CN109097835A - KHg4Ga5Se12Nonlinear optical crystal, preparation method and device for non-linear optical - Google Patents
KHg4Ga5Se12Nonlinear optical crystal, preparation method and device for non-linear optical Download PDFInfo
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- CN109097835A CN109097835A CN201710772239.4A CN201710772239A CN109097835A CN 109097835 A CN109097835 A CN 109097835A CN 201710772239 A CN201710772239 A CN 201710772239A CN 109097835 A CN109097835 A CN 109097835A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/35—Non-linear optics
- G02F1/355—Non-linear optics characterised by the materials used
- G02F1/3551—Crystals
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Abstract
The invention discloses KHg4Ga5Se12Nonlinear optical crystal and preparation method and purposes.KHg of the invention4Ga5Se12Nonlinear optical crystal uses high-temperature fusant spontaneous crystallization method or Bridgman-Stockbarge method for growing；In the KHg4Ga5Se12In the growth of nonlinear optical crystal, crystal have many advantages, such as the speed of growth it is very fast, it is at low cost, be easy to get larger size crystal；Gained KHg4Ga5Se12Nonlinear optical crystal has the advantages that nonlinear optical effect is very big, transmission region is wide, and hardness is larger, good mechanical property, easy to process.KHg of the invention4Ga5Se12Nonlinear optical crystal can be used for making device for non-linear optical.
Description
Technical field
The present invention relates to a kind of KHg4Ga5Se12Nonlinear optical crystal (KHg4Ga5Se12Monocrystalline) and the KHg4Ga5Se12
The preparation method of monocrystalline and the KHg4Ga5Se12Device for non-linear optical of the monocrystalline for production.
Background technique
Crystal with nonlinear optical effect is known as nonlinear optical crystal.Here nonlinear optical effect refers to again
Frequently with frequency, difference frequency, parameter amplification etc. effects.Only the crystal without symmetrical centre has been likely to nonlinear optical effect.Benefit
With the nonlinear optical effect of crystal, second harmonic generator, upper and lower frequency converter, optical parametric oscillator etc. can be made
Device for non-linear optical.The laser that laser generates can carry out frequency conversion by device for non-linear optical, to obtain more
The laser of useful wavelength, makes laser be more widely used.
According to the difference of material application band, ultraviolet region, visible and near-infrared region and mid-infrared light can be divided into
Area's nonlinear optical material three categories.The non-linear optical crystal material of visible region and ultraviolet region, which has been able to satisfy, actually answers
It is required that；It is practical such as in two frequencys multiplication (532nm) crystal mainly to have KTP (KTiOPO4)、BBO(β-SnB2O4)、LBO
(LiB3O5) crystal；It is practical in frequency tripling (355nm) crystal to have BBO, LBO, CBO (CsB3O5) available.And infrared waves
The nonlinear crystal development of section is slow；The material of infrared light district is ABC mostly2The chalcopyrite structure semiconductor material of type, such as
AgGaQ2(Q=S, Se, Te), the light injury threshold of infrared non-linear crystal is too low and crystal growth is difficult, directly affects reality
Border uses.
Middle infrared band nonlinear optical crystal has important application in optoelectronic areas, such as it can pass through beche-de-mer without spike
The laser (such as 1.064 μm) of near infrared band is extended to middle infrared by the means such as amount oscillation or optically erasing；It can also be right
Important laser (such as CO in mid-infrared light area2Laser, 10.6 μm) frequency multiplication is carried out, this has for obtaining the continuously adjustable laser of wavelength
It is significant.Therefore the large scale novel infrared nonlinear optical crystal material of searching excellent performance has become current non-linear
One of the difficult point of optical material research field and forward position direction.
Summary of the invention
One of the objects of the present invention is to provide a kind of large-sized KHg4Ga5Se12Nonlinear optical crystal.
Another object of the present invention is to provide KHg4Ga5Se12The preparation method of nonlinear optical crystal.
Still a further object of the present invention is to provide KHg4Ga5Se12The purposes and device for non-linear optical of nonlinear optical crystal.
The present invention provides a kind of KHg4Ga5Se12Nonlinear optical crystal, the KHg4Ga5Se12Nonlinear optical crystal is not
Have symmetrical centre, belong to trigonal system, space group R3, cell parameter are as follows:
α=β=90 °, γ=120 °, Z=3.
