CN109936046A - A method of preparing rodlike micro-nano crystalline substance laser - Google Patents

A method of preparing rodlike micro-nano crystalline substance laser Download PDF

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Publication number
CN109936046A
CN109936046A CN201711359533.9A CN201711359533A CN109936046A CN 109936046 A CN109936046 A CN 109936046A CN 201711359533 A CN201711359533 A CN 201711359533A CN 109936046 A CN109936046 A CN 109936046A
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China
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micro
crystalline substance
nano
nano crystalline
rodlike
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CN201711359533.9A
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廖清
高庆刚
付红兵
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Capital Normal University
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Capital Normal University
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  • Luminescent Compositions (AREA)
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Abstract

The invention discloses a kind of methods for preparing rodlike micro-nano crystalline substance laser.This method is realized by the method for physical vapour deposition (PVD), is included the following steps: under vacuum conditions, and semi-conductor luminescent material molecule is placed on vacuum tube furnace heat source position.Temperature programming is set, the sublimation temperature of molecule is set according to the thermogravimetric curve of molecule.And lead to the inert carrier gas of given pace, such as nitrogen, argon gas from left to right, glass slide, which is placed, in the downstream of gas is used to collect rodlike micro-nano crystalline substance.Semiconductor can obtain purer rodlike semiconductor microactuator nano-crystal in fixed region due to the specificity of its de-sublimation temperature.This method solve the purity problems of rodlike micro-nano crystalline substance, and micro-nano crystalline substance purity is made to reach 100%.Device therefor is simple, quick and convenient, easy to operate, at low cost, and repeatability is very high, and the micro-nano crystalline substance of higher degree improves the properties of semiconductor laser, reduces semiconductor laser threshold value, improves laser stability, application value with higher.

