CN104577697B - Perovskite optical pulse modulation device and its preparation technology and application - Google Patents
Perovskite optical pulse modulation device and its preparation technology and application Download PDFInfo
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Abstract
The present invention relates to perovskite optical pulse modulation device and its preparation technology and application.Perovskite optical pulse modulation device includes quartz glass substrate and prepares the perovskite material film on substrate.The one side for not being loaded with perovskite material is plated with the deielectric-coating high to 1.05 1.1 μm or not plated film.Perovskite optical pulse modulation device is used in laser, have the one of perovskite thin film facing in laser cavity, another side is towards outside laser cavity, pump light is by, again by this perovskite optical pulse device, the front cavity mirror being placed in before gain medium forms resonator as input mirror with the Effect of Back-Cavity Mirror being placed in behind perovskite optical pulse device after gain medium；Can be used for the regulation being lost to the laser of infrared band.Impulse modulation device of the invention makes simple, low cost, is conducive to industrialization production.
Description
Technical field
The present invention relates to a kind of Organic-inorganic composite perovskite optical pulse modulation device and its preparation technology with and should
With belonging to laser device technical field.
Background technology
Organic metal halide perovskite crystal is a kind of compound semiconductor, because there is solar spectrum high to absorb for it
Coefficient, compared with common solar energy film layer, can be made it is thinner, as prepare planar heterojunction solar cell it is ideal
Material.Most representational in organic metal halide perovskite crystal is methylamino lead iodide (CH3NH3PbI3)。
Methylamino lead iodide (CH3NH3PbI3) belong to perovskite structure (ABX3) material, the crystal knot with stabilization
Structure, unique electromagnetic performance and redox very high, hydrogenolysis, isomerization, light absorptive, electro-catalysis isoreactivity, are a kind of new
The functional material of type, and the transformation efficiency of Yin Qigao, low production cost and simple manufacture craft turn into nearly 2 years whole world
The study hotspot of area of solar cell, is expected to turn into the main force of following clean energy resource.CN104084699A provides a kind of flexible
The method that uniform organic-inorganic perovskite crystal film is prepared on substrate, including：Soaked in the flexible substrate for be coated with conductive film
Apply or be spin-coated on and organic-inorganic perovskite thin film is prepared on conductive film, less than 100 DEG C low temperature preannealings；Use ultra-short pulse laser
The surface of the organic-inorganic perovskite thin film is focused on by object lens, the perovskite material of focal point occurs fusing regrowth,
Form uniform film.For preparing planar heterojunction solar cell.
CN104250723A discloses a kind of based on metallic lead simple substance membrane original position large area control synthesis Ca-Ti ore type
CH3NH3PbI3The chemical method of thin-film material, sputters lead simple substance membrane, then by the base with lead simple substance membrane in substrate surface
In the organic solution containing iodine and iodate methylamine, isothermal reaction is in situ to be obtained CH to bottom material horizontal immersion3NH3PbI3It is thin
Membrane material；Gained CH3NH3PbI3Film purity is high, film surface crystal uniform, can be used for third generation solar cell.
Optical pulse modulation device is important device in laser, and passive modulation device has small volume, structure letter
Singly, it is easy to the advantage such as integrated, is the first-selection of pulse optical device.The principle of passive modulation mainly uses the non-linear of material can
Saturated absorption is that, when high light is irradiated, the electrons in its valence band all transit to conduction band, are formed completely in conduction band
Distribution, so as to will not be absorbed to the light again, that is, keeps transmitance higher to the light.Conventional semiconductor saturable
Absorber mainly has two kinds of devices of saturable absorbing mirror (SESAM) and GaAs (GaAs), and both device making technics compare
Complexity, production cost is higher, and energy consumption is larger.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of inexpensive perovskite optical pulse modulation device and its preparation
Technique.
The present invention also provides application of the perovskite optical pulse modulation device in pulse laser.
Technical scheme is as follows：
A kind of perovskite optical pulse modulation device, including：
One quartz glass substrate, and the substrate top surface, thickness are deposited on for 300-600nm perovskite thin films；
Optionally, the deielectric-coating for being conducive to laser generation is plated with the substrate back；
When the device is used for pulse laser, deposition has the one of perovskite thin film facing in laser cavity, another side direction
Outside laser cavity, realize being modulated the laser of 1.05-1.1 μm of infrared band.
