CN1239776A - High-temperature sample heater for real-time spectrum measurement - Google Patents
High-temperature sample heater for real-time spectrum measurement Download PDFInfo
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- CN1239776A CN1239776A CN 98115334 CN98115334A CN1239776A CN 1239776 A CN1239776 A CN 1239776A CN 98115334 CN98115334 CN 98115334 CN 98115334 A CN98115334 A CN 98115334A CN 1239776 A CN1239776 A CN 1239776A
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- temperature
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- spectrum measurement
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Abstract
The sample heater consists of mainly one platinum wire ring as sample holder and one small automatic temperature controlling heating furnace with three through holes. The sample may be heated to temperature as has as 400-1200 deg.c and the very thin sample (below 0.5 mm) may be measured through either transmission or reflection process. Applying the heater and through regulating and controlling the temperature inside the high temperature heating furnace, may be reached the aim of researching the physical and chemical properties of some material in high temperature state and studying the liquid phase structure of material and the structure change of the material during solid-liquid transformation.
Description
The present invention relates to the spectral measurement field, particularly relate to the real-time measurement of the molecular spectrum of high temperature mushy stage sample.
The real-time measurement of the molecular spectrum of high temperature mushy stage material is under the researching high-temperature state, and the physico-chemical property of material is particularly understood the liquid phase structure of material and solid---the important means of structural change in the liquid phase transition process.This means also have important use in the research of crystal growth.It can be used for studying the structure of growth mother liquid in the crystal growing process, growth unit forms and consequent influence to structure phase and crystallization process: can study the influence of cosolvent to mother liquor crystallization and crystal growth, provide information and foundation for selecting cosolvent.One of key of the real-time measurement of the molecular spectrum of realization high temperature mushy stage phase transition process is to make the high-temperature sample heater that a cover is applicable to real-time spectrum measurement.So far, though also have much about report with structural change in the molecular spectrum research phase transition process, as document: 1) W.P.Pet al.J.Polym.Sci, Polym Phys Ed, 1986,24 (24) 827; 2) Wen Zaiqing etc., macromolecule journal 1991 (2), 206,1991 (4), 430 and 3) Wu Guangsun etc., Journal of Molecular Catalysis 1987,1 (1) 45) in introduced these research.But concentrate on mostly on some superpolymer and the liquid crystal etc., its heated perimeter is generally at 200-400 ℃, and is the highest not above 400 ℃, can not satisfy the research of the liquation (generally more than 1000 ℃) of most of high temperature crystal growth.
The object of the present invention is to provide the temperature automatically controlled small sample high-temperature heating equipment of a cover, to satisfy the needs of measuring high temperature mushy stage sample molecule spectrum in real time.
Technical scheme of the present invention is that high-temperature sample heater (Fig. 1) is by the outer furnace shell (1) that can lead to chilled water, internal furnace (2), heating element (3), specimen holder (4), light hole (5), temperature-control heat couple (6), temperature thermocouple (7) and insulation material (8) are formed.Furnace temperature is by temperature-control heat couple, temperature thermocouple and self-actuated controller be control and measurement automatically, on half height of level face of high temperature furnace, have three light holes (Fig. 2), wherein the center of two holes (9) and (10) is on same straight line, another hole (11) then with the center on line in these two holes form an angle (10 °-170 °).Specimen holder is made by platinum filament, an end of platinum filament is curved the ringlet of diameter 5～8mm.During use, the crucible of earlier sample being packed into, place muffle furnace to be heated to the sample fusing then, with proposing the liquid level cooling then in the platinum filament ringlet immersion liquation, in the platinum filament ringlet, adhere to the very thin solid sample of one deck this moment, move to this platinum filament ringlet in the high temperature furnace heating arrangement then and place half high position (light hole position) of stove, stove begins to be warming up to the sample fusing.When transmission configuration was measured, flashlight was from receiving with a collection optical system with pump light ingate (9) aperture (10) on a straight line; When reflection configuration was measured, flashlight received from aperture (11) collection that forms an angle with the ingate, enters fiber coupler then, is measured by optical fiber input spectrum instrument.
Owing to adopt said apparatus, the heated perimeter of sample can expand to 1200 ℃ of samples very thin (0.5mm is following) simultaneously, can adopt transmission and method for reflection to measure like this.In addition, because the sample on the specimen holder can be converted to solid-state from the solid state transformation to the liquid state in the heating and cooling process of high temperature furnace again from liquid state.Like this can by regulate with control high-temperature heating equipment stove in temperature reach the solid-liquid purpose of the real-time spectrum measurement of structural change in the transition process mutually.In addition, owing in internal furnace, filled foamed brick (a kind of fire resistive material of porous) around the specimen holder, alleviated the influence of heat radiation significantly to spectrum test.
