conditions can obtain Pr equally with embodiment 116
0.01Yb
1Y
0.99O
3Crystalline ceramics.
Embodiment 118
The sintered heat insulating temperature is 1850 ℃, and other conditions can obtain Pr equally with embodiment 116
0.01Yb
1Y
0.99O
3Crystalline ceramics.
Embodiment 119
The sintered heat insulating time is 30 hours, and other conditions can obtain Pr equally with embodiment 116
0.01Yb
1Y
0.99O
3Crystalline ceramics.
Embodiment 120
The sintered heat insulating time is 20 hours, and other conditions can obtain Pr equally with embodiment 116
0.01Yb
1Y
0.99O
3Crystalline ceramics.
Claims (2)
1, a kind of crystalline ceramics is characterized in that the structural formula of this crystalline ceramics is: Ln
xYb
yY
(3-x-y)Al
5O
12Or Ln
wYb
zY
(2-w-z)O
3, wherein, 0.003≤x≤0.03,0.006≤y≤1.5,0.002≤w≤0.02,0.004≤z≤1, Ln represents Ce, Tm, Pr or Tb element.
2, the preparation method of the described crystalline ceramics of claim 1 is characterized in that comprising the following steps:
1. select the structural formula Ln of crystalline ceramics to be prepared
xYb
yY
(3-x-y)Al
5O
12Or Ln
wYb
zY
(2-w-z)O
3And respective x, y, w, z and concrete Ln element;
2. adopt purity to be not less than 99.9% yttrium oxide, aluminum oxide, ytterbium oxide, choose a kind of in the oxide powder of cerium oxide, trioxide, Praseodymium trioxide or terbium sesquioxide again and be raw material, by the stoicheiometry configuration powder raw material of selected structural formula;
3. with the 2. the raw material in step put into ball grinder, be that medium prepares ceramic powder with the dehydrated alcohol with wet ball grinding, powder carries out granulation, compressing tablet after drying;
4. the isostatic cool pressing that compressing tablet is imposed more than the 200MPa becomes base substrate;
5. put into vacuum sintering furnace at last and under following condition, carry out sintering acquisition crystalline ceramics:
(a) be Ln to structural formula
xYb
yY
(3-x-y)Al
5O
12Base substrate, the holding temperature during vacuum sintering is 1600～1750 ℃, soaking time is 5～30 hours, vacuum tightness is better than 3 * 10
-3Pa;
(b) be Ln to structural formula
wYb
zY
(2-w-z)O
3Ceramic body, the holding temperature during vacuum sintering is 1750～2150 ℃, soaking time is 5～30 hours, vacuum tightness is better than 3 * 10
-3Pa.
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