It is methylamino lead iodide (CH according to currently preferred, described perovskite thin film3NH3PbI3, organic-inorganic
Perovskite) film.Particularly preferably, perovskite thin film thickness is 400-500nm.The perovskite thin film uses half vapor phase method or liquid
Phase method makes PbI2With CH3NH3I reaction generations CH3NH3PbI3Quartz glass substrate top surface is deposited on to be made；Can be by existing half gas
It is prepared by phase method or liquid phase method deposition technique.
It is 0.5mm-2mm according to currently preferred, described quartz glass substrate thickness；Particularly preferred quartz glass lining
Base thickness degree is 2mm.
Perovskite optical pulse modulation device of the present invention, can be processed into arbitrary shape, and preferred shape is rectangle
Or it is circular.Device size can be selected as needed.Preferred perovskite thin film thickness is 400-500nm.
The deielectric-coating for being plated in quartz glass substrate back of the present invention can change oscillation light according to requirement when applying
Reflectivity, the shortcoming that the factor such as reflectivity is immutable when overcoming not plated film is brought is conducive to the design of pulse laser.It is preferred that
, it is plated with the deielectric-coating to 1.05-1.1 μm high in quartz glass substrate back.
A kind of preparation method of inexpensive perovskite optical pulse modulation device, including：
- using quartz glass plate as substrate, make PbI with half vapour deposition process or liquid phase deposition2With CH3NH3I reaction lifes
Into CH3NH3PbI3It is deposited on quartz glass substrate and is made perovskite thin film,
- optional, in another plated surface of substrate with the deielectric-coating to 1.05-1.1 μm high or not plated film,
Form perovskite optical pulse modulation device.
The perovskite thin film thickness is 300-600nm, and particularly preferred thickness is 400-500nm；Described quartz glass
Substrate thickness is 0.5mm-2mm；Particularly preferred substrate thickness is 2mm.
Preferably, perovskite thin film is prepared on quartz glass substrate with half vapour deposition process, step is as follows：
(1) spontaneously dried after being cleaned by ultrasonic to quartz glass plate；
(2) spin-coating method is used by PbI2Anhydrous DMF solution be coated on quartz glass plate, formed PbI2
Film, dries；
(3) by CH3NH3I powder is uniformly plated in and is loaded with PbI2Around the quartz plate of film, culture dish is covered, and be heated to
150 DEG C are kept for 30-35 minutes, obtain CH3NH3PbI3Film；CH3NH3I and PbI2Mol ratio 1-1.2:1；
(4) after cooling down, by CH3NH3PbI3Film is rinsed with isopropanol, is dried.
Preferably, perovskite thin film is prepared on quartz glass substrate with liquid phase deposition, step is as follows：
(1) spontaneously dried after being cleaned by ultrasonic to quartz glass plate；
(2) using spin-coating method by PbI2Anhydrous DMF solution be coated on quartz glass plate, formed
PbI2 films；
(3) after drying, PbI will be loaded with2The quartz glass plate of film is immersed in CH3NH35-8 points in the aqueous isopropanol of I
Clock, obtains CH3NH3PbI3Film；The PbI2With CH3NH3The mol ratio 1 of I：1-1.2；
(4) by CH3NH3PbI3Thin-film material is rinsed with isopropanol, and the optics arteries and veins described in the present embodiment is can obtain after drying
Modulated device.
Equal can be prepared by existing half vapor phase method or liquid phase method deposition technique with what is do not limited in detail in up to step.
According to the present invention, the application of the perovskite optical pulse modulation device, as pulse tuning Q device or mode-locking device
For in laser.
In laser utilization, by the way of end face or profile pump, pump light is input to gain medium
In, the pump light after gain medium by, again by perovskite impulse modulation device of the invention, being placed in laser gain
Front cavity mirror before medium forms resonator with the outgoing mirror being placed in behind perovskite impulse modulation device.Described front and rear hysteroscope
Plating is conducive to the deielectric-coating of laser generation.
