CN102162793A - Raman system for high-pressure in situ measurement - Google Patents
Raman system for high-pressure in situ measurement Download PDFInfo
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- CN102162793A CN102162793A CN 201110001677 CN201110001677A CN102162793A CN 102162793 A CN102162793 A CN 102162793A CN 201110001677 CN201110001677 CN 201110001677 CN 201110001677 A CN201110001677 A CN 201110001677A CN 102162793 A CN102162793 A CN 102162793A
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Abstract
The invention discloses a simple and effective Raman system for high-pressure in situ measurement, comprising a laser light source, a laser transmission light path, a Raman signal stimulating, collecting and transmitting light path, a microscopic observation light path and Raman signal detecting and processing equipment. According to the Raman system for high-pressure in situ measurement, the problems of big stray signal interference, high fluorescence background and small possibility of measuring singles of low wave number in the high-pressure Raman test environment can be overcome. The application of a Raman spectrum in the high-pressure science is widened, and a test means for analyzing layered samples is provided. The simple and effective Raman system has a good application prospect.
Description
Technical field
The present invention relates to a kind of Raman system, relate in particular to a kind of Raman system that is used for carrying out the situ high pressure measurement at adamas opposed anvils (DAC).
Background technology
Traditional Raman system is to the comparative maturity of the raman spectroscopy measurement technology under the sample normal temperature and pressure, and to high pressure (tens to millions of atmospheric pressure) the raman spectroscopy measurement difficulty relatively of sample down.This is that used sample size is (micron order) seldom owing to sample in the high pressure research is to be contained in adamas opposed anvils the inside, and adamas has absorption and can produce the fluorescence back of the body end.Obtain the high Raman spectrum of quality under the sample high pressure, Raman system is had some specific (special) requirements: the laser focusing hot spot must be enough little; Inhibition ability to fluorescence and parasitic light is eager to excel; Spectrometer will possess very high resolution; To monitoring intuitive and convenient of sample state etc.Traditional commercial Raman spectroscopy is difficult to satisfy above-mentioned requirements simultaneously, thereby it is very difficult to obtain the measurement of Raman spectrum under the sample high pressure.
Summary of the invention
Disturb big in order to overcome in the high pressure Raman test environment spurious signal, the problem of fluorescence back of the body end height and lower wave number signal measurement difficulty, the invention provides a kind of simple and effective situ high pressure and measure Raman system, it comprises the detection and the treatment facility that excite, collect and transmit light path, microexamination light path and Raman signal of LASER Light Source, Laser Transmission light path, Raman signal, wherein, exciting, collecting and transmit usage space wave filter and holographic notch filters in the light path at Raman signal.In the system, LASER Light Source is an Argon ion laser; Spatial filter comprises the achromat of two same model and places the confocal pinhole of their centers; The micro-imaging observation optical path comprises white light source, semi-transparent semi-reflecting lens, collector lens, camera and display screen; The detection of Raman signal and treatment facility comprise spectrometer, ccd detector and computing machine.
Situ high pressure of the present invention is measured Raman system and is had very high three-dimensional resolution characteristic, can do optical section to some samples.The present invention not only be Raman spectrum in high-pressure science application extension channel, and provide a kind of means of testing of analyzing the stratiform sample, have good application prospects.
Description of drawings
Fig. 1 is the design concept figure of Raman system of the present invention.
Fig. 2 is the design concept figure of Raman system spatial filter of the present invention.
The HfO of Fig. 3 for using Raman system of the present invention to obtain
2The high pressure Raman spectrum.
The Gd of Fig. 4 for using Raman system of the present invention to obtain
2O
3Raman spectrum.
Fig. 5 obtains Dy for using Raman system of the present invention
2O
3Raman spectrum.
Fig. 6 is Nd under the different pressures that uses Raman system of the present invention and obtain
2O
3Raman spectrum.
Embodiment
In order to make those skilled in the art can clearer understanding the present invention, the present invention will be further described by embodiment below in conjunction with accompanying drawing.
Disturb big in order to overcome in the high pressure Raman test environment spurious signal, problems such as fluorescence back of the body end height and lower wave number signal measurement difficulty, the invention provides a kind of situ high pressure raman spectroscopy measurement instrument, the detection and the treatment facility that excite, collect and transmit light path, micro-imaging observation optical path and Raman signal that comprise Laser Transmission light path, Raman signal, wherein in the collection of Raman signal and transmission light path, introduce spatial filter and holographic notch filters, overcome the interference of the fluorescence back of the body end and spurious signal.
As shown in Figure 1, situ high pressure Raman system 1 of the present invention comprises following components:
1. LASER Light Source and Laser Transmission light path
The Laser Transmission light path is meant that laser instrument is exported to this section of complex objective lens light path.LASER Light Source 2 adopts Argon ion laser as excitation source.Laser beam expands bundle through beam expander 3, and the angle of divergence is reduced, and spot diameter increases, and then through catoptron 4 break-in vertical incidence forward (FWD) bandpass filters (band pass filter) 5, shoot laser is on complex objective lens 6 focuses on sample 7 among the DAC.
