CN2476811Y - High-temp thermal stage device for measuring laser micro-Raman spectrum - Google Patents

High-temp thermal stage device for measuring laser micro-Raman spectrum Download PDF

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Publication number
CN2476811Y
CN2476811Y CN 01238010 CN01238010U CN2476811Y CN 2476811 Y CN2476811 Y CN 2476811Y CN 01238010 CN01238010 CN 01238010 CN 01238010 U CN01238010 U CN 01238010U CN 2476811 Y CN2476811 Y CN 2476811Y
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CN
China
Prior art keywords
temperature
electric heater
boundary layer
stage body
high temperature
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Expired - Fee Related
Application number
CN 01238010
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Chinese (zh)
Inventor
殷绍唐
王爱华
仇怀利
刘晓静
许国志
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Anhui Institute of Optics and Fine Mechanics of CAS
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Anhui Institute of Optics and Fine Mechanics of CAS
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Priority to CN 01238010 priority Critical patent/CN2476811Y/en
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Publication of CN2476811Y publication Critical patent/CN2476811Y/en
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Abstract

The utility model discloses a high temperature table which is applied in laser-micro Roman spectrum measuring. Body and cover of the high temperature table respectively have two shell layers. An air extracting hole is positioned in the cover of the table. A thermal insulation medium is arranged in the body of the table and a platinum crucible is positioned on an electric heater which is interwinded with platinum heating wires. With the structure, temperature gradient in longitudinal direction and transverse direction can be realized. The utility model adopts automatic heating up and controlling system to accurately control temperature. Stable solid/liquid boundary layer comes into being when crystals are heated to melting point. When the boundary layer is connected with inactive gas, samples can be prevented from oxidizing. When the boundary layer is connected with cooling water circulation, surface temperature of the micro high temperature table keeps the same as room temperature. The boundary layer is connected with an air extracting system, thereby crystal window can be prevented from polluted by volatile substance and connecting the boundary layer to laser-micro Roman spectrometer, real time measurement of Roman spectrum of crystal phase, solid or liquid boundary phase and molten bath can be made at the time of high temperature crystal growth to research the structure and the formation mechanism of the crystal phase, the crystal phase, the solid or liquid boundary phase and the molten bath.

Description

The high-temperature stage device that micro raman spectra is measured
The measuring technique equipment of solid/liquid interfaces layer structure belonged to the optical experiment instrument field when the utility model related to a kind of real-time measurement crystal growth.
Crystal growth is the Dynamic Coupling of transport process (heat transportation and mass transport) and interface growth process.In crystal growth method by melt, physics, chemical variable parameter are more, and number of drawbacks can appear in crystal.Therefore to obtain high-quality optical crystal, be necessary structure, character and the variation thereof of solid/liquid interfaces layer in the crystal growing process are studied, nineteen ninety-five Yuan Hui openly reported from crystal growing process surface tension and action of gravity in the artificial lens journal third phase, observed particle transporting direction device.Device includes the high temperature crystal growth chamber; crystal growth is indoor annular platinum filament well heater; there is quartz window the device top; can lead to protective gas in the growth room; it is the BH-2 type differential interference microscope that the Japanese OLKMPUS of employing company produces that part is observed in its crystal growth; and done corresponding improvement; the crystal growth recording section has comprised long-focus CCD camera, VTR device and television monitoring mouth; the cinephotomicrography light path is connected with the shooting register system, observes in the high temperature crystal growth process in the horizontal direction and gravity direction particle transport phenomena.
Professor Yu Xiling of Shandong University in 1998 designs a cover glass crystallizer and measures low temperature (less than 30 ℃) Crystal Growth from Aqueous Solution solid/liquid interfaces and boundary layer structure down at 100 ℃, and applied for patent of invention and practical patent, the patent No. is respectively 981100309,98220096.
Above-mentioned several method does not all have in real time to be observed thickness, shape, the structure of the functional crystal material growth solid/liquid interfaces of high temperature (1000 ℃), and the micro-Raman spectrum of Laser Measurement, further variation, the growth mechanism of research structure.
The purpose of this utility model provides the high-temperature stage device that a kind of micro raman spectra is measured.
The purpose of this utility model is achieved through the following technical solutions.
The high-temperature stage device that micro raman spectra is measured, stage body, Tai Gai are arranged, platform has covered quartz window, and thermal insulation medium is arranged in the stage body, it is characterized in that stage body and Tai Gai are two layers of housing, platform covers and has aspirating hole, have an inert gas through hole on the stage body, stage body, platform cover respectively two water inlet pipe and water outlet pipes, is placed with electric heater on the thermal insulation medium, be placed with crucible on the electric heater, the back backing of band light hole is arranged on the crucible.
Described electric heater is that three blocks of corundum are formed flute profile, on every block of corundum, at the intensive winding heating wire in needs high temperature place, do not twine heating wire not needing heating place, twine a small amount of heating wire in a small amount of heating place, realize the thermograde of vertical and horizontal on the electric heater, composition can form the temperature field of stablizing solid/liquid interfaces layer structure.
Described thermal insulation medium is a foamed alumina, and crucible is a Platinum crucible, and back backing is a graphite flake.
Compare with prior art, the utility model is rational in infrastructure, and multiple functional and micro raman spectra instrument combination has realized Real Time Observation and measurement to the high temperature crystal growth solid/liquid interfaces.
1. the platinum heating wire connects the intensification temperature-controlling system, and temperature can be raised to 1200 ℃, and constant temperature is at fusing point time error ± .01 ℃.
2. connection cooling water recirculation system, the hot platform surface temperature when being warming up to 1200 ℃ still keeps room temperature.
3. the Re Tainei filling with inert gas can prevent sample oxidation when high temperature, guarantees that the crystal chemistry composition is constant.
4. venthole connects extract system, can extract the melt volatile matter out, guarantees that the experiment window is not contaminated, normally obtains light signal.
5. thermal insulation medium can keep temperature stabilization in the platform, reduces thermal loss.
Electric heater have laterally, longitudinal temperature gradient, form stable solid/liquid interfaces layer structure.
Accompanying drawing is the utility model structural representation.
Below in conjunction with accompanying drawing,, the utility model is further described by embodiment.
Embodiment:
Referring to accompanying drawing
The utility model has stage body 9, platform lid 11, on the platform lid 11 aspirating hole is arranged, quartz window 8, thermal insulation medium 12 is arranged in the stage body 9, stage body 9, on the platform lid 11 two water inlet pipe and water outlet pipes 2 are arranged respectively, stage body 9, platform lid 11 is two layers of shell structure, water inlet pipe and water outlet pipe 2 can connect cooling circulating water, keeping the stage body surface temperature is room temperature, have an inert gas through hole 3 on the stage body 9, can connect the inert gas steel cylinder, prevent sample oxidation when high temperature, the chemical composition of guaranteeing crystal is constant, be placed with electric heater 6 on the thermal insulation medium 12, electric heater is that three blocks of corundum are formed flute profile, be wound with platinum heating wire 1 on the electric heater 6, platinum heating wire 1 connects the intensification temperature-controlling system by lead, electric heater 6 platinum heating wire from right to left twines by close and rare, until not twining, to realize laterally, gradient temperature longitudinally, be placed with Platinum crucible 10 on the electric heater 6, high-temperature fusant method grown crystal sample 5 is arranged in the Platinum crucible 10, be placed with graphite flake 7 on the Platinum crucible 10, there is a logical light viewport in graphite flake 7 central authorities.
When the utility model uses, because electric heater has laterally, thermograde longitudinally, can form stable solid/liquid interfaces layer structure, by Raman spectrometer energy Real Time Observation solid/liquid interfaces layer, and measure its shape and thickness, measure the micro raman spectra of crystal solid/liquid interfaces layer simultaneously in real time.

