CN103031605A - Nonlinear optical crystal potassium strontium fluorine carbonate - Google Patents
Nonlinear optical crystal potassium strontium fluorine carbonate Download PDFInfo
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- CN103031605A CN103031605A CN2011103040685A CN201110304068A CN103031605A CN 103031605 A CN103031605 A CN 103031605A CN 2011103040685 A CN2011103040685 A CN 2011103040685A CN 201110304068 A CN201110304068 A CN 201110304068A CN 103031605 A CN103031605 A CN 103031605A
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Abstract
一种非线性光学晶体氟碳酸锶钾，其化学式为KSrCO3F(简称KSCF)。其晶体结构属于六方晶系，空间群为
A nonlinear optical crystal potassium strontium fluorocarbonate, the chemical formula of which is KSrCO 3 F (abbreviated as KSCF). Its crystal structure belongs to the hexagonal crystal system, and its space group is
Description
Technical field
The present invention relates to a kind of photoelectron functional materials and growth method and purposes, particularly relate to a kind of non-linear optical crystal material and its production and use, i.e. fluorine Strontium carbonate powder potassium, its chemical formula is KSrCO
3F is called for short KSCF.
Background technology
The non-linear optical effect of crystal refers to a kind of like this effect: when a branch of laser with certain polarization direction passes through a non-linear optic crystal (such as KSCF) by certain incident direction, the frequency of this light beam will change.
Crystal with non-linearity optical effect is called non-linear optic crystal.Utilize non-linear optic crystal to carry out the laser frequency conversion, widen the scope of optical maser wavelength, make applications of laser more extensive.Especially the crystal such as borate family non-linear optic crystal such as BBO, LBO, KBBF, SBBO, TBO, KABO, BABO receive much attention with its excellent optical property.Development in photo-optics, photoengraving, precision instrument processing and other fields more and more needs ultraviolet and deep ultraviolet laser coherent source, namely needs ultraviolet and the deep ultraviolet nonlinear optical crystal of excellent performance.
The basic structure primitive of KBBF is (BO
3)
3-Plane group, the ultraviolet absorption edge of this crystal have moderate degree of birefringence (Δ n=0.07) about 155nm, can realize very wide phase matched scope, are classic deep ultraviolet nonlinear optical crystals so far.But because KBBF is a kind of crystal of laminate structure, be connected by electrostatic attraction rather than by valence link between layers, the stratiform habit is serious, and is very slow in the z direction speed of growth, and the single crystal demixing phenomenon that grows is obvious, and crystal is difficult for growth.
The basic structure primitive of SBBO also is (BO
3)
3-The plane group, but it replaces fluorion with oxygen, and so that interconnect by oxo bridge between layers, in order to improve the stratiform habit of KBBF, it is substantially constant that the structure of every one deck then keeps.SBBO not only has larger macroscopical Clock Multiplier Factor, low ultraviolet absorption edge (165nm), and moderate degree of birefringence (Δ n=0.06), and thoroughly overcome the stratiform habit of crystal, solved the problem of crystal growth.On this basis, keep (BO
3)
3-The structural condition of group is substantially constant, replaces kation S r
2+With the Be atom, in succession developed a series of non-linear optic crystals such as TBO, KABO, BABO, they are referred to as the SBBO group crystal.They have overcome the stratiform habit of KBBF single crystal growing, but up to the present these crystal can't replace the KBBF monocrystalline, because the structural integrity of SBBO and TBO crystal is bad, the non-constant of optical homogeneity that its macro property shows also can't be applied in practical devices at present; The structural integrity of KABO and BABO crystal is fine, has preferably optical homogeneity, but because Al has replaced Be, their ABSORPTION EDGE red shift is difficult to the harmonic wave of deep ultraviolet to about the 180nm.
Because (CO
3)
2-With (BO
3)
3-Structure similar with ligancy, we think available (CO
3)
2-Replace (BO
3)
3-, then with the alkali and alkaline earth metal ions ion as positively charged ion, add fluorion and adjust interlayer structure, thereby obtain novel compound, the application of developing deep ultraviolet nonlinear optical crystal.Through solid phase synthesis, the crystal growth, single crystal structure determination has confirmed that this imagination is possible.
Summary of the invention
The object of the present invention is to provide a kind of fluorine Strontium carbonate powder potassium compound, its chemical formula is KSrCO
3F.
Another object of the present invention is to provide a kind of fluorine Strontium carbonate powder potassium compound preparation method.
