CN102660772A - Nonlinear optics crystal boric acid of oxygen, cadmium and lutetium - Google Patents
Nonlinear optics crystal boric acid of oxygen, cadmium and lutetium Download PDFInfo
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- CN102660772A CN102660772A CN2012101252299A CN201210125229A CN102660772A CN 102660772 A CN102660772 A CN 102660772A CN 2012101252299 A CN2012101252299 A CN 2012101252299A CN 201210125229 A CN201210125229 A CN 201210125229A CN 102660772 A CN102660772 A CN 102660772A
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- lutetium
- boric acid
- cadmium
- crystal
- acid oxygen
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Abstract
The present invention relates to crystal boric acid of oxygen, cadmium lutetiums. Its chemical formula Cd4LuO (BO3) 3, belongs to monoclinic system, space group Cm, and cell parameter is
α=γ=90 °, β=99.972 °, z=2, unit-cell volume are
Its Clock Multiplier Factor is 5.3 times of KH2PO4 (KDP). It is 340-6250nm through wave band. It is sintered at high temperature using solid phase synthesis process and obtains Cd4LuO (BO3) 3 compound. Using molten-salt growth method, monocrystal can be gone out with successful growth by making fluxing agent with B2O3. Cd4LuO (BO3) 3 has nonlinear optical effect, and does not deliquesce, and physico-chemical property is stablized, and can be used widely in various non-linear optical fields.
Description
Technical field
The present invention relates to a kind of new type light electronic functional material and growth method and purposes, particularly relate to a kind of non-linear optical crystal material, i.e. boric acid oxygen cadmium lutetium, its chemical formula is Cd
4LuO (BO
3)
3
Technical background
The crystalline non-linear optical effect is meant a kind of like this effect: when a branch of laser with certain polarization direction passes through a non-linear optic crystal (like Cd by certain incident direction
4LuO (BO
3)
3) time, 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 the application of laser more extensive.Especially 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.
Applicable non-linear optic crystal mainly is LBO (LiB in the ultraviolet region at present
3O
5) and BBO (BaB
2O
4) two kinds, their growing technology and growth technique are very ripe, can grow high quality, large-sized monocrystalline.Bbo crystal is one of ultraviolet non-linear optic crystal that can produce up to now effective five frequencys multiplication, can also obtain the output of effective 193nm simultaneously through the method with frequency.This crystal has bigger specific refractory power, can realize the direct frequency multiplication from 202.8nm to the 2600nm scope, therefore is widely used in optical parametric oscillation and the various harmonic generator.LBO has wide transparency range, and optical homogeneity is good, and Clock Multiplier Factor is moderate, and acceptance angle can be realized 90 ° of noncritical phase matchings than broad.Because the degree of birefringence of LBO is too little, thereby limited its phase matched scope in the ultraviolet region.Because the anisotropy of the thermal expansivity of lbo crystal; Cause when the high temperature plated film, causing easily the damage of quartz crystal device; And bbo crystal has faint deliquescence, in the device fabrication process, causes damage easily, remedies this defective so we must seek novel ultraviolet nonlinear crystal.
The novel non-linearity crystal should have and very wide sees through wave band and big non-linear effectiveness, and good physical and chemical performance.Introduce asymmetric unitary CdO
nGet into the RE borate system and can effectively increase non-linear effect, also can obtain good physical and chemical performance.Through solid phase synthesis, crystal growth, single crystal structure determination, we have obtained Cd
4LuO (BO
3)
3, confirmed that this imagination is possible.
Summary of the invention
The object of the present invention is to provide a kind of boric acid oxygen cadmium lutetium compound, its chemical formula is Cd
4LuO (BO
3)
3
Another object of the present invention is to provide a kind of boric acid oxygen cadmium lutetium compound preparation method.
