CN115710748A - Zinc carbonate ammonia nonlinear optical crystal and preparation method and application thereof - Google Patents
Zinc carbonate ammonia nonlinear optical crystal and preparation method and application thereof Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 90
- 230000003287 optical effect Effects 0.000 title claims abstract description 35
- CUHLTWOGTOCQBK-UHFFFAOYSA-L zinc;azane;carbonate Chemical compound N.[Zn+2].[O-]C([O-])=O CUHLTWOGTOCQBK-UHFFFAOYSA-L 0.000 title claims abstract description 6
- 238000002360 preparation method Methods 0.000 title abstract description 6
- HHICRQHZPBOQPI-UHFFFAOYSA-L diazanium;zinc;dicarbonate Chemical compound [NH4+].[NH4+].[Zn+2].[O-]C([O-])=O.[O-]C([O-])=O HHICRQHZPBOQPI-UHFFFAOYSA-L 0.000 claims abstract description 35
- 239000011701 zinc Substances 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000004729 solvothermal method Methods 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 3
- -1 nitrogen-containing compound Chemical class 0.000 claims description 28
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 claims description 14
- 229910052725 zinc Inorganic materials 0.000 claims description 12
- WBRIIVSCBYNWJT-UHFFFAOYSA-L zinc;azane;carbonate Chemical compound N.N.N.N.[Zn+2].[O-]C([O-])=O WBRIIVSCBYNWJT-UHFFFAOYSA-L 0.000 claims description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 9
- 239000004202 carbamide Substances 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 8
- 229960002989 glutamic acid Drugs 0.000 claims description 7
- WPFGFHJALYCVMO-UHFFFAOYSA-L rubidium carbonate Chemical compound [Rb+].[Rb+].[O-]C([O-])=O WPFGFHJALYCVMO-UHFFFAOYSA-L 0.000 claims description 7
- 229910000026 rubidium carbonate Inorganic materials 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000000634 powder X-ray diffraction Methods 0.000 claims description 4
- 238000002834 transmittance Methods 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 2
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims description 2
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 2
- 229910000288 alkali metal carbonate Inorganic materials 0.000 claims description 2
- 150000008041 alkali metal carbonates Chemical class 0.000 claims description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 2
- 229940024606 amino acid Drugs 0.000 claims description 2
- 150000001413 amino acids Chemical class 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- 239000001099 ammonium carbonate Substances 0.000 claims description 2
- 150000003863 ammonium salts Chemical class 0.000 claims description 2
- 238000004891 communication Methods 0.000 claims description 2
- 239000003814 drug Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 150000004767 nitrides Chemical class 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 239000004065 semiconductor Substances 0.000 claims description 2
- 235000016804 zinc Nutrition 0.000 claims description 2
- 239000004246 zinc acetate Substances 0.000 claims description 2
- 239000011667 zinc carbonate Substances 0.000 claims description 2
- 235000004416 zinc carbonate Nutrition 0.000 claims description 2
- 229910000010 zinc carbonate Inorganic materials 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- SRWMQSFFRFWREA-UHFFFAOYSA-M zinc formate Chemical group [Zn+2].[O-]C=O SRWMQSFFRFWREA-UHFFFAOYSA-M 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 235000014692 zinc oxide Nutrition 0.000 claims description 2
- 230000005693 optoelectronics Effects 0.000 claims 1
- 230000005540 biological transmission Effects 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 230000007423 decrease Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000009022 nonlinear effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000411 transmission spectrum Methods 0.000 description 1
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Abstract
The invention belongs to the technical field of inorganic nonlinear optical materials, and relates to a zinc ammonium carbonate nonlinear optical crystal, and a preparation method and application thereof. The chemical formula of the crystal is Zn (NH) 3 )CO 3 Belongs to the orthorhombic system, and has a space group Pna2 1 The unit cell parameter is
α＝β＝γ＝90°，
And (3) growing a large-size zinc carbonate ammonia nonlinear optical crystal by adopting a solvothermal method. A powder of the crystalThe double frequency intensity is about KH 2 PO 4 (KDP) is 1.5 times of that of the (KDP), the ultraviolet light transmission range is wide, and the ultraviolet cut-off side length is 204nm. The zinc carbonate ammonia nonlinear optical crystal can realize frequency doubling laser output in an ultraviolet region, has good stability, is not deliquesced, is easy to grow large-size high-quality single crystals, and can be used as the ultraviolet nonlinear optical crystal.