Another object of the present invention is to provide a kind of fluorine Strontium carbonate powder nonlinear optical crystal of potassium, its chemical formula is KSrCO
3F.
A further object of the present invention is to provide a kind of growth method of fluorine Strontium carbonate powder nonlinear optical crystal of potassium.
A further object of the invention is to provide the purposes of fluorine Strontium carbonate powder nonlinear optical crystal of potassium.
Technical scheme of the present invention is as follows:
Fluorine Strontium carbonate powder potassium compound provided by the invention, its chemical formula is KSrCO
3F.
The preparation method of fluorine Strontium carbonate powder potassium compound provided by the invention, its step is as follows: the raw materials of compound that will contain K, Sr, C and F is K: Sr: C: F=1 in its mol ratio: behind the even mixed grinding of 1: 1: 1 ratio, pack in the platinum alloy crucible, after 300～400 ℃ of the slow intensifications, pre-burning 1～5 hour; Be cooled to room temperature, take out and grind; Then 500～600 ℃ of lower sintering 12～20 hours, be cooled to room temperature, take out and grind, obtain Powdered fluorine Strontium carbonate powder potassium compound of the present invention, it is carried out XRD detect that (Fig. 3 a), its molecular formula is KSrCO
3F.The described K of containing raw materials of compound is fluorochemical or the carbonate that contains potassium, and the described Sr of containing raw materials of compound is fluorochemical or the carbonate that contains strontium, and the described C of containing raw materials of compound is K
3CO
3Or SrCO
3, the described F of containing raw materials of compound is KF or SrF
2
Fluorine Strontium carbonate powder nonlinear optical crystal of potassium provided by the invention, its chemical formula is KSrCO
3F, this crystal does not have symmetry centre, belongs to hexagonal system, and spacer is P6m2, and unit cell parameters is
α=β=90 °, γ=120 °, z=1, unit-cell volume is
Crystalline structure such as Fig. 2.
The growth method of fluorine Strontium carbonate powder nonlinear optical crystal of potassium provided by the invention, its step is as follows: with KF and K
2CO
3Be fluxing agent growth, KF/K
2CO
3Mol ratio is 1/2～2/1, solute and solvent mol ratio are 1/4～1/2 during take K as benchmark, raw material is mixed according to the above ratio, heat up 700～800 ℃ and melt fully to raw material, behind the constant temperature 1～20 hour, be cooled to rapidly above 5～10 ℃ of temperature of saturation, then by every day 1～5 ℃ speed be cooled to 600 ℃, close stove; After sample was cooled to room temperature, water flush away fusing assistant namely obtained fluorine Strontium carbonate powder nonlinear optical crystal of potassium of the present invention, is of a size of 0.5 * 0.4 * 0.3mm.The raw materials of compound that adopts is fluorochemical or the carbonate that contains potassium, the fluorochemical that contains strontium or carbonate, K
2CO
3Or SrCO
3With KF or SrF
2The lenticular fluorine Strontium carbonate powder potassium that obtains, grind into powder carries out XRD to it and detects result such as Fig. 3 b again.
The growth method of fluorine Strontium carbonate powder nonlinear optical crystal of potassium provided by the invention, its step is as follows: adopt KF-SrF
2The fusing assistant system, KF/SrF
2Mol ratio is 1/3～3/1, solute and solvent mol ratio are 1/4～1/2 during take K as benchmark, raw material is mixed according to the above ratio, heat up 700～800 ℃ and melt fully to raw material, behind the constant temperature 1～20 hour, be cooled to rapidly above 5～10 ℃ of temperature of saturation, the lower end that seed crystal is fixed on seed rod contacts the growth of beginning crystal with melt liquid level; The speed of rotation of seed rod is 10～20 rev/mins, is cooled to temperature of saturation, then presses 1～5 ℃/day speed slow cooling; Cooling is lifted from liquid level with crystal after finishing, and is down to room temperature with 10～30 ℃/hour speed, obtains fluorine Strontium carbonate powder nonlinear optical crystal of potassium of the present invention.The raw materials of compound that adopts is fluorochemical or the carbonate that contains potassium, the fluorochemical that contains strontium or carbonate, K
2CO
3Or SrCO
3With KF or SrF
2The lenticular fluorine Strontium carbonate powder potassium that obtains is of a size of 12 * 10 * 6mm, and grind into powder carries out XRD to it and detects result such as Fig. 3 b again.