As a kind of better choice of above-mentioned nonlinear optical crystal, the second nonlinear light of the nonlinear optical crystal
Coefficient is d33=65pm/V, transparency range be 0.8-20 μm, 2.09 μm at it is birefringent be 0.07.Within this range non-thread
Property optical crystal has the advantages that nonlinear optical effect is very big, transparency range is wide.
As a kind of better choice of above-mentioned nonlinear optical crystal, the nonlinear optical crystal thermal stable temperature is not low
In 900K.
As a kind of better choice of above-mentioned nonlinear optical crystal, the nonlinear optical crystal size is not less than40*
100mm.The size of nonlinear optical crystal of the invention is larger, so that more having application value.
The present invention also provides the preparation methods of above-mentioned nonlinear optical crystal, to pass through high-temperature fusant spontaneous crystallization method
Grow KHg4Ga5Se12Nonlinear optical crystal the steps include: powdered KHg4Ga5Se12Compound is heated to melting to obtain high temperature
Melt and after being kept for 24-96 hours, is cooled to room temperature with 1-10 DEG C/h of rate of temperature fall, it is transparent to obtain peony
KHg4Ga5Se12Crystal.
The powdered KHg4Ga5Se12Preparing for compound is as follows:
By K source material, Hg source material, Ga source material and Se simple substance according to the ratio of molar ratio K:Hg:Ga:Se=1:4:5:12
After mixing, be heated to 800-950 DEG C of progress solid phase reaction (in principle, can be made using general chemical synthesis process example
Standby KHg4Ga5Se12Compound；The preferred solid reaction process of the present invention), obtaining chemical formula is KHg4Ga5Se12Compound, through smashing to pieces
Grind to obtain powdered KHg4Ga5Se12Compound；
The K source material is K or K2Se；
The Hg source material is Hg or HgSe；
The Ga source material is Ga or Ga2Se3。
The KHg4Ga5Se12Compound can be prepared by following chemical equations:
(1) K+4Hg+5Ga+12Se=KHg4Ga5Se12；
(2)K2Se+8Hg+10Ga+23Se=2KHg4Ga5Se12；
(3) K+4HgSe+5Ga+8Se=KHg4Ga5Se12；
(4)2K+8Hg+5Ga2Se3+ 9Se=2KHg4Ga5Se12；
(5)K2Se+8HgSe+10Ga+15Se=2KHg4Ga5Se12；
(6)K2Se+8Hg+5Ga2Se3+ 8Se=2KHg4Ga5Se12；
(7)2K+8HgSe+5Ga2Se3+ 8Se=2KHg4Ga5Se12；
(8)K2Se+8HgSe+5Ga2Se3=2KHg4Ga5Se12。
The present invention also provides KHg4Ga5Se12Another preparation method of nonlinear optical crystal, to be declined by crucible
Method grows KHg4Ga5Se12Nonlinear optical crystal, its step are as follows:
By K source material, Hg source material, Ga source material and simple substance Se simple substance according to molar ratio K:Hg:Ga:Se=1:4:5:12
Ratio be put into crystal growing apparatus, be to slowly warm up to melting sources, after raw material is completely melt, crystal growing apparatus with
The speed of 0.1-10mm/h vertically declines, and carries out KHg during crystal growing apparatus decline4Ga5Se12Nonlinear optical crystal
Growth, growth cycle are 5-20 days；
The K source material is K or K2Se；
The Hg source material is Hg or HgSe；
The Ga source material is Ga or Ga2Se3。
KHg having a size of Centimeter Level can get using above two method4Ga5Se12Nonlinear optical crystal obtains ruler
It is very little to be not less thanThe nonlinear optical crystal of 40*100mm.Using large scale crucible, and extend growth period, then can get accordingly more
Large scale KHg4Ga5Se12Nonlinear optical crystal.
According to the crystallography data of crystal, crystal boule is oriented, is cut by required angle, thickness and sectional dimension brilliant
Body polishes crystal light pass surface, can be used as device for non-linear optical use, the KHg4Ga5Se12Nonlinear optical crystal has
Nonlinear optical effect is very big, transparency range is wide, physical and chemical performance is stable, and hardness is larger, good mechanical property, not easily broken,
Be not easy to deliquesce, it is easy to process and save the advantages that.
The present invention furthermore provides KHg4Ga5Se12The purposes of nonlinear optical crystal, the KHg4Ga5Se12Nonlinear optical
It learns crystal and is used to prepare device for non-linear optical, which includes to pass through at least a branch of incidence electromagnetic radiation extremely
Few one piece of KHg4Ga5Se12The output spoke that at least a branch of frequency is different from incidence electromagnetic radiation is generated after nonlinear optical crystal
The device penetrated.