Description
Technical Field
The invention belongs to the technical field of inorganic nonlinear optical materials, and relates to a zinc ammonium carbonate nonlinear optical crystal, a preparation method thereof and application thereof as a nonlinear optical device.
Background
The nonlinear optical material can obtain laser with different wavelengths by utilizing nonlinear effects such as frequency doubling, difference frequency and the like generated when the laser is transmitted in a medium, and has important application in different fields such as lasers, medical treatment, national defense and military and the like. Inorganic nonlinear optical materials are becoming mature in application and industrialization due to their excellent comprehensive properties, for example: KH (natural Kill) 2 PO 4 (KDP)、KTiOPO 4 (KTP)、β-BaB 2 O 4 (BBO)、LiB 3 O 5 (LBO), etc., and many new nonlinear optical crystal materials are continuously reported. Ultraviolet laser light sources have been widely paid attention to and studied because they have irreplaceable roles in the fields of scientific research, industrial manufacturing, and the like. The nonlinear optical crystal material is a necessary device for realizing ultraviolet laser conversion and output, so that the nonlinear optical crystal material suitable for the ultraviolet region becomes a hot spot of research in the field. However, most ultraviolet nonlinear optical crystal materials have difficulty in simultaneously realizing practical conditions such as strong frequency doubling, wide ultraviolet transmittance, phase matching, and bulk growth.
Therefore, the search for new nonlinear optical crystal materials which can be used for the output of ultraviolet laser has important significance and value.
Disclosure of Invention
In order to solve the technical problems, the invention provides a zinc ammonium carbonate crystal, and the chemical formula of the crystal is Zn (NH) 3 )CO 3 Belongs to the orthorhombic system, and has a space group Pna2 1 (ii) a The size of the zinc ammonium carbonate crystals is centimeter-level.
The centimeter level is at least one dimension (e.g., length, width, height) up to the centimeter level, such as at least 1cm in length.
According to the invention, the zinc ammonium carbonate crystals have unit cell parameters of
α＝β＝γ＝90°，
According to the invention, the zinc ammonia carbonate crystals are transparent crystals.
According to the invention, the zinc ammonium carbonate crystals have a morphology substantially as shown in figure 1.
According to the invention, the zinc ammonium carbonate crystal is a nonlinear optical crystal.
According to the invention, the zinc ammonium carbonate crystal can realize phase matching under the irradiation of laser with the wavelength of about 1064 nm.
According to the invention, the double frequency intensity of the zinc ammonium carbonate crystals at a particle size of 150-212 μm is about 1.5 KH 2 PO 4 (KDP)。
According to the invention, the ultraviolet absorption cut-off edge length of the zinc ammonium carbonate crystal is 204nm.
According to the invention, the zinc ammonia carbonate crystals have an X-ray powder diffraction pattern substantially as shown in figure 2.
According to the invention, the zinc ammonia carbonate crystal is a single crystal.
According to the invention, the zinc ammonia carbonate crystals have a single crystal transmission substantially as shown in figure 3.
According to the invention, the zinc ammonium carbonate crystal has a particle size-frequency doubling effect graph basically as shown in figure 4 under 1064nm laser irradiation.
The invention also provides a preparation method of the zinc ammonium carbonate crystal, which comprises the following steps: and mixing a zinc-containing compound, a nitrogen-containing compound and a carbonate compound with a solvent, and carrying out solvothermal reaction to obtain the zinc carbonate ammonia crystal.
According to the invention, the solvothermal reaction is carried out at high temperature and high pressure.
According to the invention, the molar ratio of the zinc-containing compound to the nitrogen-containing compound to the carbonate is (1-8) to (2-6) to (0.05-1).
According to the invention, the molar volume ratio of the zinc-containing compound, the nitrogen-containing compound, the carbonate and the solvent is (1-8) mmol, (2-8) mmol, (0.05-1) mmol, (2-20) mL.
According to the invention, the solvent comprises an organic solvent and/or water; preferably, the solvent is one, two or more of ethanol, methanol, N-Dimethylformamide (DMF), ethylene glycol or water, for example, DMF or a mixture of DMF and water.