The purposes of fluorine Strontium carbonate powder nonlinear optical crystal of potassium provided by the invention, this non-linear optic crystal fluorine Strontium carbonate powder potassium is used for the frequency transformation of laser device laser output.
The purposes of fluorine Strontium carbonate powder nonlinear optical crystal of potassium provided by the invention, this crystal produces 2 frequencys multiplication for the laser beam that to wavelength is 1.064 μ m, 3 frequencys multiplication, 4 frequencys multiplication, the humorous glistening light of waves output of 5 frequencys multiplication.
The purposes of fluorine Strontium carbonate powder nonlinear optical crystal of potassium provided by the invention, this crystal are lower than the humorous glistening light of waves output of 200nm for generation of wavelength.
The purposes of fluorine Strontium carbonate powder nonlinear optical crystal of potassium provided by the invention, described non-linear optic crystal is for being used for the harmonic generator of ultraviolet region, optical parameter and amplifying device and fiber waveguide device.
The purposes of fluorine Strontium carbonate powder nonlinear optical crystal of potassium provided by the invention, described non-linear optic crystal are optical parameter and the amplifying device from infrared to the ultraviolet region.
It is KSrCO that effect of the present invention is to provide a kind of chemical formula
3The compound of F, non-linear optic crystal of this compound and its production and use.Use the powder frequency doubling testing method to measure KSrCO
3The phase matched ability of F, its powder SHG effect is KH for its Clock Multiplier Factor
2PO
4(KDP) 3.4 times.Its ultraviolet absorption edge is shorter than 200nm.KSrCO
3The F crystal can be realized 2 frequencys multiplication of Nd:YAG (λ=1.064 μ m), and, can predict KSrCO
3F can be used in 3 frequencys multiplication, 4 frequencys multiplication of Nd:YAG, the harmonic generator of 5 frequencys multiplication, even for generation of the humorous glistening light of waves output shorter than 200nm.In addition, KSrCO
3F monocrystalline water white transparency is congruent compound, approximately 690 ℃ of fusing points, and chemical stability is good.So can predict KSrCO
3F will obtain widespread use in various non-linear optical fields, and will open up the nonlinear optics application of deep ultraviolet wave band.
Description of drawings
Fig. 1 is KSrCO
3The F crystal is used the canonical schema of non-linear hour optical effect as frequency-doubling crystal, wherein 1 is laser apparatus, and the 2nd, incoming laser beam, the 3rd, through the KSrCO of crystal aftertreatment and optics processing
3The F single crystal, the 4th, the outgoing laser beam that produces, the 5th, filter plate.
Fig. 2 is KSrCO
3F crystal unit cell structural representation.
Fig. 3 is KSrCO
3The x ray diffraction collection of illustrative plates of F, wherein 3a is solid phase synthesis KSrCO
3The diffractogram of F powdered sample, 3b are KSrCO
3The F monocrystalline last diffractogram of pulverizing.
Embodiment
Embodiment 1
Adopt high temperature solid state reaction synthetic compound KSrCO
3F
Raw materials used: SrCO
31.4763 gram (0.01mol)
KF 0.5810 gram (0.01mol)
Its chemical equation is:
SrCO
3+KF＝KSrCO
3F
Concrete operation step is as follows: after in operation box above-mentioned raw materials being weighed up by above-mentioned dosage, put into that mortar mixes and carefully grind, then pack in the platinum alloy crucible of Φ 30 * 30mm, with spoon its compression is added a cover, put into retort furnace (retort furnace places stink cupboard, and the fume hood exhaust mouth is by the water tank exhaust), slowly be warming up to 400 ℃ and constant temperature pre-burning 3 hours, the beginning temperature rise rate must be slow, and control causes the variation of proportioning because of decomposition, solid state reaction is fully carried out.Take out crucible after the cooling, this moment, sample was more loose.Then take out sample and again grind evenly in operation box, place crucible to compress again and add a cover, in 600 ℃ of lower sintering 20 hours, take out after the cooling in retort furnace, at this moment sample is formed one, sample is put into mortar smash grinding to pieces and namely get product.This product is carried out X-ray analysis, and (Fig. 3 a) and KSrCO for the gained spectrogram
3The F monocrystalline last X ray picture (Fig. 3 b) of pulverizing is consistent.