Described gain medium can select semiconductor, laser crystal, laser ceramics or laser glass etc. to own
The medium of laser gain can be produced, cylinder or cuboid is processed into, its end face is plated with the absorption that is conducive to pump light and swashs
The deielectric-coating of light generation, it is also possible to simply finishing polish not plated film.Preferably, described gain medium is Nd:YAG or Nd:
YVO4Crystal, Nd3+Ion concentration is 0.01-0.5at.%.
Described pumping source is the light source that semiconductor laser diode (LD) or xenon lamp etc. can provide pump energy.
The deielectric-coating of the input mirror of described front cavity mirror can directly be plated on gain medium apart from perovskite farther out
On face, another face can be plated with the deielectric-coating for being conducive to laser generation and Pumping light absorption, it is also possible to not plated film.Effect of Back-Cavity Mirror
The deielectric-coating of outgoing mirror can directly be plated on gain medium on perovskite face farther out, and another face can be plated with
Beneficial to the deielectric-coating of laser generation, it is also possible to not plated film.
Described front cavity mirror is the plano lens of 10-100mm from a radius, and minute surface is plated with to 1.05-1.1 μm of high reflection
Deielectric-coating, the distance between front cavity mirror and modulation element are 0.05-8cm, preferably 5-8cm.
Described Effect of Back-Cavity Mirror is the plano-concave mirror of 10-100mm from a radius, and concave surface is plated with saturating to 1.05-1.1 μm of part
The deielectric-coating crossed, preferably through 3-10%；The distance between Effect of Back-Cavity Mirror and modulation element are 0.05-8cm, preferably 0.05-
1cm.Further preferably, front cavity mirror and the distance of Effect of Back-Cavity Mirror are 3-10cm.
A kind of pulse laser, including the above-mentioned perovskite impulse modulation device of the present invention, deposition have perovskite thin film
One facing in laser cavity, and another side is realized being modulated the laser of 1.05-1.1 μm of infrared band towards outside laser cavity.
The perovskite optical pulse modulation device that the present invention is provided can be used to the laser for producing infrared band is lost
Regulation, include semiconductor, the laser that laser crystal, laser ceramics and laser glass are produced.It is capable of achieving to LD or xenon lamp
The modulation of pumping laser.The present invention takes full advantage of the optics arteries and veins that the saturable absorption performance of organic-inorganic perovskite thin film makes
Modulated device, raw material is made using cheap lead, halogen and amine salt, and substrate does raw material using quartz glass, and these raw materials are on ground
Reserves very abundant on ball, with low cost, purchase is easy.Perovskite thin film technological operation letter is prepared on quartz glass substrate
It is single.Perovskite optical pulse modulation device shape of the invention and size depend on the size and dimension of substrate, can be according to not
Same demand, is processed into different shape and size is applied, and is easy to large-scale production.
Brief description of the drawings
Fig. 1 is the pictorial diagram of perovskite optical pulse modulation device of the invention.
Fig. 2 is the structural representation of perovskite optical pulse modulation device of the invention.Wherein, 1. perovskite thin film, 2.
Quartz glass substrate, 15. media coatings.
Fig. 3 be LD end pumpings, using perovskite optical pulse modulation device of the invention as the laser device of Q switched element
Structural representation, wherein, 3. pumping source, 4. fiber coupling system, 5. focusing system, 6. front cavity mirror, 7. Effect of Back-Cavity Mirror, 8. laser increase
Beneficial medium, 9. perovskite impulse modulation device.
Fig. 4 be xenon lamp profile pump, using perovskite optical pulse modulation device of the invention as the laser of Q switched element
Part structural representation, wherein, 10. front cavity mirror, 11. xenon lamps, 12. gain mediums, 13 perovskite impulse modulation devices, 14.
Effect of Back-Cavity Mirror.
Fig. 5 is the 1.05-1.1 μm of infrared waves that the pulse laser that perovskite impulse modulation device of the invention is made is produced
The laser pulse sequence of section.Abscissa：Time (μ s), ordinate：Intensity (arbitrary unit).
Specific embodiment
The present invention is described further with reference to embodiment, but not limited to this.
