CN105523753A - Visible/shortwave infrared/mediumwave infrared YAG transparent ceramic and preparation method thereof - Google Patents

Visible/shortwave infrared/mediumwave infrared YAG transparent ceramic and preparation method thereof Download PDF

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CN105523753A
CN105523753A CN201610006374.3A CN201610006374A CN105523753A CN 105523753 A CN105523753 A CN 105523753A CN 201610006374 A CN201610006374 A CN 201610006374A CN 105523753 A CN105523753 A CN 105523753A
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wave infrared
visible
crystalline ceramics
infrared
transmitance
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CN105523753B (en
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毛小建
王传逢
张龙
许杨阳
姜本学
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Shanghai Institute of Optics and Fine Mechanics of CAS
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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Abstract

The invention provides a visible/shortwave infrared/mediumwave infrared YAG transparent ceramic. The ceramic only comprises MgO with a weight percentage of 0.01-0.1% as a sintering aid. The transmittance range of the product covers 300nm-6mum. The transmittance at 600nm is no lower than 76%, and the transmittance at the wave band of 1-4mum is no lower than 80%. The invention also provides a preparation method of the ceramic. According to the invention, only MgO with the weight percentage of 0.01-0.1wt% is added. No SiO2 is needed as a sintering aid, and the ceramic does not contain other oxide. The product provided by the invention has good visible/infrared transmittance, and has better thermal conductivity.