Description

A method of preparing rodlike micro-nano crystalline substance laser
Technical field
The present invention relates to a kind of methods for preparing rodlike micro-nano crystalline substance laser.
Background technique
Micron nano material is the novel photoelectric functional material of Twenty-First Century, is that current World Science circle is studied Hot spot.Since micro nano structure unit is in micron/nano scale, the physicochemical characteristic of micro Nano material and micro nano structure was both different In microcosmic atom, molecule, also different from macro object, to people are explored naturally, a possibility that creating new knowledge extends To the middle field between both macro and micro object.It also implies simultaneously and finds new phenomenon in micro-nano field, understanding is new Rule proposes new concept, establishes the potentiality of new theory.
Micro nano structure system plays an important role in the technology that oneself some warps are existing and rising.In nanometer Preparation realizes the micromation of function element on scale, in microelectronic field, the smaller more complicated chip, anti-faster of meaning It answers, lower price, lower energy consumption, better performance.However, micro Nano material still has one from extensive industrial applications Set a distance, it is also necessary to further theoretical research and research of technique.This often requires that people: (1) being optimized using new method Control the component units and ordered fabrication of micro Nano material;(2) new phenomenon for exploring micro Nano material is excavated, new property and new Application value;(3) connection between micro Nano material structure and function is systematically established, particular law therein is found out.
Summary of the invention
The object of the present invention is to provide a kind of methods for preparing rodlike micro-nano crystalline substance laser.
The method provided by the invention for preparing rodlike micro-nano crystalline substance laser, includes the following steps:
Under vacuum conditions, semi-conductor luminescent material molecule is placed on vacuum tube furnace heat source position, sets program liter Temperature.And lead to the inert carrier gas of given pace, such as nitrogen, argon gas from left to right, glass slide, which is placed, in the downstream of gas is used to It is brilliant to collect rodlike micro-nano, which is rodlike micro-nano crystalline substance laser.
Semiconductor fluorescence molecule described in the above method is luminous small organic molecule.
The vacuum tube furnace is that vacuum environment is manufactured by oil-sealed rotary pump, and realization vacuum degree is 100-300 Pascal.
The heat source is diamond heating silk middle position.
Described program heating setting condition is determined by the small molecule thermogravimetric curve, and the general specific heat weightless temperature of temperature is low A bit.
The inert carrier gas rate is determined that rate is general by molecular size range and molecule deposition band of position temperature In 10-30ml/min.
The inert carrier gas ingredient is the gas molecule not reacted with fluorescent molecule, general to select nitrogen or argon Gas.
The position for placing glass slide is the suitable position that micro-nano crystalline substance largely deposits.
The present invention weighs about 1mg fluorescent molecule using TPSB small molecule as raw material, is placed in heating source position, vacuum condition Under, carrier gas flow rate is regulated, temperature programming condition, opening program heating are set.After heating and heat preservation, micro-nano laser Device can be prepared and be finished.Semiconductor can obtain purer rodlike half in fixed region due to the specificity of its de-sublimation temperature Conductor micro-nano is brilliant.This method solve the purity problems of rodlike micro-nano crystalline substance, and micro-nano crystalline substance purity is made to be up to nearly 100%.Device therefor Easy to operate, the preparation method used time is shorter, and raw materials used amount is fewer, at low cost, and repeatability is very high, higher degree Micro-nano crystalline substance improves the properties of semiconductor laser, reduces semiconductor laser threshold value, improves laser stability, has Higher application value realizes the multinomial target such as economic and environment-friendly energy conservation.
Detailed description of the invention
Fig. 1 is 1 products therefrom photograph via bright field of embodiment and fluorescence photo
Fig. 2 is 1 products therefrom laser photo of embodiment and laser spectrum.
Specific embodiment
The present invention is further elaborated combined with specific embodiments below, but the present invention is not limited to following embodiments.Institute State method is conventional method unless otherwise instructed.The raw material can be gotten from open business unless otherwise instructed.
A method of rodlike micro-nano crystalline substance laser is prepared, is included the following steps:
Under vacuum conditions, semi-conductor luminescent material molecule is placed on vacuum tube furnace heat source position, sets program liter The sublimation temperature of molecule is arranged according to the thermogravimetric curve of molecule for temperature, and leads to the inert carrier gas of given pace from left to right, in inertia The downstream of carrier gas places glass slide and is used to collect rodlike micro-nano crystalline substance.
Wherein, the vacuum is relative vacuum environment, and pressure is between 100-300 Pascal.The temperature of the distillation by Semi-conductor luminescent material thermogravimetric curve determines, is not higher than thermal weight loss minimum temperature.The inert carrier gas is anti-for that cannot participate in high temperature The gas answered, such as nitrogen, argon gas.In the step of distillation, temperature control is temperature programming.In the step of distillation, Time is 5-8 hours.In the step of distillation, the carrier gas rate is 10ml-30ml/min.The collection position of the micro-nano crystalline substance Setting in carrier gas downstream position.Collecting micro-nano crystalline substance substrate can be high temperature resistant quartz substrate.Rodlike semiconductor microactuator can be selected Nano-crystal carries out Laser Experiments.
In following embodiments, illustrate so that semi-conductor luminescent material molecule is TPSB fluorescent molecule as an example, by 2,5- diformazan Oxy-1,4- xylyl-two (diethyl phosphonate) react Horner- by Huo Naer-Wordsworth-Ai Mengsi Wadsworth-Emmons (HWE) reaction obtains.It can make micro-nano crystalline substance without exquisiteness and prepare raw material.
Embodiment 1,
It weighs TPSB semi-conductor luminescent material molecule 0.8mg and is placed on vacuum tube furnace heat source position, and lead to from left to right The inert carrier gas argon gas of 10ml/min flow velocity places glass slide in the downstream of gas and is used to collect rodlike micro-nano crystalline substance, in vacuum Under condition 100pa, temperature programming is set, sets gradient increased temperature condition, holding temperature is arranged at 350 DEG C, constant temperature 5 hours. After tube furnace is restored to room temperature, glass slide is taken out, deposits a large amount of micro-nano Jingjing bodies above, which is that rodlike micro-nano crystalline substance swashs Light device.
Micro-nano crystalline substance length is mainly distributed in 15 micron ranges, and carrying out pumping by 400nm femtosecond laser can be collected into The laser that rodlike micro-nano trichite goes out.
Embodiment 2,
It weighs TPSB semi-conductor luminescent material molecule 1.3mg and is placed on vacuum tube furnace heat source position, and lead to from left to right The inert carrier gas argon gas of 20ml/min flow velocity places glass slide in the downstream of gas and is used to collect rodlike micro-nano crystalline substance, in vacuum Under condition 130pa, temperature programming is set, sets gradient increased temperature condition, holding temperature is arranged at 330 DEG C, constant temperature 5 hours. After tube furnace is restored to room temperature, glass slide is taken out, deposits a large amount of micro-nano Jingjing bodies above, which is that rodlike micro-nano crystalline substance swashs Light device.
Micro-nano crystalline substance length is mainly distributed in 25 micron ranges, and carrying out pumping by 400nm femtosecond laser can be collected into The laser that rodlike micro-nano trichite goes out.