Another object of the present invention is to provide a kind of boric acid oxygen cadmium lutetium non-linear optic crystal, its chemical formula is Cd
4LuO (BO
3)
3
A purpose more of the present invention is to provide a kind of growth method of boric acid oxygen cadmium lutetium non-linear optic crystal.
A further object of the invention is to provide the purposes of boric acid oxygen cadmium lutetium non-linear optic crystal.
Technical scheme of the present invention is following:
Boric acid oxygen cadmium lutetium compound provided by the invention, its chemical formula is Cd
4LuO (BO
3)
3
The preparation method of boric acid oxygen cadmium lutetium compound provided by the invention; Its step is following: the raw materials of compound that will contain Cd, Lu and B is Cd: Lu: B=4 in its mol ratio: after 1: 3 ratio uniform mixing grinds; Pack in the platinum alloy crucible, slowly heat up after 300~400 ℃ pre-burning 1~5 hour; Be cooled to room temperature, take out and grind; 800~900 ℃ of following sintering 12~20 hours, be cooled to room temperature then, take out and grind, obtain Powdered boric acid oxygen cadmium lutetium compound of the present invention, it is carried out XRD detect that (Fig. 3 a), its molecular formula is Cd
4LuO (BO
3)
3The described Cd of containing raw materials of compound is oxide compound or the carbonate that contains cadmium, and the described Lu of containing raw materials of compound is oxide compound or the carbonate that contains yttrium, and the described B of containing raw materials of compound is B
2O
3Or H
3BO
3.
Boric acid oxygen cadmium lutetium non-linear optic crystal provided by the invention, its chemical formula is Cd
4LuO (BO
3)
3, belonging to oblique system, spacer is Cm, unit cell parameters does
α=γ=90 °, β=99.972 °, z=2, unit-cell volume does
Crystalline structure such as Fig. 2.
The growth method of boric acid oxygen cadmium lutetium non-linear optic crystal provided by the invention, its step is following: with B
2O
3Be fluxing agent growth; Solute and solvent mol ratio are 1/2~1/1 when being benchmark with B, and raw material is mixed according to the above ratio, heat up 1150~1200 ℃ to melt fully to raw material; Behind the constant temperature 1~20 hour; Be cooled to above 5~10 ℃ of temperature of saturation rapidly, then by every day 1~5 ℃ speed be cooled to 800 ℃, close stove; After treating that sample is cooled to room temperature, water flush away fusing assistant promptly obtains 0.5 * 0.4 * 0.4mm boric acid oxygen cadmium lutetium non-linear optic crystal that is of a size of of the present invention.
The raw materials of compound that adopts is oxide compound or the carbonate that contains cadmium, contains the oxide compound or the carbonate of lutetium, and B
2O
3Or H
3BO
3, the lenticular boric acid oxygen cadmium lutetium that obtains, grind into powder carries out XRD to it and detects result such as Fig. 3 b again.
The growth method of boric acid oxygen cadmium lutetium non-linear optic crystal provided by the invention, its step is following: adopt B
2O
3The fusing assistant system; Solute and solvent mol ratio are 1/2~1/1 when being benchmark with B; Raw material is mixed according to the above ratio, heat up 1150~1200 ℃ and melt fully to raw material, constant temperature is after 1~20 hour; Be cooled to above 5~10 ℃ of temperature of saturation rapidly, the lower end that seed crystal is fixed on seed rod contacts the beginning crystal growth with melt liquid level; The speed of rotation of seed rod is 10~20 rev/mins, is cooled to temperature of saturation, slowly lowers the temperature by 1~5 ℃/day speed then; Cooling is lifted from liquid level with crystal after finishing, and reduces to room temperature with 10~30 ℃/hour speed, obtains 12 * 10 * 10mm boric acid oxygen cadmium lutetium non-linear optic crystal that is of a size of of the present invention.Be of a size of 12 * 10 * 10mm, grind into powder carries out XRD to it and detects result such as Fig. 3 b again.