Description

Visible/short-wave infrared/medium-wave infrared YAG crystalline ceramics and manufacture method thereof
Technical field
The present invention relates to as seen a kind of/short-wave infrared/medium-wave infrared crystalline ceramics and manufacture method thereof, be specifically related to only to add MgO and prepare YAG crystalline ceramics and goods thereof as sintering aid through two step vacuum sinterings.
Background technology
Yttrium aluminum garnet (being called for short YAG) has cubic structure, free of birefringence effect, and high temperature creep is little, optical property and excellent in mechanical performance, is widely used in laser host material, also can be used for making high temperature visible ray and infrared window.Compared with YAG single crystal, YAG crystalline ceramics can meet the doping content preparing large size sample needed for high power laser and Geng Gao, therefore in replacement YAG monocrystalline, demonstrate good application prospect, and become a study hotspot of Material Field in recent years.YAG, as crystalline ceramics matrix, usually mixes Nd 3+, Yb 3+, Er 3+, Eu 3+, Cr 3+, Pr 3+usually add in raw material in the form of the oxide Deng, these dopant ions and sinter together.Both as functional ionic, again can acceleration of sintering as sintering aid.In addition, still need to add SiO except adding functional ionic 2and MgO is as common sintering aid, these ion (Nd added 3+, Yb 3+, Er 3+, Eu 3+, Cr 3+, Pr 3+) absorption can be produced at different wave bands, SiO 2phonon energy is large, has strong absorption in 3-5 μm of conventional middle-infrared band.In addition, substance is more, and YAG thermal conductivity is less, and its heat-shock resistance is deteriorated.
Therefore, as visible/near infrared/middle infrared transparent ceramic window, need the introducing as far as possible avoiding above-mentioned various ion, avoid them to cause the decline of YAG crystalline ceramics optical property.
Summary of the invention
The present invention is as seen a kind of/short-wave infrared/medium-wave infrared YAG crystalline ceramics openly, it covers 300nm-6 μm through scope, and the transmitance at 600nm place is not less than 76%, the transmitance of 1-4 mu m waveband is not less than 80%, wherein only add the MgO that weight ratio (except specified otherwise, composition of the present invention is all weight percentage) is 0.01-0.1%.The present invention provides the manufacture method of as seen a kind of/short-wave infrared/medium-wave infrared YAG crystalline ceramics simultaneously.
Technical scheme of the present invention is as follows:
As seen a kind of/short-wave infrared/medium-wave infrared YAG crystalline ceramics, is characterized in that MgO weight ratio is the 0.01-0.1% of YAG, and it covers 300nm-6 μm through scope, and the transmitance that the transmitance at 600nm place is not less than 76%, 1-4 mu m waveband is not less than 80%.
The average crystal grain size of this YAG crystalline ceramics is 4-5 μm.
The transmitance at 600nm place is not less than 78%.
Manufacture described visible/method of short-wave infrared/medium-wave infrared YAG crystalline ceramics, be not less than 99.99% with purity, median size is between high-purity Y of 0.2-1 μm 2o 3and Al 2o 3powder is raw material, it is characterized in that comprising following steps:
1. by material powder according to Y 3al 5o 12stoichiometric ratio ball milling mix, simultaneously only add the MgO of 0.01-0.1wt% as sintering aid;
2. the compound of step 1 is passed through isostatic cool pressing compression moulding, obtain biscuit;
3. sinter after above-mentioned biscuit pre-burning in vacuum tungsten coil furnace, first sintering temperature is 1730 DEG C-1830 DEG C, and sintering time is 5-15 hour;
4. then furnace temperature continues rising 30 DEG C-80 DEG C and carries out double sintering, and sintering time is 5-30 hour.
As a preferred version of the present invention, the addition of sintering aid is 0.03-0.05wt%.
Compared with prior art, the invention has the beneficial effects as follows the preparation method providing as seen a kind of/short-wave infrared/medium-wave infrared YAG crystalline ceramics, only adding weight ratio is the MgO of 0.01-0.1wt%, neither needs to add SiO 2as sintering aid also not containing other oxide compounds.Product of the present invention have good visible/infrared transmission performance, and there is better thermal conductivity.
Accompanying drawing explanation
Fig. 1 is the SEM shape appearance figure of the YAG crystalline ceramics obtained by the embodiment of the present invention 1;
The YAG crystalline ceramics of Fig. 2 obtained by embodiment 1 visible/short-wave infrared transmittance curve;
The medium-wave infrared transmittance curve of the YAG crystalline ceramics of Fig. 3 obtained by embodiment 1;
The visible/near infrared transmittance curve of the YAG crystalline ceramics of Fig. 4 obtained by embodiment 2;
The medium-wave infrared transmittance curve of the YAG crystalline ceramics of Fig. 5 obtained by embodiment 2;
The visible/near infrared transmittance curve of the YAG crystalline ceramics of Fig. 6 obtained by embodiment 3;
The medium-wave infrared transmittance curve of the YAG crystalline ceramics of Fig. 7 obtained by embodiment 3;
The visible/near infrared transmittance curve of the YAG crystalline ceramics of Fig. 8 obtained by embodiment 4;
The medium-wave infrared transmittance curve of the YAG crystalline ceramics of Fig. 9 obtained by embodiment 4;
The visible/near infrared transmittance curve of the YAG crystalline ceramics of Figure 10 obtained by embodiment 5;
