CN102393356A - Microscope heating stage for Raman spectral measurement of high-temperature volatile molten salt - Google Patents
Microscope heating stage for Raman spectral measurement of high-temperature volatile molten salt Download PDFInfo
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- CN102393356A CN102393356A CN201110329976XA CN201110329976A CN102393356A CN 102393356 A CN102393356 A CN 102393356A CN 201110329976X A CN201110329976X A CN 201110329976XA CN 201110329976 A CN201110329976 A CN 201110329976A CN 102393356 A CN102393356 A CN 102393356A
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Abstract
The invention provides a microscope heating stage for the Raman spectral measurement of high-temperature volatile molten salt. The microscope heating stage comprises a heating stage main body and an internal heating body, wherein a microlens hole is arranged on one side of the heating stage main body; a heating stage cover is arranged above the heating stage main body; a thermocouple insertion hole and an air hole are formed on the heating stage cover; a platform for placing a sample pool is arranged at the lower part of the interior of the heating stage main body, and a winding post is fixed at the bottom part of the interior of the heating stage; a bobbin is sleeved outside the winding post; a heating wire is wound on the bobbin; the winding post, the bobbin and the heating wire form the internal heating body; the heating wire extends out of the heating stage main body and is connected with an external power supply; the bottom part of the heating stage main body is connected to a strut and a base; and a sample pool made of quartz is correspondingly arranged in the heating stage main body. The heating stage provided by the invention adopts a heating mode in the sample pool and avoids influence of non-uniform volatilization of the molten salt on the accuracy of the Raman spectral measurement by sealing the sample pool; and as the excitation laser enters from the side of the sample pool, a thermocouple and a measurement focus are located on the same horizontal line, and the accuracy of temperature measurement is ensured.
Description
Technical field
The invention belongs to the instrument analysis technology field, particularly a kind of cell for Raman spectrum measurement of high-temperature volatile molten salt is used microscopic heating stand.
Background technology
Since the last century the eighties; Micro-Raman spectrometric techniques develops rapidly and widespread use; Yet but there are many difficulties in the micro-Raman spectroscopic assay of high-temperature volatile molten salt; High-temperature molten salt all has corrosivity usually, so desire realizes that the Raman spectral measurement of its structure need adopt special material.Industry research personnel have developed the form of several kinds of sample cells to the Raman spectroscopic assay of volatile molten salt, but all exist shortcoming.
A kind of typical " windowless sample cell " and microscopic heating stand, as shown in Figure 1, utilize the surface tension effect of liquid and make fused salt not flow out sample cell; On the identical plane of sample cell, offer two more holes of minor diameter, its direction is perpendicular to main aperture, two more the hole of minor diameter be used for incident laser, and main aperture is used for the Raman scattering of light.
The micro-Raman spectroscopic assay of a kind of new high-temperature volatile melt is with sample cell and Re Tai, and is as shown in Figure 2, and its main purpose of design is in order to prevent the infringement of fused salt volatile matter for spectrometer.Sample places the thin platinotron of end sealing, and the capillary action of surface tension effects and the platinotron of high-temperature fusant through liquid remains in the platinum pipe and can not flow out; Sample cell configuration chromel-alumel thermopair in order to prevent the corrosion of high-temperature fusant, is placed in another platinotron, and two platinotrons closely connect, and outer cover is with quartz ampoule, and the whole sample pond places the hot platform of a traverse.
Hot platform is used in the micro-Raman spectroscopic assay of a kind of high-temperature volatile molten salt with fan, and is as shown in Figure 3, adopts top to advance the mode of light; Because when using this hot platform, amount of samples is very big, produces volatilization in a large number; So between microlens and Sheng appearance crucible, put a fan, volatile matter blown away.
In the above-mentioned sample cell, windowless sample cell and tubular specimen pond specimen in use amount are less, volatilize to the external world owing to wait to study fused salt, if volatile matter is different with research fused salt composition, the internal composition of fused salt will change, thus the accuracy of influence research.And the sample cell of band fan; The influence that the component that causes owing to the fused salt volatilization changes experimental precision still exists; And when using this microscopic heating stand, need microscope bigger focal length to be arranged to guarantee the space of fan, higher to the requirement of micro-Raman spectrometer.