According to the invention, the zinc-containing compound is one or a mixture of two or more of zinc oxide, zinc carbonate, zinc chloride and zinc organic acid salt, preferably, the zinc organic acid salt is zinc formate, zinc acetate or zinc acetate dihydrate, such as zinc acetate dihydrate.
According to the invention, the nitrogen-containing compound is one or a mixture of two or more of ammonium salt, ammonia gas, urea, nitride and amino acid, for example, the nitrogen-containing compound is a mixture of urea and L-glutamic acid.
According to the invention, the carbonate compound is one, a mixture of two or more of alkali metal carbonate, alkaline earth metal carbonate or ammonium carbonate, for example the carbonate compound is rubidium carbonate.
According to the invention, the molar ratio of zinc acetate dihydrate, urea, L-glutamic acid and rubidium carbonate is (1-8): (2-6): (0.4-2): (0.05-1), preferably (2-6): (3-5): (0.8-1.5): (0.06-0.08).
According to the invention, the solvent thermal reaction adopts a program temperature control method: firstly heating, then keeping constant temperature and then cooling. For example, the temperature is raised to 130-180 ℃ within 60-180 minutes, the temperature is kept constant for 12-48 hours, and then the temperature is lowered to the room temperature at 1-7 ℃/hour. Preferably, the temperature is raised to 140-160 ℃ within 90-150 minutes, the temperature is kept for 18-30 hours, and then the temperature is lowered to the room temperature at 1-3 ℃/hour.
The invention also provides a nonlinear optical material at least containing the zinc ammonia carbonate crystal.
The invention also provides an application of the zinc ammonium carbonate crystal as a nonlinear optical material.
The invention also provides the application of the zinc ammonium carbonate crystal in the output of ultraviolet frequency doubling laser.
The invention also provides the application of the zinc ammonium carbonate crystal in an all-solid-state laser; for example, the all-solid-state laser is used for laser medicine, laser communication, and semiconductor processing.
The invention also provides the application of the zinc ammonium carbonate crystal in photoelectric devices; for example, the optical device is an optical detector, an optical parametric oscillator, or the like.
Advantageous effects
The invention obtains Zn (NH) with large size for the first time 3 )CO 3 Crystal and use it as nonlinear optical crystal. The crystal has excellent optical performance and wide ultraviolet light transmission range, the ultraviolet cut-off side length is 204nm, the KDP of which the powder frequency doubling strength is about 1.5 times of that of the crystal, and the frequency doubling laser output of an Nd: YAG (1064 nm) laser can be realized. The crystal has the advantages of no deliquescence, high purity, simple growth method, high crystal quality, good mechanical property, capability of being polished, cut and the like, suitability for manufacturing laser frequency conversion devices, and capability of being used for all-solid-state lasers, optical parametric oscillators and the like.
Drawings
FIG. 1 shows a centimeter-sized zinc ammonium zinc carbonate Zn (NH) grown by the present invention 3 )CO 3 A crystal photograph;
FIG. 2 shows zinc ammonium carbonate Zn (NH) according to the invention 3 )CO 3 An X-ray powder diffraction pattern of the crystal;
FIG. 3 shows zinc ammonium carbonate Zn (NH) according to the invention 3 )CO 3 A single crystal transmittance plot of the crystal;
FIG. 4 shows zinc ammonium carbonate Zn (NH) according to the invention 3 )CO 3 The relationship graph of the frequency doubling effect size and the grain size of the crystal under 1064nm laser irradiation.
Detailed Description
The crystal of the present invention, its preparation and use will be described in further detail with reference to specific examples. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
Example 1
Putting 6mmol of zinc acetate dihydrate, 4mmol of urea, 0.68mmol of L-glutamic acid, 0.1mmol of rubidium carbonate, 0.5mL of water and 2.5mL of N, N-Dimethylformamide (DMF) into a 23mL stainless steel hydrothermal reaction kettle with a polytetrafluoroethylene lining, then putting the hydrothermal reaction kettle into a muffle furnace, heating to 150 ℃ for 2 hours, keeping the temperature for 24 hours, and then cooling to room temperature at the cooling rate of 1 ℃/h; after the reaction is finished, washing the product for a plurality of times by using ethanol, and filtering to obtain pure zinc ammonium carbonate Zn (NH) 3 )CO 3 And (4) crystals.
The picture of the crystal is shown in fig. 1, which is a large size crystal, at least up to the centimeter level in length.