The medium-wave infrared transmittance curve of the YAG crystalline ceramics of Figure 11 obtained by embodiment 5;
Embodiment
Below in conjunction with embodiment, the invention will be further described, and these examples only should not to limit the scope of the invention with this for illustration of the present invention.The present invention's high pure raw material used is that the known purity in crystalline ceramics field is not less than 99.99%.Product of the present invention visible/test of the optical transmittance of short-wave infrared/medium-wave infrared carries out on PerkinElmer spectrophotometer Lambda750 and Nicolet Fourier transformation infrared spectrometer FT-IR5700, test sample polishing both surfaces, thickness is 5mm.
Embodiment 1
With commercially available high-purity Al 2o 3, Y 2o 3and high-purity nm MgO is raw material, wherein Al 2o 3powder median size is 0.45 μm, Y 2o 3powder median size is 0.2 μm.By Y 3al 5o 12stoichiometric ratio take Al 2o 3and Y 2o 3, and add 0.04wt%MgO composition powder raw material.Adopt ethanol as ball-milling medium, with high-purity Al 2o 3powder raw material, as ball-milling medium, with the rotating speed ball milling 5h of 250r/min, is made uniform slurry by ball.Cross 200 mesh sieves by after slurry drying, adopt cold isostatic compaction technology 200MPa to be pressed into biscuit.Biscuit is better than 5*10 in vacuum tightness -3sinter in the vacuum tungsten coil furnace of Pa, be warming up at 1780 DEG C of insulation 8h with the speed of 2-10 DEG C/min, be then warming up to 1840 DEG C of insulation 25h.The microstructure of products obtained therefrom as shown in Figure 1, does not have the defects such as pore.Average crystal grain size is 4-5 μm.The transmitance of product as shown in Figure 2 and Figure 3, is 300nm-6 μm through scope, and the transmitance that 600nm place transmitance reaches 82.4%, 1-4 mu m waveband reaches 83.8-84.5%.
Comparative example 1
By the biscuit step sintering in the vacuum tungsten coil furnace described in embodiment 1 obtained in embodiment 1, be warming up to 1780 DEG C of insulation 33h with the speed of 2-10 DEG C/min.Recording product in 600nm place transmitance is that the transmitance of 58%, 1-4 mu m waveband is between 60-63%.
Comparative example 2
By the biscuit step sintering in the vacuum tungsten coil furnace described in embodiment 1 obtained in embodiment 1, be warming up to 1840 DEG C of insulation 33h with the speed of 2-10 DEG C/min.Recording product in 600nm place transmitance is that the transmitance of 65%, 1-4 mu m waveband is between 67-70%.
Embodiment 2
With commercially available high-purity Al 2o 3, Y 2o 3and high-purity nm MgO is raw material, wherein Al 2o 3powder median size is 0.2 μm, Y 2o 3powder median size is 0.6 μm.By Y 3al 5o 12stoichiometric ratio take Al 2o 3and Y 2o 3, and add 0.03wt%MgO composition powder raw material.The step of ball milling mixing and forming of green body is with embodiment 1.Biscuit is better than 5*10 in vacuum tightness -3sinter in the vacuum tungsten coil furnace of Pa, be warming up to 1730 DEG C of insulation 15h with the speed of 2-10 DEG C/min, be then warming up to 1810 DEG C of insulation 30h.The transmitance of product as shown in Figure 4, Figure 5, is 300nm-6 μm through scope, and the transmitance that 600nm place transmitance reaches 80.9%, 1-4 mu m waveband reaches 82.6-83%.
Embodiment 3
With commercially available high-purity Al 2o 3, Y 2o 3and MgO is raw material, wherein Al 2o 3powder median size is 0.8 μm, Y 2o 3powder median size is 1.0 μm.By Y 3al 5o 12stoichiometric ratio take Al 2o 3and Y 2o 3, and add 0.1wt%MgO composition powder raw material.Adopt ethanol as ball-milling medium, with high-purity Al 2o 3powder raw material, as ball-milling medium, with the rotating speed ball milling 48h of 250r/min, is made uniform slurry by ball.Cross 200 mesh sieves by after slurry drying, adopt cold isostatic compaction technology to be pressed into biscuit at 200MPa.Biscuit is better than 5*10 in vacuum tightness -3sinter in the vacuum tungsten coil furnace of Pa, and the speed of 2-10 DEG C/min is warming up to 1830 DEG C of insulation 5h, is then warming up to 1880 DEG C of insulation 20h.The transmitance of product as shown in Figure 6, Figure 7, is 300nm-6 μm through scope, and the transmitance that 600nm place transmitance reaches 80.1%, 1-4 mu m waveband reaches 82.9-83.2%.
Embodiment 4
Adopt the raw material identical with embodiment 1, by Y 3al 5o 12stoichiometric ratio take, wherein the addition of MgO is 0.05wt%.The step of ball milling mixing and forming of green body in embodiment 1 is adopted to manufacture biscuit.Biscuit is better than 5*10 in vacuum tightness -3sinter in the vacuum tungsten coil furnace of Pa, be warming up to 1730 DEG C of insulation 10h with the speed of 2-10 DEG C/min, be then warming up to 1760 DEG C of insulation 30h.The transmitance of product as shown in Figure 8, Figure 9, is 300nm-6 μm through scope, and the transmitance that 600nm place transmitance reaches 78.1%, 1-4 mu m waveband reaches 82.9-83.7%.
Embodiment 5
Adopt the raw material identical with embodiment 2, by Y 3al 5o 12stoichiometric ratio take, wherein the addition of MgO is 0.01wt%.The step of ball milling mixing and forming of green body in embodiment 1 is adopted to manufacture biscuit.Biscuit is better than 5*10 in vacuum tightness -3sinter in the vacuum tungsten coil furnace of Pa, be warming up to 1750 DEG C of insulation 10h with the speed of 2-10 DEG C/min, be then warming up to 1810 DEG C of insulation 20h.The transmitance of product as shown in Figure 10, Figure 11, is 300nm-6 μm through scope, and the transmitance that 600nm place transmitance reaches 76.5%, 1-4 mu m waveband reaches 80.3-81.2%.

