CN102627317B - Compound-basic lead nitrate and basic lead nitrate nonlinear optical crystal as well as preparation method and application thereof - Google Patents
Compound-basic lead nitrate and basic lead nitrate nonlinear optical crystal as well as preparation method and application thereof Download PDFInfo
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- CN102627317B CN102627317B CN2012100943567A CN201210094356A CN102627317B CN 102627317 B CN102627317 B CN 102627317B CN 2012100943567 A CN2012100943567 A CN 2012100943567A CN 201210094356 A CN201210094356 A CN 201210094356A CN 102627317 B CN102627317 B CN 102627317B
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Abstract
The present invention relates to a kind of compound basic lead nitrate and basic lead nitrate nonlinear optical crystal and preparation methods and purposes, the compound molecule formula is Pb16 (OH) 16 (NO3) 16, molecular weight is 4579.36, is prepared using hydro-thermal method, product be crystal; Basic lead nitrate nonlinear optical crystal, the molecular formula of the crystal are Pb16 (OH) 16 (NO3) 16, belong to monoclinic system, space group Cc, molecular weight 4579.36, and cell parameter is
β=133.54 ° are prepared using hydro-thermal method; Gained basic lead nitrate nonlinear optical crystal effect is 3 times of KDP crystal, transmission region 318nm to 2500nm. The compound growth process has the advantages that easy to operate, at low cost, toxicity is low, and growth cycle is short, and physico-chemical property is stablized. Basic lead nitrate of the invention is used widely in the device for non-linear optical such as frequency-doubled conversion, optical parametric oscillator.
Description
Technical field
The present invention relates to a kind of compound lead hydroxynitrate and lead hydroxynitrate non-linear optic crystal and preparation method and purposes, belong to domain of inorganic chemistry, also belong to material science and optical field.
Background technology
Non-linear optical effect originates from the interaction of laser and medium.When laser, when having the Propagation of non-zero second order susceptibility, can produce the non-linear optical effects such as frequency multiplication and frequency, difference frequency, optical parameter amplification.Utilize the second order nonlinear optical effect of crystal, can make the device for non-linear optical such as second harmonic generator, frequency converter, optical parametric oscillator, in a lot of fields, as aspects such as laser technology, atmospheric surveillance, national defence, important using value is arranged.Through exploring decades and research, non-linear optical crystal material has been obtained great successes, especially the research of laser frequency conversion crystal is more deep, and the non-linear optic crystal of many excellent performances has obtained widespread use at aspects such as optics, communication, medical treatment, military affairs.Just because of non-linear optical crystal material, so important application prospect is arranged, thus always very active about the research of non-linear optical crystal material both at home and abroad.However, still there are many deficiencies in the over-all properties of non-linear optic crystal, finds and studies the novel nonlinear optical crystal material and remain when previous very important work.
Inorganic Nonlinear Optical Materials occupies dominant position in the practical research of second-order non-linear optical materials.According to transmission region and the scope of application, the inorganic nonlinear optical crystal material can be divided into ultraviolet region nonlinear optical material, visible region nonlinear optical material and infrared light district nonlinear optical material.
For a long time, find the ultraviolet nonlinear optical material with advantageous property is the focus that domestic and international scientist pays close attention to always.The frequency inverted crystal of research ultraviolet band the earliest is potassium pentaborate (KB
5O
84H
2O) crystal, although its wave band that sees through reaches vacuum ultraviolet (VUV), because of its Clock Multiplier Factor very little (be only ADP crystal 1/10), so be very limited on applying.To the eighties, scientists has been found a series of ultraviolet non-linear optic crystals with premium properties in succession from late 1970s, as BBO (beta-barium metaborate), LBO (lithium tetraborate), KBBF (fluoroboric acid beryllium potassium) etc.Although the crystal technique of these materials reaches its maturity, but still exist obvious weak point: deliquescence as easy as crystal, growth cycle are long, the layer growth habit seriously and expensive etc.Therefore, find new non-linear optical crystal material and remain a very important job.