The X-ray powder diffraction pattern of the crystal is shown in FIG. 2.
Example 2
Putting 8mmol of zinc acetate dihydrate, 4mmol of urea, 1.5mmol of L-glutamic acid, 0.2mmol of rubidium carbonate and 3mL of DMF into a 23mL stainless steel hydrothermal reaction kettle with a polytetrafluoroethylene lining, then putting the hydrothermal reaction kettle into a muffle furnace, heating to 140 ℃ for 2 hours, keeping the temperature for 24 hours, and then cooling to room temperature at the cooling rate of 1 ℃/h; after the reaction is finished, washing the product for a plurality of times by using ethanol, and filtering to obtain pure zinc ammonium carbonate Zn (NH) 3 )CO 3 And (4) crystals.
Example 3
Referring to FIG. 3, a single crystal transmission spectrum of the crystal of example 1 shows high optical transmittance in the ultraviolet region (200 to 380 nm). Referring to fig. 4, the frequency doubling intensity of the crystal of example 1 under 1064nm laser irradiation continuously decreases with the decrease of the particle size, which shows that the crystal can realize phase matching, and the frequency doubling coefficient is about 1.5 times that of the commercial KDP. The example 2 crystal had the same properties as the example 1 crystal.
Example 4
The crystal obtained in example 1-2 was placed in an all-solid-state laser using an ultraviolet nonlinear optical device, nd: YAG laser emits infrared beam with 1064nm wavelength, which passes through zinc ammonium carbonate Zn (NH) 3 )CO 3 After the crystal is crystallized, a visible light beam with the wavelength of 532nm can be output.
In conclusion, the zinc ammonia carbonate Zn (NH) of the invention 3 )CO 3 The crystal has excellent ultraviolet nonlinear optical performance, can be used as a nonlinear optical material, and can also be used for other optical devices and equipment.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A zinc ammonium carbonate crystal, which is characterized in that the chemical formula of the crystal is Zn (NH) 3 )CO 3 Belongs to the orthorhombic system and has a space group Pna2 1 (ii) a The size of the zinc ammonium carbonate crystal is centimeter level.
2. The zinc ammonia carbonate crystal of claim 1, wherein the zinc ammonia carbonate crystal has a unit cell parameter of
α＝β＝γ＝90°，
Preferably, the zinc ammonium carbonate crystal is a nonlinear optical crystal.
Preferably, the zinc ammonium carbonate crystals have a morphology photograph as shown in fig. 1.
Preferably, the zinc ammonium carbonate crystals are transparent crystals.
3. The zinc ammonium carbonate crystal of claim 1 or 2, wherein the zinc ammonium carbonate crystal is capable of phase matching under laser irradiation at about 1064 nm.
Preferably, the double frequency intensity of the zinc ammonium carbonate crystals at the particle size of 150-212 mu m is 1.5 times KH 2 PO 4 (KDP)。
Preferably, the ultraviolet absorption cut edge length of the zinc ammonium carbonate crystal is 204nm.
Preferably, the zinc ammonium carbonate crystals have an X-ray powder diffraction pattern as shown in figure 2.
Preferably, the zinc ammonia carbonate crystal is a single crystal.
Preferably, the zinc ammonia carbonate crystals have a single crystal transmittance as shown in fig. 3.
Preferably, the zinc ammonium carbonate crystal has a particle size-frequency doubling effect graph shown in fig. 4 under 1064nm laser irradiation.
4. A method for producing the zinc ammonium carbonate crystals as defined in any one of claims 1 to 3, comprising the steps of: and mixing a zinc-containing compound, a nitrogen-containing compound and a carbonate compound with a solvent, and carrying out solvothermal reaction to obtain the zinc carbonate ammonia crystal.
5. The method of claim 4, wherein the molar ratio of the zinc-containing compound to the nitrogen-containing compound to the carbonate is (1-8) to (2-6) to (0.05-1).
Preferably, the molar volume ratio of the zinc-containing compound, the nitrogen-containing compound, the carbonate and the solvent is (1-8) (2-8) (0.05-1) (2-20) mL.
Preferably, the solvothermal reaction is carried out at elevated temperature and pressure.
6. The production method according to claim 4 or 5, wherein the solvent comprises an organic solvent and/or water; preferably, the solvent is one or a mixture of two or more of ethanol, methanol, N-Dimethylformamide (DMF), ethylene glycol or water.