Perovskite optical pulse modulation device prepared by embodiment 1, half vapor phase method
Preferred dimension is the JGS1 type optical quartz glass disks of 25*1mm as substrate.Using half vapor phase method in substrate one
Side surface prepares perovskite thin film material, and film thickness is 350-450nm.Step is as follows：
(1) spontaneously dried after being cleaned by ultrasonic to quartz glass plate；
(2) it is the PbI of 400mg/mL by concentration by the technological parameter of 2000 revs/min, 30s to use spin-coating method2Anhydrous N,
Dinethylformamide solution is coated on quartz glass plate, forms PbI2Film, dries；
(3) by CH3NH3I powder is uniformly layered on and is loaded with PbI2Around the quartz plate of film, culture dish is covered, and be heated to
150 DEG C are kept for 30-35 minutes, obtain CH3NH3PbI3Film；CH3NH3I and PbI2Consumption mol ratio be 1:1；
(4) after cooling down, by CH3NH3PbI3Film is rinsed with isopropanol, is dried, and film thickness is 350-450nm.
(5) quartz glass plate opposite side plated surface is with the deielectric-coating to 1.05-1.1 μm high.
The perovskite optical pulse modulation device material object photo of preparation is as shown in Figure 1a.
Perovskite optical pulse modulation device prepared by embodiment 2, liquid phase method
Preferred dimension is the JGS1 type optical quartz glass disks of 25*1mm as substrate.Using liquid phase method in substrate side
Surface prepares perovskite thin film material, and film thickness is 400-500nm.Step is as follows：
(1) spontaneously dried after being cleaned by ultrasonic to quartz glass plate；
(2) 6500 revs/min, the technological parameter of 90s are pressed using spin-coating method, is the PbI of 463mg/mL by concentration2Anhydrous N,
Dinethylformamide solution is coated on quartz glass plate, forms PbI2Film；
(3) after drying, PbI will be loaded with2The quartz glass plate of film is immersed in the CH that concentration is 10mg/mL3NH3The isopropyl of I
5-8 minutes in alcoholic solution, CH is obtained3NH3PbI3Film；CH3NH3I and PbI2Consumption mol ratio be 1:1；
(4) by CH3NH3PbI3Thin-film material is rinsed with isopropanol, is dried, and film thickness is 400-500nm.
(5) quartz glass plate opposite side plated surface is with the deielectric-coating to 1.05-1.1 μm high.
The perovskite optical pulse modulation device material object photo of preparation is as shown in Figure 1 b.
Embodiment 3, perovskite optical pulse modulation device as Q switched element, for the pulse laser of plano-concave cavity configuration
A kind of pulse laser, the laser includes successively：Laser diode is used as pumping source 3, coupled system 4 and 5, preceding
Hysteroscope 6, Nd:YVO4Crystal 8 is made to adjust Q units as perovskite optical pulse modulation device prepared by gain medium, embodiment 1
Part 9, the part of Effect of Back-Cavity Mirror 7 six, constitute plano-concave cavity configuration as shown in Figure 3.
It is 808nm laser as pumping source 3 by the use of launch wavelength；
The Nd:YVO4The Nd of crystal3+Ion concentration is 0.10at.%, Nd:YVO4The pumping light-incident end plating of crystal
Have to 808nm and to the deielectric-coating of 1.05-1.1 mu m waveband high transmissions, plate high to 1.05-1.1 mu m wavebands on output end face
Deielectric-coating；
Front cavity mirror 6 is that Radius are the plano lens of 30mm, and outside is plated with, inner side high to 808nm and is plated with to 1.05-1.1 μ
The deielectric-coating of m high reflections, Effect of Back-Cavity Mirror 7 is that Radius are the plano-concave mirror of 30mm, and inwardly, be plated with has 6- to 1.05-1.1 μm for concave surface
The deielectric-coating of 10% transmitance；The distance between front cavity mirror 6 and Effect of Back-Cavity Mirror 7 are 3-10cm.
The perovskite optical pulse modulation device that Q switched element 9 is prepared from half vapor phase method, places near Effect of Back-Cavity Mirror, deposition
Have the one of perovskite thin film facing in laser cavity, another side is towards outside laser cavity.Increase pump power and exceed threshold value, can be direct
Obtain pulse laser output.The laser pulse sequence of 1.05-1.1 μm of produced infrared band is as shown in Figure 5.
Embodiment 4, as described in Example 3, except that Q switched element 9 is perovskite optical pulse prepared by embodiment 2
Modulation device.