Accompanying drawing 1 is the high-temperature sample heating furnace longitudinal profile synoptic diagram that is used for real-time spectrum measurement.
Accompanying drawing 2 is heating furnace A-B position horizontal section synoptic diagram.
Embodiment 1: as shown in Figure 2, pump light focused on sample through high-temperature heating equipment aperture (9) when transmission configuration was measured, and infrared signal light and ingate (9) aperture (10) in a straight line of seeing through style are sent into the infrared spectrometer measurement with an optical system for collecting and fiber coupling system.Measuring samples is B
aB
2O
4(BBO), the specimen holder diameter is 5mm, and sample heating-up temperature scope is 800～1100 ℃.
Embodiment 2: as shown in Figure 2, pump light focused on sample through high-temperature heating equipment aperture (9) when reflection configuration was measured.The aperture (11) that the infrared signal light of reflection style and ingate (9) folder are 120 ° is sent into infrared spectrometer with an optical system for collecting and fiber coupling system and is measured.Measuring samples is B
aB
2O
4(BBO), the specimen holder diameter is 8mm, and sample heating-up temperature scope is 800～1200 ℃.
Claims (3)
1. the high-temperature sample heater of a real-time spectrum measurement, furnace shell (1) out, interior boiler tube (2), heating element (3), specimen holder (4), light hole (5), temperature-control heat couple (6), temperature thermocouple (7) and insulation material (8) are formed, and it is characterized in that also having in this device an end of a usefulness platinum filament to curve the specimen holder that ringlet is made, and this device can carry out solid, liquid attitude spectrum test in 400～1200 ℃ hot environment.
2. the high-temperature sample heater of real-time spectrum measurement as claimed in claim 1 is characterized in that having on the described furnace wall several and measures aperture.
3. the high-temperature sample heater of real-time spectrum measurement as claimed in claim 1 is characterized in that mentioning cooling after described sample is with platinum filament ringlet immersion sample liquation manufactures.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98115334 CN1116602C (en) | 1998-06-18 | 1998-06-18 | High-temperature sample heater for real-time spectrum measurement |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98115334 CN1116602C (en) | 1998-06-18 | 1998-06-18 | High-temperature sample heater for real-time spectrum measurement |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1239776A true CN1239776A (en) | 1999-12-29 |
| CN1116602C CN1116602C (en) | 2003-07-30 |
Family
ID=5224515
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 98115334 Expired - Fee Related CN1116602C (en) | 1998-06-18 | 1998-06-18 | High-temperature sample heater for real-time spectrum measurement |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1116602C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100422717C (en) * | 2004-05-11 | 2008-10-01 | 深圳大学 | Optical cryostat |
| CN102564955A (en) * | 2011-12-30 | 2012-07-11 | 浙江师范大学 | In-situ dual infrared spectrum pool |
| CN104914059A (en) * | 2015-06-04 | 2015-09-16 | 中国科学院上海应用物理研究所 | Absorption spectrometer |
| CN106918223A (en) * | 2015-12-25 | 2017-07-04 | 天津市维之丰科技有限公司 | A kind of electric furnace with spectral detection function |
| CN108072672A (en) * | 2017-12-14 | 2018-05-25 | 清华大学 | The on-Line Monitor Device and its monitoring method of a kind of ablation structure and morphology and product |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100353171C (en) * | 2004-12-23 | 2007-12-05 | 中国科学院半导体研究所 | Sample holder in use for measuring spectrum of photoluminescence of electrical modulation |
-
1998
- 1998-06-18 CN CN 98115334 patent/CN1116602C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100422717C (en) * | 2004-05-11 | 2008-10-01 | 深圳大学 | Optical cryostat |
| CN102564955A (en) * | 2011-12-30 | 2012-07-11 | 浙江师范大学 | In-situ dual infrared spectrum pool |
| CN104914059A (en) * | 2015-06-04 | 2015-09-16 | 中国科学院上海应用物理研究所 | Absorption spectrometer |
| CN106918223A (en) * | 2015-12-25 | 2017-07-04 | 天津市维之丰科技有限公司 | A kind of electric furnace with spectral detection function |
| CN108072672A (en) * | 2017-12-14 | 2018-05-25 | 清华大学 | The on-Line Monitor Device and its monitoring method of a kind of ablation structure and morphology and product |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1116602C (en) | 2003-07-30 |
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