In laser technology, directly utilize the obtainable laser wavelength of laser crystals institute limited, from the ultraviolet to the infrared spectral region, remained sky white wave section.Use non-linear optic crystal, by non-linear optical effects such as frequency multiplication, mixing, optical parametric oscillations, limited optical maser wavelength can be converted to the laser of new wave band.Utilize this technology can fill up the blank spectral region of all kinds of Laser Devices Emission Lasers wavelength, laser apparatus is more widely used.The all-solid state laser system can produce near-infrared laser by solid statelaser and through non-linear optic crystal, carry out frequency inverted again and realize, at laser technology field, huge application prospect and economic worth are arranged.
It is wider that problem to be solved by this invention is to provide a kind of transmission region, nonlinear second-order optical susceptibility is larger, can realize phase matched, easily preparation and stability mineral compound lead hydroxynitrate powder and lead hydroxynitrate non-linear optic crystal and preparation method and purposes preferably.
Summary of the invention
The object of the invention is to, a kind of compound lead hydroxynitrate is provided, this compound molecule formula is Pb
16(OH)
16(NO
3)
16, molecular weight is 4579.36, adopts the hydrothermal method preparation, product be crystal.
Another object of the present invention is to provide a kind of lead hydroxynitrate non-linear optic crystal, and the molecular formula of this crystal is Pb
16(OH)
16(NO
3)
16, belonging to oblique system, spacer is Cc, and molecular weight is 4579.36, and cell parameter is
β=133.54 °, adopt the hydrothermal method preparation.
Another purpose of the present invention is to provide the performance analysis of lead hydroxynitrate non-linear optic crystal;
A further object of the present invention is to provide the purposes of lead hydroxynitrate non-linear optic crystal.
A kind of compound lead hydroxynitrate of the present invention, this compound molecule formula is Pb
16(OH)
16(NO
3)
16, molecular weight is 4579.36, adopts the hydrothermal method preparation, and products therefrom is directly crystal, and concrete operations follow these steps to carry out:
A, by Pb (NO
3)
2Join volume and be in the polytetrafluoroethyllining lining of autoclave of 25-250mL, then add deionized water 5-200mL, it is fully mixed, adding LiOH, KOH or NaOH to regulate pH value scope is 3-10;
B, mixing solutions in step a is transferred in autoclave, be placed in thermostat container, rise to 120-200 ℃, constant temperature 1-15 days with the temperature rise rate of temperature 20-60 ℃/h, with the rate of temperature fall of temperature 4-50 ℃/h or naturally cool to room temperature, obtain containing the solution of crystal again;
C, step b is contained to the solution filter of crystal, water and concentration are the alternately washing of 25% ethanol, can obtain the crystal of transparent compound lead hydroxynitrate.
A kind of lead hydroxynitrate non-linear optic crystal, the molecular formula of this crystal are Pb
16(OH)
16(NO
3)
16, belonging to oblique system, spacer is Cc, and molecular weight is 4579.36, and cell parameter is
β=133.54 °.
The preparation method of described lead hydroxynitrate non-linear optic crystal, adopt hydrothermal method to prepare crystal, and concrete operations follow these steps to carry out:
A, by Pb (NO
3)
2Join volume and be in the polytetrafluoroethyllining lining of autoclave of 10-250mL, then add deionized water 5-200mL, it is fully mixed, adding LiOH, KOH or NaOH to regulate pH value scope is 3-10;
B, mixing solutions in step a is transferred in autoclave, be placed in thermostat container, rise to 120-200 ℃, constant temperature 1-15 days with the temperature rise rate of temperature 20-60 ℃/h, with the rate of temperature fall of temperature 4-50 ℃/h or naturally cool to room temperature, obtain containing the solution of crystal again;
C, step b is contained to the solution filter of crystal, water and concentration are the alternately washing of 25% ethanol, can obtain transparent compound lead hydroxynitrate crystal, again through the frequency multiplication test in conventional nonlinear optics test, its frequency-doubled effect is 3 times of KDP, and can realize 1 type phase matched, namely be defined as the lead hydroxynitrate non-linear optic crystal.
Described method mol ratio of Pb2+ and OH-in building-up process is 1: 0.05-5.
The purposes of described lead hydroxynitrate non-linear optic crystal, described lead hydroxynitrate non-linear optic crystal is for the preparation of frequency multiplication producer, upper or lower frequency transmodulator or optical parametric oscillator.
