CN105523753B - It can be seen that/short-wave infrared/medium-wave infrared YAG crystalline ceramics and its manufacture method - Google Patents

It can be seen that/short-wave infrared/medium-wave infrared YAG crystalline ceramics and its manufacture method Download PDF

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CN105523753B
CN105523753B CN201610006374.3A CN201610006374A CN105523753B CN 105523753 B CN105523753 B CN 105523753B CN 201610006374 A CN201610006374 A CN 201610006374A CN 105523753 B CN105523753 B CN 105523753B
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wave infrared
crystalline ceramics
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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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    • C04B35/44—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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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract

The present invention provides a kind of visible/short-wave infrared/medium-wave infrared YAG crystalline ceramics, only contain weight ratio be 0.01 0.1% MgO as sintering aid, 6 μm of the 300nm of transmission scope covering of product, and the transmitance at 600nm is not less than 76%, the transmitance of 14 mu m wavebands is not less than 80%, and its manufacture method.The present invention only adds the MgO that weight ratio is 0.01 0.1wt%, need not both add SiO2Other oxides are not contained as sintering aid yet.The product of the present invention has good visible/infrared transmission performance, and has more preferable thermal conductivity.

Description

It can be seen that/short-wave infrared/medium-wave infrared YAG crystalline ceramics and its manufacture method
Technical field
The present invention relates to a kind of visible/short-wave infrared/medium-wave infrared crystalline ceramics and its manufacture method, and in particular to only adds MgO is added to prepare YAG crystalline ceramics and its product through two step vacuum-sinterings as sintering aid.
Background technology
Yttrium-aluminium-garnet (abbreviation YAG) has cubic structure, and effect free of birefringence, high-temerature creep is small, optical property and power Excellent performance is learned, is widely used in laser host material, can also be used to make high temperature visible ray and infrared window.It is mono- with YAG Crystal phase ratio, YAG crystalline ceramics can meet to prepare the doping concentration of the large scale sample and higher needed for high power laser, Therefore good application prospect is had shown that in terms of YAG monocrystalline is substituted, and as a research heat of Material Field in recent years Point.YAG usually mixes Nd as crystalline ceramics matrix3+、Yb3+、Er3+、Eu3+、Cr3+、Pr3+Deng these Doped ions are usually with oxygen The form of compound is added in raw material and sintered together.Not only functional ionic is used as, but also being capable of acceleration of sintering as sintering aid.In addition, There is still a need for addition SiO in addition to adding functional ionic2And MgO is as common sintering aid, the ion (Nd of these additions3 +、Yb3+、Er3+、Eu3+、Cr3+、Pr3+) absorption, SiO can be produced in different wave bands2Phonon energy is big, in common 3-5 μm Infrared band has strong absorption.In addition, additive is more, YAG thermal conductivities are smaller so that its thermal shock resistance is deteriorated.
Therefore, as visible/near infrared/middle infrared transparent ceramic window, it is necessary to avoid drawing for above-mentioned various ions as far as possible Enter, avoid them from causing the decline of YAG crystalline ceramics optical properties.
The content of the invention
The present invention discloses a kind of visible/short-wave infrared/medium-wave infrared YAG crystalline ceramics, it is through scope covering 300nm-6 μm, and the transmitance at 600nm is not less than 80% not less than the transmitance of 76%, 1-4 mu m wavebands, wherein only adding weight ratio (removing specified otherwise, composition of the invention is weight percentage) is the MgO of 0.01-0.1%.Can present invention simultaneously provides one kind See/the manufacture method of short-wave infrared/medium-wave infrared YAG crystalline ceramics.
Technical scheme is as follows：
A kind of visible/short-wave infrared/medium-wave infrared YAG crystalline ceramics, its main feature is that MgO weight ratios are the 0.01- of YAG 0.1%, it covers 300nm-6 μm through scope, and the transmitance at 600nm is not less than the transmitance of 76%, 1-4 mu m wavebands Not less than 80%.
The average grain size of the YAG crystalline ceramics is 4-5 μm.
Transmitance at 600nm is not less than 78%.
A kind of method of visible/short-wave infrared/medium-wave infrared YAG crystalline ceramics described in manufacture, is not less than with purity 99.99%, average grain diameter is between 0.2-1 μm of high-purity Y2O3And Al2O3Powder is raw material, it is characterised in that is comprised the following steps：
1. by material powder according to Y3Al5O12Stoichiometric ratio ball milling mixing it is uniform, while only add 0.01- The MgO of 0.1wt% is as sintering aid；
2. the mixture of step 1 is compressing by isostatic cool pressing, obtain biscuit；
3. will be sintered after above-mentioned biscuit pre-burning in vacuum tungsten coil furnace, first sintering temperature is 1730 DEG C -1830 DEG C, sintering When time is 5-15 small；
4. and then furnace temperature continues 30 DEG C of -80 DEG C of progress double sinterings of rise, when sintering time is 5-30 small.
As the preferred solution of the present invention, the additive amount of sintering aid is 0.03-0.05wt%.
Compared with prior art, it is saturating the beneficial effects of the invention are as follows one kind visible/short-wave infrared/medium-wave infrared YAG is provided Bright ceramic preparation method, only adds the MgO that weight ratio is 0.01-0.1wt%, need not both add SiO2As sintering aid Other oxides are not contained yet.The product of the present invention has good visible/infrared transmission performance, and has more preferable thermal conductivity Rate.
Brief description of the drawings
Fig. 1 is the SEM shape appearance figures of the YAG crystalline ceramics obtained by the embodiment of the present invention 1；
Fig. 2 is visible/short-wave infrared transmittance curve of the YAG crystalline ceramics obtained by embodiment 1；