The purposes of boric acid oxygen cadmium lutetium non-linear optic crystal provided by the invention, this nonlinear optical crystal boric acid oxygen cadmium lutetium are used for the frequency transformation of laser apparatus laser output.
It is that the laser beam of 1.064 μ m produces 2 frequencys multiplication that the purposes of boric acid oxygen cadmium lutetium non-linear optic crystal provided by the invention, this crystal are used for wavelength, the humorous glistening light of waves output of 3 frequencys multiplication.
The purposes of boric acid oxygen cadmium lutetium non-linear optic crystal provided by the invention, described non-linear optic crystal is the harmonic generator that is used for the ultraviolet region, optical parameter and amplifying device and fiber waveguide device.
The purposes of boric acid oxygen cadmium lutetium non-linear optic crystal provided by the invention, described non-linear optic crystal are optical parameter and the amplifying device from infrared to the ultraviolet region.
It is Cd that effect of the present invention is to provide a kind of chemical formula
4LuO (BO
3)
3Compound, the non-linear optic crystal of this compound.Use powder frequency multiplication testing method to measure Cd
4LuO (BO
3)
3The phase matched ability, its powder frequency-doubled effect is KH for its Clock Multiplier Factor
2PO
4(KDP) 5.3 times.Cd
4LuO (BO
3)
3Crystal can be realized 2 frequencys multiplication of Nd:YAG (λ=1.064 μ m), and, can predict Cd
4LuO (BO
3)
3Can be used in the harmonic generator of 3 frequencys multiplication of Nd:YAG.In addition, Cd
4LuO (BO
3)
3The monocrystalline water white transparency is congruent melting compound, about 1100 ℃ of fusing point, and chemicalstability is good.So can predict Cd
4LuO (BO
3)
3To in various non-linear optical fields, obtain widespread use.
Description of drawings
Fig. 1 is Cd
4LuO (BO
3)
3Crystal is as the canonical schema of frequency-doubling crystal application non-linear hour optical effect, and wherein 1 is laser apparatus, and the 2nd, incoming laser beam, the 3rd, through the Cd of crystal aftertreatment and optics processing
4LuO (BO
3)
3Single crystal, the 4th, the outgoing laser beam that is produced, the 5th, filter plate.
Fig. 2 is Cd
4LuO (BO
3)
3The crystal unit cell structural representation.
Fig. 3 is Cd
4LuO (BO
3)
3X XRD X collection of illustrative plates, wherein 3a is solid phase synthesis Cd
4LuO (BO
3)
3The diffractogram of powdered sample, 3b are Cd
4LuO (BO
3)
3The monocrystalline last diffractogram of pulverizing.Powder x ray diffraction data uses the MiniFlex diffractometer to collect at normal temperatures.
Embodiment
Adopt high temperature solid state reaction synthetic compound Cd
4LuO (BO
3)
3
Raw materials used: CdCO
32.7587 gram (0.016mol)
Lu
2O
30.7959 gram (0.002mol)
H
3BO
30.7432 gram (0.012mol)
Its chemical equation is:
8CdCO
3+Lu
2O
3+6H
3BO
3=2Cd
4LuO(BO
3)
3
The concrete operations step is following: after in operation box, above-mentioned raw materials being weighed up by above-mentioned dosage, put into that mortar mixes and carefully grind, in the platinum alloy crucible of the Φ 30 * 30mm that packs into then; With spoon it is compressed and to add a cover, put into retort furnace (retort furnace places stink cupboard, and the fume hood exhaust mouth is through 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, prevents and treats the variation that causes proportioning because of decomposition, and solid state reaction is fully carried out.Crucible is taken out in the cooling back, and this moment, sample was more loose.Then take out sample and in operation box, grind again evenly, place crucible to compress again and add a cover, in 900 ℃ of following sintering 20 hours, took out the cooling back in retort furnace, and at this moment sample is formed one, sample is put into mortar smash grinding to pieces and promptly get product.This product is carried out X-ray analysis, and (Fig. 3 a) and Cd for the gained spectrogram
4LuO (BO
3)
3The monocrystalline last X ray picture (Fig. 3 b) of pulverizing is consistent.