Compound lead hydroxynitrate crystal of the present invention, both still have higher seeing through in the 318-2500nm scope of UV, visible light zone, and non-linear optical effect is about 3 times of KDP, and spacer is Cc, and this crystal preparation is simple, and growth cycle is short.
The present invention's method used is that hydrothermal method obtains compound lead hydroxynitrate crystal, again the compound lead hydroxynitrate is tested through the frequency multiplication in conventional nonlinear optics test, its frequency-doubled effect is 3 times of KDP, and can realize 1 type phase matched, namely be defined as the lead hydroxynitrate nonlinear optical material.
Lead hydroxynitrate nonlinear optical material of the present invention, adopt hydrothermal method to prepare compound by following chemical equation:
(1)Pb(NO
3)
2+OH
-+H
2O→Pb
16(OH)
16(NO
3)
16。
Raw of the present invention adopts commercially available reagent, by method of the present invention, have simple to operate, fast growth, growth cycle is short, low cost and other advantages.
Lead hydroxynitrate nonlinear optical material prepared by the present invention is as preparing device for non-linear optical, comprise and make frequency multiplication producer, upper or lower frequency transmodulator and optical parametric oscillator, described nonlinear device with the making of lead hydroxynitrate non-linear optic crystal comprises will see through the coherent light that a branch of at least frequency of a branch of at least incident fundamental wave generation be different from incident light.
Described lead hydroxynitrate nonlinear optical material to the optics working accuracy without particular requirement.
The accompanying drawing explanation
Fig. 1 is Pb
16(OH)
16(NO
3)
16X-ray diffracting spectrum.
Fig. 2 is Pb
16(OH)
16(NO
3)
16See through collection of illustrative plates.
Fig. 3 is the fundamental diagram of the device for non-linear optical made of the present invention, comprising (1), it is laser apparatus, (2) be convex lens, (3) be the lead hydroxynitrate nonlinear optical material, (4) be beam splitting prism, (5) be filter plate, ω equals incident light frequency or incident light frequency 2 times for the refraction light frequency.
Embodiment
The present invention is described in detail below in conjunction with drawings and Examples:
Embodiment 1:
With chemical equation Pb (NO
3)
2+ OH
-+ H
2O → Pb
16(OH)
16(NO
3)
16Preparation Pb
16(OH)
16(NO
3)
16Crystal:
A, by Pb (NO
3)
2Join volume and be in the polytetrafluoroethyllining lining of autoclave of 25mL, then add deionized water 10mL, it is fully mixed, add LiOH to regulate pH=3, wherein Pb
2+And OH
-Mol ratio be 1: 0.05;
B, mixing solutions in step b is packed in autoclave, be placed in thermostat container, rise to 200 ℃ with the temperature rise rate of 20 ℃/h of temperature, constant temperature 3 days, then be cooled to room temperature with the rate of temperature fall of 4 ℃/h of temperature, obtain containing the solution of crystal;
C, open autoclave, the solution filter that will contain crystal, water and concentration are the alternately washing of 25% ethanol, can obtain transparent compound lead hydroxynitrate monocrystalline, again through the frequency multiplication test in conventional nonlinear optics test, its frequency-doubled effect is 3 times of KDP, and can realize 1 type phase matched, namely is defined as the lead hydroxynitrate non-linear optic crystal.
Embodiment 2:
With chemical equation Pb (NO
3)
2+ OH
-+ H
2O → Pb
16(OH)
16(NO
3)
16Preparation Pb
16(OH)
16(NO
3)
16Crystal:
A, by Pb (NO
3)
2Join volume and be in the polytetrafluoroethyllining lining of autoclave of 50mL, then add deionized water 25mL, it is fully mixed, add NaOH to regulate pH=6, wherein Pb
2+And OH
-Mol ratio be 1: 0.5;
B, mixing solutions in step b is packed in autoclave, be placed in thermostat container, rise to 180 ℃ with the temperature rise rate of temperature 60 C/h, constant temperature 1 day, naturally cool to room temperature;
C, open autoclave, the solution filter that will contain crystal, water and concentration are the alternately washing of 25% ethanol, can obtain transparent compound lead hydroxynitrate monocrystalline, again through the frequency multiplication test in conventional nonlinear optics test, its frequency-doubled effect is 3 times of KDP, and can realize 1 type phase matched, namely is defined as the lead hydroxynitrate non-linear optic crystal.