Further, the present invention provides a kind of device for non-linear optical, which includes will at least one
Beam incidence electromagnetic radiation passes through any KHg of at least one piece of claim 1-44Ga5Se12Generated after nonlinear optical crystal to
Few a branch of frequency is different from the device of the output radiation of incidence electromagnetic radiation.
Use KHg of the invention4Ga5Se12The device of nonlinear optical crystal production can be a times frequency generator, above and below
Frequency converter, optical parametric oscillator or photoparametric amplifier etc..
KHg of the invention4Ga5Se12Nonlinear optical crystal and its preparation method and application has the effect that
In the KHg4Ga5Se12The growing crystals of nonlinear optical crystal are easily grown up and transparent no package, have growth speed
The advantages that degree is very fast, at low cost, is easy to get larger size crystal；KHg obtained4Ga5Se12Nonlinear optical crystal has
Compare that nonlinear optical effect is very big, transmission region is wide, hardness is larger, good mechanical property, not easily broken and deliquesce, is easy to process
The advantages that with saving；The KHg4Ga5Se12Nonlinear optical crystal can be used for making device for non-linear optical.
Detailed description of the invention
Fig. 1 is using KHg of the present invention4Ga5Se12A kind of typical device for non-linear optical made of nonlinear optical crystal
Working principle diagram, wherein 1 is laser, 2 be incoming laser beam, and 3 be after crystal post-processing and optical manufacturing
KHg4Ga5Se12Nonlinear optical crystal, 4 be generated shoot laser beam, and 5 be filter plate；
Fig. 2 is KHg4Ga5Se12The structural schematic diagram of nonlinear optical crystal.
Specific embodiment
It the following is the embodiment of the present invention, be used only as explanation of the invention and not limit.
Embodiment 1 prepares KHg using high-temperature fusant spontaneous crystallization method4Ga5Se12Crystal:
Weigh 0.393 gram of K2Se, 2.236 grams of HgSe and 1.882 gram of Ga2Se3(i.e. K2Se:HgSe:Ga2Se3=
0.001mol:0.008mol:0.005mol), after evenly mixing, it is fitted into the quartz glass tube of Φ 12mm × 20mm, vacuumizes
To 10-3It after pa, is packaged and placed in tubular type growth furnace with oxyhydrogen flame, is slowly increased to 900 DEG C, constant temperature 72 hours, with the speed of 1 DEG C/h
Rate slow cooling closes tubular type growth furnace to room temperature；It is cut after quartz ampoule is cooling, wine-colored KHg can be obtained4Ga5Se12It is brilliant
Body.Crystalline size is40*100mm, nonlinear second-order optical susceptibility d33=65pm/V, transparency range are 0.8-20 μm,
Birefringent at 2.09 μm is 0.07, and thermal stable temperature is not less than 900K.
Embodiment 2 prepares KHg using Bridgman-Stockbarger method4Ga5Se12Crystal:
Weigh 1.965 grams of K2Se, 11.178 grams of HgSe and 9.408 gram of Ga2Se3(i.e. K:Hg:Ga:Se=0.01mol:
0.04mol:0.05mol:0.12mol), after evenly mixing, it is fitted into the quartz glass tube of Φ 25mm × 200mm, is evacuated to
10-3It after pa, is packaged and placed in crystal growing furnace with oxyhydrogen flame, being slowly increased to 900 DEG C makes melting sources, is completely melt to raw material
Afterwards, grower was vertically declined with 0.1-10mm/ hours speed；After crystal growth, grower was down to 50 hours
Room temperature obtains wine-colored KHg4Ga5Se12Crystal.Crystalline size is45*100mm, nonlinear second-order optical susceptibility d33=
65pm/V, transparency range are that 0.8-20 μm, 2.09 μm the birefringent of place is 0.07, and thermal stable temperature is not less than 900K.
After tested, KHg prepared by above-described embodiment 1-24Ga5Se12Nonlinear optical crystal category trigonal system, space group
For R3, cell parameter are as follows: its cell parameter are as follows: α=β=90 °,
γ=120 °, Z=3,With frequency-doubled effect, nonlinear second-order optical susceptibility d33=65pm/V, light transmission
Range is that 0.8-20 μm, 2.09 μm the birefringent of place is 0.07, and thermal stable temperature is not less than 900K；Fig. 2 is the KHg4Ga5Se12
The structural schematic diagram of nonlinear optical crystal.