Claims (10)

1. a kind of method for preparing rodlike micro-nano crystalline substance laser, includes the following steps:
Under vacuum conditions, semi-conductor luminescent material molecule is placed on vacuum tube furnace heat source position, sets temperature programming, root According to the sublimation temperature of the thermogravimetric curve setting molecule of molecule, and lead to the inert carrier gas of given pace from left to right, in inert carrier gas Downstream place glass slide be used to collect rodlike micro-nano it is brilliant.
2. according to the method described in claim 1, pressure is in 100-300 it is characterized by: the vacuum is relative vacuum environment Between Pascal.
3. method according to claim 1 or 2, it is characterised in that: the temperature of the distillation is by semi-conductor luminescent material heat Weight curve determines, is not higher than thermal weight loss minimum temperature.
4. according to the method described in claim 1, it is characterized by: the inert carrier gas is the gas that cannot participate in pyroreaction Body.
5. according to the method described in claim 1, it is characterized by: temperature control is temperature programming in the step of the distillation.
6. according to the method described in claim 1, it is characterized by: the time is 5-8 hours in the step of the distillation.
7. according to the method described in claim 1, it is characterized by: the carrier gas rate is 10ml- in the step of the distillation 30ml/min。
8. according to the method described in claim 1, it is characterized by: the collection position of micro-nano crystalline substance is located at inert carrier gas downstream Position.
9. according to the method described in claim 1, it is characterized by: collecting micro-nano crystalline substance substrate is high temperature resistant quartz substrate.
10. according to the method described in claim 1, it is characterized by: rodlike semiconductor microactuator nano-crystal is selected to carry out Laser Experiments.
CN201711359533.9A 2017-12-17 2017-12-17 A method of preparing rodlike micro-nano crystalline substance laser Withdrawn CN109936046A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110359086A (en) * 2018-04-11 2019-10-22 首都师范大学 One-step method prepares the process of polychrome micro-nano crystalline substance

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015011320A1 (en) * 2013-07-23 2015-01-29 Mateo Herrero María Pilar Microencapsulated biocide repellent composition having a double repellency action, textile garment comprising same and use of said garment
CN106169693A (en) * 2016-08-23 2016-11-30 东南大学 A kind of dyestuff auto polymerization thin film accidental laser and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015011320A1 (en) * 2013-07-23 2015-01-29 Mateo Herrero María Pilar Microencapsulated biocide repellent composition having a double repellency action, textile garment comprising same and use of said garment
CN106169693A (en) * 2016-08-23 2016-11-30 东南大学 A kind of dyestuff auto polymerization thin film accidental laser and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
FANGMEI LIU ET AL.: "Controllable fabrication of copper phthalocyanine nanostructure crystals", 《NANOTECHNOLOGY》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110359086A (en) * 2018-04-11 2019-10-22 首都师范大学 One-step method prepares the process of polychrome micro-nano crystalline substance

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Application publication date: 20190625