Fig. 3 is the medium-wave infrared transmittance curve of the YAG crystalline ceramics obtained by embodiment 1；
Fig. 4 is the visible/near infrared transmittance curve of the YAG crystalline ceramics obtained by embodiment 2；
Fig. 5 is the medium-wave infrared transmittance curve of the YAG crystalline ceramics obtained by embodiment 2；
Fig. 6 is the visible/near infrared transmittance curve of the YAG crystalline ceramics obtained by embodiment 3；
Fig. 7 is the medium-wave infrared transmittance curve of the YAG crystalline ceramics obtained by embodiment 3；
Fig. 8 is the visible/near infrared transmittance curve of the YAG crystalline ceramics obtained by embodiment 4；
Fig. 9 is the medium-wave infrared transmittance curve of the YAG crystalline ceramics obtained by embodiment 4；
Figure 10 is the visible/near infrared transmittance curve of the YAG crystalline ceramics obtained by embodiment 5；
Figure 11 is the medium-wave infrared transmittance curve of the YAG crystalline ceramics obtained by embodiment 5；
Embodiment
With reference to embodiment, the invention will be further described, these examples are merely to illustrate the present invention but should not be with this Limit the scope of the invention.High pure raw material used in the present invention is not less than for purity known to crystalline ceramics field 99.99%.The optical transmittance test of visible/short-wave infrared/medium-wave infrared of product of the present invention is divided in Perkin Elmer Carried out on photometer Lambda750 and Nicolet Fourier transformation infrared spectrometer FT-IR 5700, test sample two sides is thrown Light, thickness are 5mm.
Embodiment 1
With commercially available high-purity Al2O3、Y2O3And high-purity nm MgO is raw material, wherein Al2O3Powder average grain diameter is 0.45 μm, Y2O3Powder average grain diameter is 0.2 μm.By Y3Al5O12Stoichiometric ratio weigh Al2O3And Y2O3, and add 0.04wt%MgO Form powder material.Using ethanol as ball-milling medium, with high-purity Al2O3Ball is as ball-milling medium, with the rotating speed ball of 250r/min 5h is ground, uniform slurry is made in powder material.200 mesh sieves are crossed after slurry is dried, using cold isostatic compaction technology 200MPa is pressed into biscuit.Biscuit is better than 5*10 in vacuum-3Sintered in the vacuum tungsten coil furnace of Pa, with the speed of 2-10 DEG C/min Degree is warming up to keeps the temperature 8h at 1780 DEG C, then heats to 1840 DEG C of insulation 25h.The microstructure of products obtained therefrom is not as shown in Figure 1, have There is the defects of stomata.Average grain size is 4-5 μm.The transmitance of product is 300nm-6 μ through scope as shown in Figure 2 and Figure 3 M, and transmitance reaches the transmitances of 82.4%, 1-4 mu m wavebands and reaches 83.8-84.5% at 600nm.
Comparative example 1
By the biscuit obtained in embodiment 1, a step sinters in the vacuum tungsten coil furnace described in embodiment 1, with 2-10 DEG C/min Speed be warming up to 1780 DEG C insulation 33h.Measure product at 600nm transmitance for 58%, 1-4 mu m wavebands transmitance between 60-63%.
Comparative example 2
By the biscuit obtained in embodiment 1, a step sinters in the vacuum tungsten coil furnace described in embodiment 1, with 2-10 DEG C/min Speed be warming up to 1840 DEG C insulation 33h.Measure product at 600nm transmitance for 65%, 1-4 mu m wavebands transmitance between 67-70%.
Embodiment 2
With commercially available high-purity Al2O3、Y2O3And high-purity nm MgO is raw material, wherein Al2O3Powder average grain diameter is 0.2 μm, Y2O3Powder average grain diameter is 0.6 μm.By Y3Al5O12Stoichiometric ratio weigh Al2O3And Y2O3, and add 0.03wt%MgO Form powder material.The step of ball milling mixing and forming of green body, is the same as embodiment 1.Biscuit is better than 5*10 in vacuum-3Pa's Sintered in vacuum tungsten coil furnace, 1730 DEG C of insulation 15h are warming up to the speed of 2-10 DEG C/min, then heat to 1810 DEG C of insulations 30h.The transmitance of product is 300nm-6 μm through scope, and transmitance reaches at 600nm as shown in Figure 4, Figure 5 The transmitance of 80.9%, 1-4 mu m waveband reaches 82.6-83%.
Embodiment 3
With commercially available high-purity Al2O3、Y2O3And MgO is raw material, wherein Al2O3Powder average grain diameter is 0.8 μm, Y2O3Powder is put down Equal particle diameter is 1.0 μm.By Y3Al5O12Stoichiometric ratio weigh Al2O3And Y2O3, and it is former to add 0.1wt%MgO composition powders Material.Using ethanol as ball-milling medium, with high-purity Al2O3Ball is as ball-milling medium, with the rotating speed ball milling 48h of 250r/min, by powder Uniform slurry is made in body raw material.200 mesh sieves are crossed after slurry is dried, are pressed into using cold isostatic compaction technology in 200MPa Biscuit.Biscuit is better than 5*10 in vacuum-3Sintered 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, then heat to 1880 DEG C of insulation 20h.The transmitance of product is as shown in Figure 6, Figure 7, through scope 300nm-6 μm, and transmitance reaches the transmitances of 80.1%, 1-4 mu m wavebands and reaches 82.9-83.2% at 600nm.
Embodiment 4
Using raw material same as Example 1, by Y3Al5O12Stoichiometric ratio weigh, the wherein additive amount of MgO is 0.05wt%.Biscuit is manufactured using the step of ball milling mixing in embodiment 1 and forming of green body.Biscuit is better than 5* in vacuum 10-3Sintered in the vacuum tungsten coil furnace of Pa, 1730 DEG C of insulation 10h are warming up to the speed of 2-10 DEG C/min, then heat to 1760 DEG C insulation 30h.The transmitance of product is 300nm-6 μm through scope, and transmitance reaches at 600nm as shown in Figure 8, Figure 9 The transmitance of 78.1%, 1-4 mu m waveband reaches 82.9-83.7%.
Embodiment 5
Using raw material same as Example 2, by Y3Al5O12Stoichiometric ratio weigh, the wherein additive amount of MgO is 0.01wt%.Biscuit is manufactured using the step of ball milling mixing in embodiment 1 and forming of green body.Biscuit is better than 5* in vacuum 10-3Sintered in the vacuum tungsten coil furnace of Pa, 1750 DEG C of insulation 10h are warming up to the speed of 2-10 DEG C/min, then heat to 1810 DEG C insulation 20h.The transmitance of product is 300nm-6 μm through scope, and transmitance reaches at 600nm as shown in Figure 10, Figure 11 Transmitance to 76.5%, 1-4 mu m wavebands reaches 80.3-81.2%.