Embodiment 3:
The resulting KHg of embodiment 1-24Ga5Se12Crystal is not easily broken, is not easy to deliquesce, easy to cut, polishing and guarantor
It deposits.By the resulting KHg of embodiment 1-24Ga5Se12Crystal is placed at position of 1 shown device of attached drawing marked as 3, at room temperature,
With the Ho:Tm:Cr:YAG laser light source for adjusting Q, incident wavelength is the infrared light of 2090nm, times that output wavelength is 1045nm
Frequency light, laser intensity are AgGaS under the same terms220 times.
Fig. 1 is using KHg of the present invention4Ga5Se12A kind of typical device for non-linear optical made of nonlinear optical crystal
Working principle diagram, wherein 1 is laser, 2 be incoming laser beam, and 3 be that size after crystal post-processing and optical manufacturing is
The KHg of 10x10x30mm4Ga5Se12Nonlinear optical crystal, 4 be generated shoot laser beam, and 5 be filter plate；By laser
1, which issues incoming laser beam 2, injects KHg4Ga5Se12Monocrystal 3, generated shoot laser beam 4 obtain institute by filter plate 5
The laser beam needed.
Use KHg of the invention4Ga5Se12The device of nonlinear optical crystal production can be a times frequency generator, above and below
Frequency converter, optical parametric oscillator or photoparametric amplifier etc..
It should be noted last that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting.Although ginseng
It is described the invention in detail according to embodiment, those skilled in the art should understand that, to technical side of the invention
Case is modified or replaced equivalently, and without departure from the spirit and scope of technical solution of the present invention, should all be covered in the present invention
Scope of the claims in.
Claims (7)
1. a kind of KHg4Ga5Se12Nonlinear optical crystal, the KHg4Ga5Se12Nonlinear optical crystal does not have symmetrical centre,
Belong to trigonal system, space group R3, cell parameter are as follows: α=β=
90 °, γ=120 °, Z=3.
2. nonlinear optical crystal according to claim 1, it is characterised in that: the second order of the nonlinear optical crystal is non-
Linear optics coefficient is d33=65pm/V, transparency range be 0.8-20 μm, 2.09 μm at it is birefringent be 0.07.
3. nonlinear optical crystal according to claim 1, it is characterised in that: the nonlinear optical crystal thermostabilization temperature
Degree is not less than 900K.
4. nonlinear optical crystal according to claim 1, it is characterised in that: the nonlinear optical crystal size is not small
In
5. KHg described in a kind of claim 44Ga5Se12The preparation method of nonlinear optical crystal is high-temperature fusant spontaneous crystallization
Method the steps include:
K source material, Hg source material, Ga source material and Se simple substance are mixed according to the ratio of molar ratio K:Hg:Ga:Se=1:4:5:12
Conjunction is heated to melting obtaining high temperature solution and after being kept for 24-96 hours, is cooled to room temperature with 1-10 DEG C/h of rate of temperature fall, obtains
To KHg4Ga5Se12Crystal
The K source material is K or K2Se；
The Hg source material is Hg or HgSe；
The Ga source material is Ga or Ga2Se3。
6. KHg described in a kind of claim 44Ga5Se12The preparation method of nonlinear optical crystal is Bridgman-Stockbarger method, step
It is rapid as follows:
K source material, Hg source material, Ga source material and Se simple substance are put according to the ratio of molar ratio K:Hg:Ga:Se=1:4:5:12
Enter in crystal growing apparatus, be to slowly warm up to melting sources, after raw material is completely melt, crystal growing apparatus is with 0.1-10mm/h
Speed vertically decline, crystal growing apparatus decline during carry out KHg4Ga5Se12Nonlinear optical crystal growth, life
Long period is 5-20 days；
The K source material is K or K2Se；
The Hg source material is Hg or HgSe；
The Ga source material is Ga or Ga2Se3。
7. a kind of device for non-linear optical, which is characterized in that the device for non-linear optical includes will at least a branch of incoming electromagnetic spoke
It penetrates through any KHg of at least one piece of claim 1-44Ga5Se12At least a branch of frequency is generated after nonlinear optical crystal not
It is same as the device of the output radiation of incidence electromagnetic radiation.
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| CN103031607A (en) * | 2012-12-12 | 2013-04-10 | 中国科学院福建物质结构研究所 | Infrared nonlinear optical crystal AB4C5Se12 |
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Application publication date: 20181228 |