Embodiment 2
Adopt high temperature solid state reaction synthetic compound KSrCO
3F
Raw materials used: K
2CO
31.3820 gram (0.01mol)
SrCO
31.4763 gram (0.01mol)
SrF
21.2563 gram (0.01mol)
Its chemical equation is:
K
2CO
3+SrCO
3+SrF
2＝2KSrCO
3F
Concrete operation step is as follows: after in operation box above-mentioned raw materials being weighed up by above-mentioned dosage, put into that mortar mixes and carefully grind, then pack in the platinum alloy crucible of Φ 30 * 30mm, with spoon its compression is added a cover, put into retort furnace (retort furnace places stink cupboard, and the fume hood exhaust mouth is by the water tank exhaust), slowly be warming up to 400 ℃ and constant temperature pre-burning 3 hours, the beginning temperature rise rate must be slow, and control causes the variation of proportioning because of decomposition, solid state reaction is fully carried out.Take out crucible after the cooling, this moment, sample was more loose.Then take out sample and again grind evenly in operation box, place crucible to compress again and add a cover, in 600 ℃ of lower sintering 20 hours, take out after the cooling in retort furnace, at this moment sample is formed one, sample is put into mortar smash grinding to pieces and namely get product.This product is carried out X-ray analysis, and (Fig. 3 a) and KSrCO for the gained spectrogram
3The F monocrystalline last X ray picture (Fig. 3 b) of pulverizing is consistent.
Embodiment 3
Adopt molten-salt growth crystal KSrCO
3F
Crystal growing apparatus is homemade Resistant heating stove, and temperature controlling instruments is 908PHK20 type automatic temperature control instrument able to programme.Select KF-K
2CO
3Make fusing assistant, sporadic nucleation obtains crystal.
Raw materials used: SrCO
3Analytical pure AR 29.526 grams (0.2mol)
KF analytical pure AR 11.620 grams (0.25mol)
K
2CO
3Analytical pure AR 27.639 grams (0.2mol)
Concrete operation step is as follows: after above-mentioned raw materials is weighed up by above-mentioned dosage, mix, then pack into
In the platinum alloy crucible of 60 * 60mm, place in the self-control growth furnace, heats up 750 ℃ and melt fully to raw material, constant temperature is after 10 hours, is cooled to rapidly more than the temperature of saturation 5～10 ℃, then by every day 3 ℃ speed be cooled to 600 ℃, close stove.After the sample cooling, water flush away fusing assistant namely obtains transparent KSrCO
3The F monocrystalline, it is of a size of 0.5 * 0.4 * 0.3mm.
Embodiment 4
Adopt molten-salt growth crystal KSrCO
3F
Crystal growing apparatus is homemade Resistant heating stove, and temperature controlling instruments is 908PHK20 type automatic temperature control instrument able to programme.Select KF-SrF
2Make fusing assistant, the crystal that example 3 is obtained carries out directional cutting and becomes designed seed crystal.Raw materials used:
Concrete operation step is as follows: after above-mentioned raw materials is weighed up by above-mentioned dosage, mix, then pack in the platinum alloy crucible of Φ 60 * 60mm, place in the self-control growth furnace, heat up 750 ℃ and melt fully to raw material, constant temperature is after 10 hours, be cooled to rapidly above 5～10 ℃ of temperature of saturation, seed crystal is fixed on the lower end of seed rod, from the aperture importing crucible of furnace roof section, makes seed crystal contact the growth of beginning crystal with melt liquid level.The speed of rotation of seed rod is 15 rev/mins, is cooled to temperature of saturation, then presses 1 ℃/day speed slow cooling.Cooling is lifted from liquid level with crystal after finishing, and is down to room temperature with 20 ℃/hour speed, namely obtains the KSrCO of large-size
3The F monocrystalline, it is of a size of 12 * 10 * 6mm.
Embodiment 5
The crystal that example 4 is obtained, the processing cutting, directed, polishing is placed on the position of 3 in the device shown in Figure 1, at room temperature, with transferring Q Nd:YAG laser to do the input light source, incident wavelength is 1064nm, observe obvious 532nm frequency doubling green light output, output intensity is about 3.4 times of equal conditions KDP.
Claims (10)
1. compound fluorine Strontium carbonate powder potassium, it is characterized in that: its chemical formula is KSrCO
3F belongs to hexagonal system, and spacer is P
6M2, unit cell parameters is
α=β=90 °, γ=120 °, z=1, unit-cell volume is
2. the preparation method of the fluorine Strontium carbonate powder potassium compound of a claim 1 is characterized in that: the raw materials of compound that will contain K, Sr, F and C by the even mixed grinding of suitable proportion after, slowly heat up after 300～400 ℃ pre-burning 1～5 hour; Be cooled to room temperature, take out and grind; Then 550～650 ℃ of lower sintering 12～20 hours, be cooled to room temperature and can obtain fluorine Strontium carbonate powder potassium compound.