Because volatilization has a negative impact to Raman spectroscopic assay meeting; The micro-Raman spectroscopic assay that facts have proved high-temperature volatile molten salt is adopted sidepiece to advance light more to help experimental implementation; But the focal length of microlens is shorter usually, therefore the design of microscopic heating stand and sample cell is had higher requirement.
Summary of the invention
To of defective and the designing requirement of existing cell for Raman spectrum measurement of high-temperature volatile molten salt with sample cell and microscopic heating stand; The present invention provides a kind of cell for Raman spectrum measurement of high-temperature volatile molten salt with microscopic heating stand and sample cell; Reduce the influence of the effusion of volatile matter, to improve the mensuration precision of Raman spectrum to the composition of fused salt to be measured.
Microscopic heating stand provided by the invention comprises hot platform main body and inner calandria; Hot platform main body is columnar structured; Hot platform main body one side is provided with the microlens hole that microlens is stretched into; Hot platform main body is respectively equipped with circulation waterway in top, the bottom in microlens hole, and circulation waterway links to each other with the cooling water recirculation system of outside through the recirculated water connecting pipe; Hot platform main body upper fixed is connected with Re Taigai, and hot platform covers and offers hole and the pore that thermopair inserts, and top, two holes is installed thermopair respectively and stretched into pipe and tracheae, and tracheae links to each other with the aspiration pump system of outside; The bottom is provided with the platform of placing sample cell in the hot platform main body; The bottom is fixedly connected wrapping post, and wrapping post is set with bobbin outward, and bobbin is an alundum tube; Heater wire is wrapped on the bobbin; Wrapping post, bobbin and heater wire constitute inner calandria, and the both sides of platform and wrapping post junction are provided with through hole, and heater wire stretches out hot platform main body by two through hole and links to each other with external power source; Hot platform bottom part body connecting struts, the pillar other end is connected on the base, and the pillar height need guarantee to have between base and the Re Tai main body binding post of enough space mounting heater wires; The supporting sample cell that is provided with in the hot platform main body.
Said hot platform base is fixedly connected on the platform that can move horizontally, to realize whole the moving of hot platform, the operation of convenient adjustment focal length.
Said sample cell is made up of sample cell lid and sample cell main body; The sample cell main body is concave structure, the upper opening that cooperates with inner calandria; Sample cell lid is fitted on the sample cell main body, and through ground or the high-temperature cement slit that is sealed and matched, sample cell covers a side and is provided with porose; Be provided with a closed pore quartz ampoule in the hole, quartz ampoule stretches in the sample cell main body.
When using this microscopic heating stand and sample cell; Sample is put into sample cell, build sample cell lid and sealing, sample cell is inserted the calandria outside, inside of microscopic heating stand; Cover Re Taigai; The thermopair that again thermopair is covered from hot platform stretches into pipe and stretches into the quartz ampoule of remaining silent in the sample cell main body, and power-on provides electric current to heater wire, the beginning heating sample; Use energizer to produce laser; Microlens is stretched in the microlens hole of hot platform main body and fixing; Microlens is aimed at the sample of sample cell main body, realizes accurately focusing through horizontal shifting platform, uses micro laser Raman spectrometer to carry out the Raman spectroscopic assay.
The invention has the beneficial effects as follows:
⑴ sample cell of the present invention is arranged on the calandria outside; The space constraint of having avoided traditional sample cell to be brought in calandria inside; Can suitably increase the sample cell capacity; Hold more sample, thereby improve the degree of accuracy of experiment and guaranteed the strict demand of micro-Raman spectroscopic assay for focal length;
⑵ the spectrometric excitation laser of Raman gets into sample cell from sidepiece, guarantees that enough spaces make thermopair go deep into the sample cell from top, makes thermopair and measures focus on same horizontal line, guarantees to measure the accuracy of temperature;
⑶ microlens is arranged on the sample cell sidepiece, the pollution that can effectively avoid the sample volatile matter possibly cause camera lens.