Embodiment 5, perovskite optical pulse modulation device are used for the pulse laser of plano-concave cavity configuration as Q switched element
A kind of pulse laser, the laser includes successively：Xenon lamp is used as pumping source 11, Nd:YAG crystal increases as laser
Beneficial medium 12, front cavity mirror 10, Effect of Back-Cavity Mirror 14 and perovskite optical pulse modulation device are used as the part of Q switched element 13 5, composition
Plano-concave cavity configuration as shown in Figure 4.
The Nd:The Nd of YAG crystal3+Ion concentration is 0.5at.%.Nd:YAG crystal pro cessings into cylinder, two end
Face is coated with the deielectric-coating to 1.05-1.1 mu m waveband high transmissions；
Front cavity mirror 10 is that Radius are the plano lens of 50mm, and inner side is coated with to the 1.05-1.1 μm of deielectric-coating of high reflection, after
Hysteroscope 14 is that Radius are the plano-concave mirror of 50mm, and concave surface inwardly, is plated with the medium for having 3%-10% transmitances to 1.05-1.1 μm
Film；
The perovskite optical pulse modulation device that Q switched element 13 is prepared from half vapor phase method in embodiment 1, near Effect of Back-Cavity Mirror
Place, deposition has the one of perovskite thin film facing in laser cavity, another side is towards outside laser cavity.Front cavity mirror 10 and Effect of Back-Cavity Mirror 14
The distance between be 5-10cm.Increase pump power and exceed threshold value, pulse laser output can be directly obtained.
Embodiment 6, as described in Example 5, except that optical pulse modulation device 13 is from the liquid described in embodiment 2
Perovskite optical pulse modulation device prepared by phase method.
Claims (7)
1. a kind of application of perovskite optical pulse modulation device, it is characterised in that the device is used as pulse tuning Q device in laser
The application of part or mode-locking device；
The perovskite optical pulse modulation device include a quartz glass substrate, and be deposited on above the substrate, thickness is
300-600nm perovskite thin films；The deielectric-coating for being conducive to laser generation is plated with the substrate back；Deposition has perovskite thin film
One facing in laser cavity, and another side is realized being modulated the laser of 1.05-1.1 μm of infrared band towards outside laser cavity；
In laser utilization, by the way of end face or profile pump, pump light is input in gain medium, institute
Pump light is stated by, again by described perovskite impulse modulation device, being placed in before gain medium after gain medium
Front cavity mirror and the outgoing mirror that is placed in behind perovskite impulse modulation device form resonator；Described front and rear hysteroscope is plated favorably
In the deielectric-coating of laser generation.
2. the application of perovskite optical pulse modulation device as claimed in claim 1, it is characterised in that described perovskite is thin
Film is methylamino lead iodide；Perovskite thin film thickness is 400-500nm.
3. the application of perovskite optical pulse modulation device as claimed in claim 1, it is characterised in that described quartz glass
Substrate thickness is 0.5mm-2mm.
4. the application of perovskite optical pulse modulation device as claimed in claim 1, it is characterised in that in the substrate back
It is plated with the deielectric-coating to 1.05-1.1 μm high.
5. the application of perovskite optical pulse modulation device as claimed in claim 1, wherein, described gain medium is
Nd:YAG or Nd:YVO4Crystal, Nd3+Ion concentration is 0.01-0.5at.%.
6. the application of perovskite optical pulse modulation device as claimed in claim 1, wherein, described pumping source is semiconductor
Laser diode or xenon source.
7. the application of perovskite optical pulse modulation device as claimed in claim 1, wherein, described front cavity mirror selects one
Radius is the plano lens of 10-100mm, and minute surface is plated with to the 1.05-1.1 μm of deielectric-coating of high reflection, between front cavity mirror and Q-switching device
Distance be 0.05-8cm；Described Effect of Back-Cavity Mirror is the plano-concave mirror of 10-100mm from a radius, and concave surface is plated with to 1.05-
The distance between the deielectric-coating that 1.1 μm of parts pass through, Effect of Back-Cavity Mirror and Q-switching device are 0.05-8cm；Front cavity mirror and Effect of Back-Cavity Mirror away from
From being 1-10cm.
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