Adopt high temperature solid state reaction synthetic compound Cd
4LuO (BO
3)
3
Raw materials used: CdO 2.0546 grams (0.016mol)
Lu
2O
30.7959 gram (0.002mol)
H
3BO
30.7432 gram (0.012mol)
Its chemical equation is:
8CdO+Lu
2O
3+6H
3BO
3=2Cd
4LuO(BO
3)
3
The concrete operations step is following: after in operation box, above-mentioned raw materials being weighed up by above-mentioned dosage, put into that mortar mixes and carefully grind, in the platinum alloy crucible of the Φ 30 * 30mm that packs into then; With spoon it is compressed and to add a cover, put into retort furnace (retort furnace places stink cupboard, and the fume hood exhaust mouth is through 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, prevents and treats the variation that causes proportioning because of decomposition, and solid state reaction is fully carried out.Crucible is taken out in the cooling back, and this moment, sample was more loose.Then take out sample and in operation box, grind again evenly, place crucible to compress again and add a cover, in 900 ℃ of following sintering 20 hours, took out the cooling back in retort furnace, and at this moment sample is formed one, sample is put into mortar smash grinding to pieces and promptly get product.This product is carried out X-ray analysis, and (Fig. 3 a) and Cd for the gained spectrogram
4LuO (BO
3)
3The monocrystalline last X ray picture (Fig. 3 b) of pulverizing is consistent.
Adopt molten-salt growth crystal Cd
4LuO (BO
3)
3
Crystal growing apparatus is homemade wire spiral process furnace, and temperature controlling instruments is a 908PHK20 type automatic temperature control instrument able to programme.Select B for use
2O
3Make fusing assistant, sporadic nucleation obtains crystal.
The concrete operations step is following: after above-mentioned raw materials is weighed up by above-mentioned dosage, mix, in the platinum alloy crucible of the Φ 60 * 60mm that packs into then; Place in the self-control reactors; Heat up 1200 ℃ and melt fully to raw material, constant temperature was cooled to above 5~10 ℃ of temperature of saturation rapidly after 10 hours; Then by every day 3 ℃ speed be cooled to 600 ℃, close stove.After treating the sample cooling, water flush away fusing assistant promptly obtains transparent Cd
4LuO (BO
3)
3Monocrystalline, it is of a size of 0.5 * 0.4 * 0.4mm.
Adopt molten-salt growth crystal Cd
4LuO (BO
3)
3
Crystal growing apparatus is homemade wire spiral process furnace, and temperature controlling instruments is a 908PHK20 type automatic temperature control instrument able to programme.Select B for use
2O
3Make fusing assistant, the crystal that instance 3 is obtained carries out orientation and cuts into the seed crystal that is designed.
The concrete operations step is following: after above-mentioned raw materials is weighed up by above-mentioned dosage, mix, in the platinum alloy crucible of the Φ 60 * 60mm that packs into then; Place in the self-control reactors, heat up 1200 ℃ and melt fully to raw material, constant temperature is after 10 hours; Be cooled to above 5~10 ℃ of temperature of saturation rapidly; Seed crystal is fixed on the lower end of seed rod, imports crucible, seed crystal is contacted with melt liquid level begin crystal growth from the aperture of furnace roof portion.The speed of rotation of seed rod is 15 rev/mins, is cooled to temperature of saturation, slowly lowers the temperature by 1 ℃/day speed then.Cooling is lifted from liquid level with crystal after finishing, and reduces to room temperature with 20 ℃/hour speed, promptly obtains the Cd of large-size
4LuO (BO
3)
3Monocrystalline, it is of a size of 12 * 10 * 10mm.