Description of drawings
Fig. 1 is typical case's " windowless sample cell " and microscopic heating stand synoptic diagram;
Fig. 2 is that tubulose Raman spectroscopic assay is with sample cell and microscopic heating stand synoptic diagram;
Fig. 3 is with the micro-Raman spectroscopic assay of high-temperature volatile molten salt of fan with hot platform synoptic diagram;
Fig. 4 is the microscopic heating stand and the sample cell assembling synoptic diagram of the embodiment of the invention;
Fig. 5 is the sample pool structure synoptic diagram of the embodiment of the invention;
Among the figure: 1-tracheae, the hot platform lid of 2-, 3-cocycle water route, 4-cocycle water connecting pipe; 5-microlens hole, 6-pillar, 7-base, 8-thermopair; The 9-thermopair stretches into pipe, 10-sample cell lid, 11-sample cell main body, 12-wrapping post; The 13-bobbin, recirculated water connecting pipe under the 14-, circulation waterway under the 15-, 16-heater wire.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is further specified.
Microscopic heating stand provided by the invention and sample cell; Microscopic heating stand comprises hot platform main body and inner calandria; Hot platform main body is columnar structured; Hot platform main body one side is provided with the truncated cone-shaped microlens hole 5 that microlens is stretched into, and the diameter in hole is beneficial to the adjusting of focal length greater than the diameter of microlens; Hot platform main body is at the top in microlens hole 5, the cocycle water route 3 that the bottom is respectively equipped with circumferential annular, following circulation waterway 15, and circulation waterway links to each other with the cooling water recirculation system of outside through cocycle water connecting pipe 4, following recirculated water connecting pipe 14 respectively; Hot platform main body top is fixedly connected with hot platform lid 2 through being threaded; Offer hole and the pore that thermopair inserts on the hot platform lid 2; Pipe 9 and tracheae 1 are stretched in top, the two holes thermopair of welded and installed aluminum alloy material respectively, and tracheae 1 links to each other with the aspiration pump system of outside and realizes feeding or the discharge that the inner gas of hot platform divides; Inner calandria comprises wrapping post 12, bobbin 13 and heater wire 16; Hot platform main body lower inner is provided with the circular platform of placing sample cell, and the bottom is through the internal and external threads wrapping post 12 that is connected, and bobbin 13 adopts alundum tubes; The wrapping post 12 outer bobbins 13 that are set with; Heater wire 16 is wrapped on the bobbin 13, and the both sides of platform and wrapping post 12 junctions are provided with through hole, and heater wire 16 stretches out hot platform main body by two through hole and links to each other with external power source; Hot platform bottom part body is through threaded engagement connecting struts 6; Pillar 6 other ends are connected on the base 7 through threaded engagement; Pillar 6 highly needs to guarantee to have between base 7 and the Re Tai main body binding post of enough space mounting heater wires 16; Hot platform base 7 is fixedly connected on the horizontal shifting platform, to realize whole the moving of hot platform, the operation of convenient adjustment focal length; Sample cell is arranged on hot platform body interior, is made up of with sample cell main body 11 sample cell lid 10, and sample cell main body 11 is the quartz construction of spill light-permeable; Upper opening, groove are placed on around heater wire 16 on the platform of hot platform bottom part body, and 10 cooperations of sample cell lid are assemblied on the sample cell main body 11; And through the high-temperature cement slit that is sealed and matched; Sample cell lid 10 stretches into pipe 9 corresponding positions with thermopair and is provided with a hole, is provided with a closed pore quartz ampoule in the hole, and quartz ampoule and sample cell lid 10 are integral structure; Quartz ampoule stretches in the sample cell main body 11, and thermopair 8 stretches into pipe 9 through the thermopair on the hot platform lid 2 and stretches in the quartz ampoule.