Embodiment 3:
With chemical equation Pb (NO
3)
2+ OH
-+ H
2O → Pb
16(OH)
16(NO
3)
16Preparation Pb
16(OH)
16(NO
3)
16Crystal:
A, by Pb (NO
3)
2Join volume and be in the polytetrafluoroethyllining lining of autoclave of 150mL, then add deionized water 100mL, it is fully mixed, add KOH to regulate pH=7, wherein Pb
2+And OH
-Mol ratio be 1: 1.0;
B, mixing solutions in step b is packed in autoclave, be placed in thermostat container, rise to 150 ℃ with the temperature rise rate of temperature 50 C/h, constant temperature 10 days, then be cooled to room temperature with the rate of temperature fall of 10 ℃/h of temperature, obtain containing the solution of crystal;
C, open autoclave, the solution filter that will contain crystal, water and concentration are the alternately washing of 25% ethanol, can obtain transparent compound lead hydroxynitrate monocrystalline, again through the frequency multiplication test in conventional nonlinear optics test, its frequency-doubled effect is 3 times of KDP, and can realize 1 type phase matched, namely is defined as the lead hydroxynitrate non-linear optic crystal.
Embodiment 4
With chemical equation Pb (NO
3)
2+ OH
-+ H
2O → Pb
16(OH)
16(NO
3)
16Preparation Pb
16(OH)
16(NO
3)
16Crystal:
A, by Pb (NO
3)
2Join volume and be in the polytetrafluoroethyllining lining of autoclave of 100mL, then add deionized water 50mL, it is fully mixed, add KOH to regulate pH value 5, wherein Pb
2+And OH
-Mol ratio be 1: 3;
B, mixing solutions is transferred in autoclave, is placed in thermostat container, rise to 120 ℃ with the temperature rise rate of 35 ℃/h of temperature, constant temperature 5 days, then be cooled to room temperature with the rate of temperature fall of 30 ℃/h of temperature, obtain containing the solution of crystal;
C, open autoclave, the solution filter that will contain crystal, water and concentration are the alternately washing of 25% ethanol, can obtain transparent compound lead hydroxynitrate monocrystalline, again through the frequency multiplication test in conventional nonlinear optics test, its frequency-doubled effect is 3 times of KDP, and can realize 1 type phase matched, namely is defined as the lead hydroxynitrate non-linear optic crystal.
With chemical equation Pb (NO
3)
2+ OH
-+ H
2O → Pb
16(OH)
16(NO
3)
16Preparation Pb
16(OH)
16(NO
3)
16Crystal:
A, by Pb (NO
3)
2Join volume and be in the polytetrafluoroethyllining lining of autoclave of 250mL, then add deionized water 200mL, it is fully mixed, add LiOH to regulate pH value 10, wherein Pb
2+And OH
-Mol ratio be 1: 5;
B, mixing solutions is transferred in autoclave, is placed in thermostat container, rise to 200 ℃ with the temperature rise rate of temperature 60 C/h, constant temperature 15 days, then be cooled to room temperature with the rate of temperature fall of temperature 50 C/h, obtain containing the solution of crystal;
C, open autoclave, the solution filter that will contain crystal, water and concentration are the alternately washing of 25% ethanol, can obtain transparent compound lead hydroxynitrate monocrystalline, again through the frequency multiplication test in conventional nonlinear optics test, its frequency-doubled effect is 3 times of KDP, and can realize 1 type phase matched, namely is defined as the lead hydroxynitrate non-linear optic crystal.
Described method is in building-up process.