With the crystal that instance 4 obtains, processing cutting, orientation; 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 tangible 532nm frequency multiplication green glow output, output intensity is about 5.3 times of equal conditions KDP.
Claims (9)
2. the preparation method of the boric acid oxygen cadmium lutetium compound of a claim 1 is characterized in that: after the raw materials of compound that will contain Cd, Lu and B grinds by the suitable proportion uniform mixing, slowly heat up after 300~400 ℃ pre-burning 1~5 hour; Be cooled to room temperature, take out and grind; 800~900 ℃ of following sintering 12~20 hours, be cooled to room temperature and can obtain boric acid oxygen cadmium lutetium compound then.
3. the non-linear optic crystal of the compound boric acid oxygen cadmium lutetium of claim 1.
4. the growth method of the described boric acid oxygen of claim 3 a cadmium lutetium non-linear optic crystal adopts molten-salt growth, it is characterized in that: with B
2O
3Be fluxing agent growth; Solute and solvent mol ratio are 1/2~1/1 when being benchmark with B, and raw material is mixed according to the above ratio, heat up 1150~1200 ℃ to melt fully to raw material; Behind the constant temperature 1~20 hour; Be cooled to above 5~10 ℃ of temperature of saturation rapidly, then by every day 1~5 ℃ speed be cooled to 800 ℃, close stove; After treating that sample is cooled to room temperature, water flush away fusing assistant promptly obtains described boric acid oxygen cadmium lutetium non-linear optic crystal.
5. the growth method of the described boric acid oxygen of claim 3 a cadmium lutetium non-linear optic crystal adopts molten-salt growth, it is characterized in that: adopt B
2O
3The fusing assistant system; Solute and solvent mol ratio are 1/2~1/1 when being benchmark with B; Raw material is mixed according to the above ratio, heat up 1150~1200 ℃ and melt fully to raw material, constant temperature is after 1~20 hour; Be cooled to above 5~10 ℃ of temperature of saturation rapidly, the lower end that seed crystal is fixed on seed rod contacts the beginning crystal growth with melt liquid level; The speed of rotation of seed rod is 10~20 rev/mins, is cooled to temperature of saturation, slowly lowers the temperature by 1~5 ℃/day speed then; Cooling is lifted from liquid level with crystal after finishing, and reduces to room temperature with 10~30 ℃/hour speed, obtains described boric acid oxygen cadmium lutetium non-linear optic crystal.
6. the purposes of the described boric acid oxygen of claim 3 a cadmium lutetium non-linear optic crystal is characterized in that: this non-linear optic crystal is used for the frequency transformation of laser apparatus laser output.
7. the purposes of the described boric acid oxygen of claim 6 a cadmium lutetium non-linear optic crystal is characterized in that: it is that the laser beam of 1.064 μ m produces 2 frequencys multiplication or the humorous glistening light of waves output of 3 frequencys multiplication that this crystal is used for wavelength.
8. the purposes of the described boric acid oxygen of claim 6 a cadmium lutetium non-linear optic crystal, it is characterized in that: described non-linear optic crystal is used to prepare the harmonic generator of ultraviolet region, optical parameter and amplifying device and fiber waveguide device.
9. the purposes of the described boric acid oxygen of claim 6 a cadmium lutetium non-linear optic crystal, it is characterized in that: described non-linear optic crystal is used to prepare optical parameter and the amplifying device from infrared to the ultraviolet region.
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Cited By (1)
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CN103451730A (en) * | 2012-06-05 | 2013-12-18 | 中国科学院理化技术研究所 | Cd4RO(BO3)3 compound, Cd4RO(BO3)3 optical crystal, and preparation method and application thereof |
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Cited By (2)
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CN103451730A (en) * | 2012-06-05 | 2013-12-18 | 中国科学院理化技术研究所 | Cd4RO(BO3)3 compound, Cd4RO(BO3)3 optical crystal, and preparation method and application thereof |
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Application publication date: 20120912 |