It is following to adopt above-mentioned microscopic heating stand and sample cell to carry out the specific operation process of Raman spectral measurement of high-temperature volatile molten salt:
⑴ pack sample to be analyzed in the quartz specimen tank main body 11; Build sample cell lid 10; The place, slit adopts the sealing of high temperature quick hardening cement between sample cell lid 10 and the sample cell main body 11; Thereby prevent that the fused salt volatile matter from overflowing, reduce composition that the inhomogeneous volatilization of sample causes and change the instrument and equipment of destruction to cause to(for) the spectrometric influence of Raman and volatile matter;
⑵ insert sample cell in the calandria outside, inside of microscopic heating stand; Build hot platform lid 2; Again the thermopair of thermopair 8 from hot platform lid 2 stretched into pipe 9 and stretch into the quartz ampoule of remaining silent in the sample cell main body 11, tracheae 1 is connected with the aspiration pump system of external belt absorption plant;
⑶ power-on provides electric current to heater wire 16, and heating sample is heated to the measurement temperature with sample to be analyzed, with fused salt specimen temperature in the thermopair 8 measuring samples ponds;
⑷ present embodiment utilizes the IK3301R-G He-Cd 325nm burst of ultraviolel device of Japanese Kimmon Koha company to produce exciting light; Adopt the microscope and the turning camera lens (10x) of Japanese Olympus company to carry out laser focusing; Microlens is stretched in the microlens hole 5 of hot platform main body and fixing; Microlens is aimed at the sample in the quartz specimen tank main body 11, accurately focuses through the Platform Implementation that moves horizontally firm banking 7;
⑸ adopt the HR800 type micro laser Raman spectrometer of Horiba Jobin Y ' von company to carry out the Raman spectroscopic assay of sample.
The present invention is applicable to high-temperature volatile molten salt such as NaNO
3, NaF-AlF
3Deng the Raman spectral measurement, through evidence, the signal to noise ratio (S/N ratio) of measured spectrum is very high.
Claims (6)
1. a cell for Raman spectrum measurement of high-temperature volatile molten salt is used microscopic heating stand, it is characterized in that: said microscopic heating stand comprises hot platform main body and inner calandria, and hot platform main body one side is provided with the microlens hole that microlens is stretched into; Hot platform main body top is provided with dismountable hot platform lid, and hot platform covers and offers hole and the pore that thermopair inserts; The bottom is provided with the platform of placing sample cell in the hot platform main body; The bottom is fixedly connected wrapping post, and wrapping post is set with bobbin outward, and heater wire is wrapped on the bobbin; Wrapping post, bobbin and heater wire constitute inner calandria, and heater wire stretches out hot platform main body and links to each other with external power source; Hot platform bottom part body is connected on pillar and the base; The supporting sample cell that is provided with in the hot platform main body.
2. cell for Raman spectrum measurement of high-temperature volatile molten salt according to claim 1 is used microscopic heating stand, it is characterized in that being provided with circulation waterway around the said hot platform main body, and circulation waterway links to each other with the cooling water recirculation system of outside through the recirculated water connecting pipe.
3. cell for Raman spectrum measurement of high-temperature volatile molten salt according to claim 1 is used microscopic heating stand, it is characterized in that said bobbin is an alundum tube.
4. cell for Raman spectrum measurement of high-temperature volatile molten salt according to claim 1 is used microscopic heating stand, it is characterized in that said hot platform base is fixedly connected on the platform that can move horizontally.
5. cell for Raman spectrum measurement of high-temperature volatile molten salt according to claim 1 is used microscopic heating stand, it is characterized in that: said sample cell comprises the sample cell main body, and the sample cell main body is the concave structure that cooperates with inner calandria, upper opening.