3. the non-linear optic crystal of the compound fluorine Strontium carbonate powder potassium of claim 1.
4. the growth method of a fluorine Strontium carbonate powder nonlinear optical crystal of potassium claimed in claim 3 adopts molten-salt growth, it is characterized in that: with KF-K
2CO
3Be fluxing agent growth, KF/K
2CO
3Mol ratio is 1/2～2/1, solute and solvent mol ratio are 1/4～1/2 during take K as benchmark, raw material is mixed according to the above ratio, heat up 700～800 ℃ and melt fully to raw material, behind the constant temperature 1～20 hour, be cooled to rapidly above 5～10 ℃ of temperature of saturation, then by every day 1～5 ℃ speed be cooled to 600 ℃, close stove; After sample was cooled to room temperature, water flush away fusing assistant namely obtained the fluorine Strontium carbonate powder nonlinear optical crystal of potassium that the present invention is of a size of 0.5 * 0.4 * 0.3mm.
5. the growth method of a fluorine Strontium carbonate powder nonlinear optical crystal of potassium claimed in claim 3 adopts molten-salt growth, it is characterized in that: adopt KF-SrF
2The fusing assistant system, KF/SrF
2Mol ratio is 1/3～3/1, solute and solvent mol ratio are 1/4～1/2 during take K as benchmark, raw material is mixed according to the above ratio, heat up 700～800 ℃ and melt fully to raw material, behind the constant temperature 1～20 hour, be cooled to rapidly above 5～10 ℃ of temperature of saturation, the lower end that seed crystal is fixed on seed rod contacts the growth of beginning crystal with melt liquid level; The speed of rotation of seed rod is 10～20 rev/mins, is cooled to temperature of saturation, then presses 1～5 ℃/day speed slow cooling; Cooling is lifted from liquid level with crystal after finishing, and is down to room temperature with 10～30 ℃/hour speed, obtains 12 * 10 * 6mm fluorine Strontium carbonate powder nonlinear optical crystal of potassium that is of a size of of the present invention.
6. the purposes of a fluorine Strontium carbonate powder nonlinear optical crystal of potassium claimed in claim 3 is characterized in that: the frequency transformation that this non-linear optic crystal is exported for laser device laser.
7. the purposes of a fluorine Strontium carbonate powder nonlinear optical crystal of potassium claimed in claim 6 is characterized in that: it is the humorous glistening light of waves output that the laser beam of 1.064 μ m produces 2 frequencys multiplication or 3 frequencys multiplication or 4 frequencys multiplication or 5 frequencys multiplication that this non-linear optic crystal is used for wavelength.
8. the purposes of a fluorine Strontium carbonate powder nonlinear optical crystal of potassium claimed in claim 6 is characterized in that: this non-linear optic crystal is lower than the humorous glistening light of waves output of 200nm for generation of wavelength.
9. the purposes of a fluorine Strontium carbonate powder nonlinear optical crystal of potassium claimed in claim 6 is characterized in that: described non-linear optic crystal is for being used for the harmonic generator of ultraviolet region, optical parameter and amplifying device and fiber waveguide device.
10. the purposes of a fluorine Strontium carbonate powder nonlinear optical crystal of potassium claimed in claim 6 is characterized in that: described non-linear optic crystal is optical parameter and amplifying device from infrared to the ultraviolet region.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018165583A1 (en) * | 2017-03-10 | 2018-09-13 | University Of Houston System | Nonlinear optical material |
| CN113481596A (en) * | 2021-06-02 | 2021-10-08 | 四川师范大学 | Nonlinear optical crystal potassium oxyfluoroniobate and preparation method and application thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018165583A1 (en) * | 2017-03-10 | 2018-09-13 | University Of Houston System | Nonlinear optical material |
| US11262640B2 (en) | 2017-03-10 | 2022-03-01 | University Of Houston System | Nonlinear optical material |
| CN113481596A (en) * | 2021-06-02 | 2021-10-08 | 四川师范大学 | Nonlinear optical crystal potassium oxyfluoroniobate and preparation method and application thereof |
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Application publication date: 20130410 |