Claims (5)

1. visible/short-wave infrared/medium-wave infrared YAG crystalline ceramics, it is characterized in that MgO weight ratio is the 0.01-0.1% of YAG, it covers 300nm-6 μm through scope, and the transmitance that the transmitance at 600nm place is not less than 76%, 1-4 mu m waveband is not less than 80%.
2. as claimed in claim 1 a kind of visible/short-wave infrared/medium-wave infrared YAG crystalline ceramics, is characterized in that the average crystal grain size of this YAG crystalline ceramics is 4-5 μm.
3. as claimed in claim 1 a kind of visible/short-wave infrared/medium-wave infrared YAG crystalline ceramics, is characterized in that the transmitance at 600nm place is not less than 78%.
4. manufacture the method for as claimed in claim 1 visible/short-wave infrared/medium-wave infrared YAG crystalline ceramics, be not less than 99.99% with purity, median size is between high-purity Y of 0.2-1 μm 2o 3and Al 2o 3powder is raw material, it is characterized in that comprising following steps:
1. by material powder according to Y 3al 5o 12stoichiometric ratio ball milling mix, simultaneously only add the MgO of 0.01-0.1wt% as sintering aid;
2. the compound of step 1 is passed through isostatic cool pressing compression moulding, obtain biscuit;
3. sinter after above-mentioned biscuit pre-burning in vacuum tungsten coil furnace, first sintering temperature is 1730 DEG C-1830 DEG C, and sintering time is 5-15 hour;
4. then furnace temperature continues rising 30 DEG C-80 DEG C and carries out double sintering, and sintering time is 5-30 hour.
5. method as claimed in claim 4, is characterized in that described MgO is 0.03-0.05wt% as the addition of sintering aid.
CN201610006374.3A 2016-01-06 2016-01-06 It can be seen that/short-wave infrared/medium-wave infrared YAG crystalline ceramics and its manufacture method Active CN105523753B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107540372A (en) * 2016-06-24 2018-01-05 中国科学院上海光学精密机械研究所 Medium-wave infrared window and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05294723A (en) * 1992-04-10 1993-11-09 Kurosaki Refract Co Ltd Production of polycrystalline transparent yag ceramic for solid laser
CN102924073A (en) * 2012-11-16 2013-02-13 北京雷生强式科技有限责任公司 Method for preparing rare earth ion-doped yttrium aluminum garnet (Re: YAG) transparent laser ceramic by using hot-pressing post treatment
CN103102156A (en) * 2011-11-10 2013-05-15 中国科学院福建物质结构研究所 Re:YAG transparent ceramic prepared through gel casting molding
CN104962993A (en) * 2015-05-26 2015-10-07 哈尔滨工业大学 Vertical Bridgman preparation method of large-size magnesium aluminate spinel-yttrium aluminum garnet eutectic ceramic
CN105110792A (en) * 2015-09-22 2015-12-02 中国工程物理研究院化工材料研究所 Ball milling preparation method for high-uniformity YAG transparent ceramic powder

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05294723A (en) * 1992-04-10 1993-11-09 Kurosaki Refract Co Ltd Production of polycrystalline transparent yag ceramic for solid laser
CN103102156A (en) * 2011-11-10 2013-05-15 中国科学院福建物质结构研究所 Re:YAG transparent ceramic prepared through gel casting molding
CN102924073A (en) * 2012-11-16 2013-02-13 北京雷生强式科技有限责任公司 Method for preparing rare earth ion-doped yttrium aluminum garnet (Re: YAG) transparent laser ceramic by using hot-pressing post treatment
CN104962993A (en) * 2015-05-26 2015-10-07 哈尔滨工业大学 Vertical Bridgman preparation method of large-size magnesium aluminate spinel-yttrium aluminum garnet eutectic ceramic
CN105110792A (en) * 2015-09-22 2015-12-02 中国工程物理研究院化工材料研究所 Ball milling preparation method for high-uniformity YAG transparent ceramic powder

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107540372A (en) * 2016-06-24 2018-01-05 中国科学院上海光学精密机械研究所 Medium-wave infrared window and preparation method thereof
CN107540372B (en) * 2016-06-24 2022-03-08 中国科学院上海光学精密机械研究所 Medium wave infrared window and preparation method thereof

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