Embodiment 6
With chemical equation Pb (NO
3)
2+ OH
-+ H
2O → Pb
16(OH)
16(NO
3)
16Preparation Pb
16(OH)
16(NO
3)
16Crystal:
A, by Pb (NO
3)
2Join volume and be in the polytetrafluoroethyllining lining of autoclave of 200mL, then add deionized water 160mL, it is fully mixed, add NaOH to regulate pH value 8, wherein Pb
2+And OH
-Mol ratio be 1: 3;
B, mixing solutions is transferred in autoclave, is placed in thermostat container, rise to 190 ℃ with the temperature rise rate of temperature 45 C/h, constant temperature 12 days, then be cooled to room temperature with the rate of temperature fall of 40 ℃/h of temperature, obtain containing the solution of crystal;
C, step b is contained to the solution filter of crystal, water and concentration are the alternately washing of 25% ethanol, can obtain transparent compound lead hydroxynitrate monocrystalline, again through the frequency multiplication test in conventional nonlinear optics test, its frequency-doubled effect is 3 times of KDP, and can realize 1 type phase matched, namely be defined as the lead hydroxynitrate non-linear optic crystal.
Embodiment 7:
By the compound of gained in embodiment 1-6, by shown in accompanying drawing 3, being placed on 3 position, at room temperature, make light source with the 1064nm output of adjusting Q Nd:YAG laser apparatus, observe obvious 532nm frequency doubling green light output, output intensity is about 3 times of equal conditions KDP.
Figure 3 shows that, by adjusting Q Nd:YAG laser apparatus 1 to send wavelength, be that the infrared beam of 1064nm is injected the lead hydroxynitrate non-linear optic crystal through convex lens 2, producing wavelength is the green frequency doubled light of 532nm, it is the infrared light of 1064nm and the green glow of 532nm that outgoing beam 4 contains wavelength, after filter plate 5 eliminations, obtains the frequency doubled light that wavelength is 532nm.
Claims (4)
1. a compound lead hydroxynitrate, is characterized in that this compound molecule formula is Pb
16(OH)
16(NO
3)
16, molecular weight is 4579.36, adopts the hydrothermal method preparation, and products therefrom is directly crystal, and concrete operations follow these steps to carry out:
A, by Pb (NO
3)
2Join volume and be in the polytetrafluoroethyllining lining of autoclave of 25-250mL, then add deionized water 5-200mL, it is fully mixed, adding LiOH, KOH or NaOH to regulate pH value scope is 3-10, wherein Pb
2+And OH
-Mol ratio be 1: 0.05-5;
B, mixing solutions in step a is transferred in autoclave, be placed in thermostat container, rise to 120-200 ℃, constant temperature 1-15 days with the temperature rise rate of temperature 20-60 ℃/h, with the rate of temperature fall of temperature 4-50 ℃/h or naturally cool to room temperature, obtain containing the solution of crystal again;
C, step b is contained to the solution filter of crystal, water and concentration are the alternately washing of 25% ethanol, can obtain the crystal of transparent compound lead hydroxynitrate.
2. lead hydroxynitrate non-linear optic crystal, the molecular formula that it is characterized in that this crystal is Pb
16(OH)
16(NO
3)
16, belonging to oblique system, spacer is Cc, and molecular weight is 4579.36, and cell parameter is
β=133.54 °.
3. the preparation method of lead hydroxynitrate non-linear optic crystal according to claim 2, is characterized in that adopting hydrothermal method to prepare crystal, and concrete operations follow these steps to carry out:
A, by Pb (NO
3)
2Join volume and be in the polytetrafluoroethyllining lining of autoclave of 10-250mL, then add deionized water 5-200mL, it is fully mixed, adding LiOH, KOH or NaOH to regulate pH value scope is 3-10, wherein Pb
2+And OH
-Mol ratio be 1: 0.05-5;
B, mixing solutions in step a is transferred in autoclave, is placed in thermostat container, rise to 120-200 ℃ with the temperature rise rate of temperature 20-60 ℃/h, constant temperature 1-15 days, then with the rate of temperature fall of temperature 4-50 ℃/h or naturally cool to room temperature;
C, will contain the solution filter of crystal, water and concentration are that 25% ethanol alternately washs and can obtain transparent compound lead hydroxynitrate crystal, again through the frequency multiplication test in conventional nonlinear optics test, its frequency-doubled effect is 3 times of KDP, and can realize 1 type phase matched, namely be defined as the lead hydroxynitrate non-linear optic crystal.
4. the purposes of lead hydroxynitrate non-linear optic crystal according to claim 2, is characterized in that described lead hydroxynitrate non-linear optic crystal is for the preparation of frequency multiplication producer, upper or lower frequency transmodulator or optical parametric oscillator.
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