6. cell for Raman spectrum measurement of high-temperature volatile molten salt according to claim 5 is used microscopic heating stand; It is characterized in that said sample cell also comprises the sample cell lid; The sample cell lid is fitted on the sample cell main body, and the slit that is sealed and matched, and sample cell covers a side and is provided with porose; Be provided with a closed pore quartz ampoule in the hole, quartz ampoule stretches in the sample cell main body.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110329976 CN102393356B (en) | 2011-10-26 | 2011-10-26 | Microscope heating stage for Raman spectral measurement of high-temperature volatile molten salt |
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| CN 201110329976 CN102393356B (en) | 2011-10-26 | 2011-10-26 | Microscope heating stage for Raman spectral measurement of high-temperature volatile molten salt |
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| CN102393356B CN102393356B (en) | 2013-07-10 |
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Cited By (3)
| 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 |
| CN106970066A (en) * | 2017-03-28 | 2017-07-21 | 东北大学 | The microscopic heating stand device of gas meltage in a kind of spectroscopy measurements high-temperature molten salt system based on Raman |
| CN105738344B (en) * | 2016-04-26 | 2018-08-28 | 东北大学 | A kind of electrochemical in-situ raman spectroscopy measurement microscopic heating stand and sample cell system |
Citations (3)
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| US20010044129A1 (en) * | 2000-03-14 | 2001-11-22 | Jian Ling | Methodology of using raman imaging microscopy for evaluating drug action within living cells |
| CN1388368A (en) * | 2001-05-27 | 2003-01-01 | 中国科学院安徽光学精密机械研究所 | Real-time measuring method of solid-liquid interface structure in high-temperature melt process of crystal growth and high-temperature heating stage |
| CN101629899A (en) * | 2009-08-28 | 2010-01-20 | 东北大学 | Sealed sample cell for Raman spectrum measurement of high-temperature volatile molten salt and use method thereof |
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2011
- 2011-10-26 CN CN 201110329976 patent/CN102393356B/en not_active Expired - Fee Related
Patent Citations (3)
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|---|---|---|---|---|
| US20010044129A1 (en) * | 2000-03-14 | 2001-11-22 | Jian Ling | Methodology of using raman imaging microscopy for evaluating drug action within living cells |
| CN1388368A (en) * | 2001-05-27 | 2003-01-01 | 中国科学院安徽光学精密机械研究所 | Real-time measuring method of solid-liquid interface structure in high-temperature melt process of crystal growth and high-temperature heating stage |
| CN101629899A (en) * | 2009-08-28 | 2010-01-20 | 东北大学 | Sealed sample cell for Raman spectrum measurement of high-temperature volatile molten salt and use method thereof |
Non-Patent Citations (1)
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| 廖远琰 等: "激光Raman多相催化原位光谱样品池", 《化学物理学报》, vol. 5, no. 5, 31 October 1992 (1992-10-31) * |
Cited By (5)
| 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 |
| CN105738344B (en) * | 2016-04-26 | 2018-08-28 | 东北大学 | A kind of electrochemical in-situ raman spectroscopy measurement microscopic heating stand and sample cell system |
| CN106970066A (en) * | 2017-03-28 | 2017-07-21 | 东北大学 | The microscopic heating stand device of gas meltage in a kind of spectroscopy measurements high-temperature molten salt system based on Raman |
| CN106970066B (en) * | 2017-03-28 | 2019-06-18 | 东北大学 | A kind of microscopic heating stand device based on gas meltage in Raman spectroscopy measurements high-temperature molten salt system |
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Inventor after: Hu Xianwei Inventor after: Gao Bingliang Inventor after: Li Huan Inventor after: Liu Jingjing Inventor after: Shi Zhongning Inventor after: Wang Zhaowen Inventor before: Hu Xianwei Inventor before: Gao Bingliang Inventor before: Li Huan Inventor before: Liu Jingjing Inventor before: Shi Zhongyu Inventor before: Wang Zhaowen |
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Free format text: CORRECT: INVENTOR; FROM: HU XIANWEI GAO BINGLIANG LI HUAN LIU JINGJING SHI ZHONGYU WANG ZHAOWEN TO: HU XIANWEI GAO BINGLIANG LI HUAN LIU JINGJING SHI ZHONGNING WANG ZHAOWEN |
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