Claims (5)

1. a kind of manufacture method of visible/short-wave infrared/medium-wave infrared YAG crystalline ceramics, is not less than 99.99% with purity, puts down Equal particle diameter is between 0.2-1 μm of high-purity Y2O3And Al2O3Powder is raw material, it is characterised in that is comprised the following steps：
1. by material powder according to Y3Al5O12Stoichiometric ratio ball milling mixing it is uniform, while only add 0.01-0.1wt% MgO is as sintering aid；
2. the mixture of step 1. is compressing by isostatic cool pressing, obtain biscuit；
3. will be sintered after above-mentioned biscuit pre-burning in vacuum tungsten coil furnace, first sintering temperature is 1730 DEG C -1830 DEG C, sintering time For 5-15 it is small when；
It is 4. obtained visible/short when sintering time is 5-30 small and then furnace temperature continues 30 DEG C of -80 DEG C of progress double sinterings of rise Ripple is infrared/medium-wave infrared YAG crystalline ceramics, it covers 300nm-6 μm through scope, and the transmitance at 600nm is not less than The transmitance of 76%, 1-4 mu m waveband is not less than 80%.
2. the method as described in claim 1, it is characterized in that the MgO is 0.03- as the additive amount of sintering aid 0.05wt%.
3. a kind of visible made from method as described in claim 1/short-wave infrared/medium-wave infrared YAG crystalline ceramics, its feature It is only to add MgO, MgO percentage by weights are the 0.01-0.1% of YAG.
4. one kind visible/short-wave infrared/medium-wave infrared YAG crystalline ceramics as claimed in claim 3, it is characterised in that the YAG The average grain size of crystalline ceramics is 4-5 μm.
5. one kind visible/short-wave infrared/medium-wave infrared YAG crystalline ceramics as claimed in claim 3, it is characterised in that 600nm The transmitance at place is not less than 78%.
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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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

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JPH05294723A (en) * 1992-04-10 1993-11-09 Kurosaki Refract Co Ltd Production of polycrystalline transparent yag ceramic for solid laser

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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

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