Preferably, the zinc-containing compound is one or a mixture of two or more of zinc oxide, zinc carbonate, zinc chloride and zinc organic acid salt, preferably, the zinc organic acid salt is zinc formate, zinc acetate or zinc acetate dihydrate, such as zinc acetate dihydrate.
Preferably, the nitrogen-containing compound is one or a mixture of two or more of ammonium salt, ammonia gas, urea, nitride and amino acid, for example, the nitrogen-containing compound is a mixture of urea and L-glutamic acid.
Preferably, the carbonate compound is one, a mixture of two or more of an alkali metal carbonate, an alkaline earth metal carbonate or ammonium carbonate, for example the carbonate compound is rubidium carbonate.
7. The production method according to any one of claims 4 to 6, wherein the molar ratio of zinc acetate dihydrate to urea to L-glutamic acid to rubidium carbonate is (1 to 8): (2-6): (0.4-2): (0.05-1);
preferably, the molar ratio of the zinc acetate dihydrate to the urea to the L-glutamic acid to the rubidium carbonate is (2-6): (3-5): (0.8-1.5): (0.06-0.08).
Preferably, the solvothermal reaction employs programmed temperature control: firstly heating, then keeping constant temperature and then cooling. For example, the temperature is raised to 130-180 ℃ within 60-180 minutes, the temperature is kept constant for 12-48 hours, and then the temperature is lowered to the room temperature at 1-7 ℃/hour.
Preferably, the temperature is raised to 140-160 ℃ within 90-150 minutes, the temperature is kept for 18-30 hours, and then the temperature is lowered to the room temperature at 1-3 ℃/hour.
8. A nonlinear optical material comprising at least the zinc ammonium carbonate crystal according to any one of claims 1 to 3.
9. Use of the zinc ammonia carbonate crystals of any one of claims 1 to 3 in an all-solid-state laser; for example, the all-solid-state laser is used for laser medicine, laser communication, and semiconductor processing.
10. Use of the zinc ammonia carbonate crystal according to any one of claims 1 to 3 in an optoelectronic device; such as optical detectors, optical parametric oscillators, etc.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5096860A (en) * | 1990-05-25 | 1992-03-17 | Alcan International Limited | Process for producing unagglomerated single crystals of aluminum nitride |
| CN103031604A (en) * | 2011-09-29 | 2013-04-10 | 中国科学院福建物质结构研究所 | Nonlinear optical crystal rubidium calcium fluorine carbonate |
| RU2490209C1 (en) * | 2012-03-15 | 2013-08-20 | Общество с ограниченной ответственностью "Новохим" | Method of obtaining basic zinc carbonates |
| US20180171505A1 (en) * | 2016-12-15 | 2018-06-21 | Government Of The United States, As Represented By The Secretary Of The Air Force | Heteroepitaxial hydrothermal crystal growth of zinc selenide |
| CN110817930A (en) * | 2019-07-25 | 2020-02-21 | 重庆东群科技有限公司 | Method for producing zinc ammonium carbonate |
-
2021
- 2021-08-23 CN CN202110970905.1A patent/CN115710748A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5096860A (en) * | 1990-05-25 | 1992-03-17 | Alcan International Limited | Process for producing unagglomerated single crystals of aluminum nitride |
| CN103031604A (en) * | 2011-09-29 | 2013-04-10 | 中国科学院福建物质结构研究所 | Nonlinear optical crystal rubidium calcium fluorine carbonate |
| RU2490209C1 (en) * | 2012-03-15 | 2013-08-20 | Общество с ограниченной ответственностью "Новохим" | Method of obtaining basic zinc carbonates |
| US20180171505A1 (en) * | 2016-12-15 | 2018-06-21 | Government Of The United States, As Represented By The Secretary Of The Air Force | Heteroepitaxial hydrothermal crystal growth of zinc selenide |
| CN110817930A (en) * | 2019-07-25 | 2020-02-21 | 重庆东群科技有限公司 | Method for producing zinc ammonium carbonate |
Non-Patent Citations (1)
| Title |
|---|
| FUSHAN WEN, ET AL: ""Solvothermal Synthesis and Characterization of Zn(NH3)CO3 Single Crystal", MATERIALS RESEARCH SOCIETY, vol. 817, 31 December 2004 (2004-12-31), pages 249 - 254 * |
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