Claims (3)

1, the high-temperature stage device of micro raman spectra measurement, stage body, Tai Gai are arranged, platform has covered quartz window, and thermal insulation medium is arranged in the stage body, it is characterized in that stage body and Tai Gai are two layers of housing, platform covers and has aspirating hole, have an inert gas through hole on the stage body, stage body, platform cover respectively two water inlet pipe and water outlet pipes, is placed with electric heater on the thermal insulation medium, be placed with crucible on the electric heater, the back backing of band light hole is arranged on the crucible.
2, the high-temperature stage device of answering 1 described micro raman spectra to measure according to claim, it is characterized in that described electric heater is that three blocks of corundum are formed flute profile, on every block of corundum, at the intensive winding heating wire in needs high temperature place, do not twine heating wire not needing heating place, twine a small amount of heating wire in a small amount of heating place, realize the thermograde of vertical and horizontal on the electric heater.
3, the high-temperature stage device of micro raman spectra measurement according to claim 1 is characterized in that described thermal insulation medium is a foamed alumina, and crucible is a Platinum crucible, and back backing is a graphite flake.
CN 01238010 2001-05-27 2001-05-27 High-temp thermal stage device for measuring laser micro-Raman spectrum Expired - Fee Related CN2476811Y (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 01238010 CN2476811Y (en) 2001-05-27 2001-05-27 High-temp thermal stage device for measuring laser micro-Raman spectrum

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 01238010 CN2476811Y (en) 2001-05-27 2001-05-27 High-temp thermal stage device for measuring laser micro-Raman spectrum

Publications (1)

Publication Number Publication Date
CN2476811Y true CN2476811Y (en) 2002-02-13

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CN 01238010 Expired - Fee Related CN2476811Y (en) 2001-05-27 2001-05-27 High-temp thermal stage device for measuring laser micro-Raman spectrum

Country Status (1)

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CN (1) CN2476811Y (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104502324A (en) * 2014-12-29 2015-04-08 东北大学 Micro heating platform for measuring molten salt electriochemistry in-situ Raman spectrum and sample cell
CN106622405A (en) * 2016-12-26 2017-05-10 天津商业大学 Anti-condensation constant-temperature box
CN109313123A (en) * 2016-06-15 2019-02-05 康宁股份有限公司 For handling method, system and the equipment of glass material according to crystal state

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104502324A (en) * 2014-12-29 2015-04-08 东北大学 Micro heating platform for measuring molten salt electriochemistry in-situ Raman spectrum and sample cell
CN104502324B (en) * 2014-12-29 2017-04-05 东北大学 Melten salt electriochemistry original position Raman spectral measurement microscopic heating stands
CN109313123A (en) * 2016-06-15 2019-02-05 康宁股份有限公司 For handling method, system and the equipment of glass material according to crystal state
CN109313123B (en) * 2016-06-15 2021-08-27 康宁股份有限公司 Method, system and apparatus for processing glass materials according to crystalline state
CN106622405A (en) * 2016-12-26 2017-05-10 天津商业大学 Anti-condensation constant-temperature box

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