2. Raman signal excites, collects and transmit light path
Exciting, collect and transmitting light path of Raman signal is meant that complex objective lens 6 is to this a part of light path of spectrometer entrance slit, comprising complex objective lens 6, spatial filter 8 and holographic notch filter plate 9.Laser focuses on the sample 7 through complex objective lens 6, inspires Raman diffused light.Scattered light becomes directional light after collecting via same complex objective lens 6, then via being focused to spectrometer 11 entrance slits by collector lens 10 after the spatial filter 8 filtering spurious signals.Spatial filter 8 is by the achromat of two same model and places the confocal pinhole of their centers to constitute, in order to the filtering fluorescence back of the body end and parasitic light.The holographic notch filter plate 9 that adopts in the light path can be eliminated Rayleigh scattering.
As shown in Figure 2, confocal pinhole (pinhole) is positioned on the focus of achromat, be slightly larger than sample in aperture place picture point size as long as choose the size of aperture, just can guarantee only to come from signal that object focal point place sample produces fully by aperture, and can not pass through aperture with the signal and the parasitic light signal of sample generation afterwards before the focus.Therefore, by the mode of this spatial filtering, the signal that can guarantee to arrive detector come from sample certain a bit, whole device has very high longitudinal frame.Owing to laser focusing hot spot very little (less than 3 microns), the lateral resolution of device is also very high again, and therefore, She Ji spectral measurement system has high dimensional resolution like this.Can carry out the pointwise detection analysis to the stratiform sample.
3. microexamination light path
The microexamination light path comprises the white light source (not shown), semi-transparent semi-reflecting lens 12, and collector lens 13, camera (ccd camera) 14 and display screen 15 can be monitored at any time to sample state.Because laser facula is very little, want to find the sample well of tens microns sizes in the diamond anvil, must sample state clearly be presented on the screen by the micro-imaging observation optical path.
4. the detection of Raman signal and treatment facility
The detection of Raman signal and treatment facility comprise spectrometer 11, ccd detector 16 and computing machine (not shown).The collimator objective that enters the Raman diffused light process spectrometer inside of spectrometer 11 entrance slits collimates the back by the 1800g/mm grating beam splitting, is then received by ccd detector 16.The signal that detector receives is handled by terminal through a series of amplifications and conversion back, realizes operation automatically.
The HfO of Fig. 3 for using Raman system of the present invention to obtain
2The high pressure Raman spectrum, show that this device can obtain high-resolution (2cm under the sample high pressure
-1), the Raman spectrum of high s/n ratio.The Gd of Fig. 4 for using Raman system of the present invention to obtain
2O
3Raman spectrum, show that device can survey minimum wave number to 90cm
-1Fig. 5 obtains Dy for using Raman system of the present invention
2O
3Raman spectrum, the arrow indication is the parasitic light signal among the figure, as can be seen from Figure 5, add spatial filter after, can effectively reduce the sample Raman spectrum at the bottom of near the back of the body the lower wave number, can effectively suppress the parasitic light signal simultaneously.Fig. 6 is Nd under the different pressures that uses Raman system of the present invention and obtain
2O
3Raman spectrum, can see when pressure reaches 400,000 atmospheric pressure, utilize this device still can obtain good Raman spectrum.
Situ high pressure of the present invention is measured Raman system and is had very high three-dimensional resolution characteristic, can do optical section to some samples.This invention not only be Raman spectrum in high-pressure science application extension channel, and provide a kind of means of testing of analyzing the stratiform sample, have good application prospects.In addition, the machinery of total system and Heat stability is good, debugging, operation and maintenance are conveniently.
Claims (3)
1. a situ high pressure is measured Raman system, it comprises LASER Light Source, the Laser Transmission light path, exciting of Raman signal, collect and the transmission light path, the detection of microexamination light path and Raman signal and treatment facility, it is characterized in that, exciting of described Raman signal, usage space wave filter and holographic notch filters in collection and the transmission light path, described LASER Light Source is an Argon ion laser, described spatial filter comprises the achromat of two same model and places the confocal pinhole of their centers, described microexamination light path comprises white light source, semi-transparent semi-reflecting lens, collector lens, camera and display screen, the detection and the treatment facility of described Raman signal comprise spectrometer, ccd detector and computing machine.
2. situ high pressure as claimed in claim 1 is measured Raman system, it is characterized in that, the sample that described Raman system is measured is arranged in high-tension unit.
3. situ high pressure as claimed in claim 2 is measured Raman system, it is characterized in that described high-tension unit is the adamas opposed anvils.
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| CN 201110001677 CN102162793A (en) | 2011-01-06 | 2011-01-06 | Raman system for high-pressure in situ measurement |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507529A (en) * | 2011-09-26 | 2012-06-20 | 中国科学院半导体研究所 | Microscopic confocal Raman spectrometer |
| CN104316507A (en) * | 2014-10-14 | 2015-01-28 | 上海交通大学 | Raman signal detection system and method |
| CN106198463A (en) * | 2015-04-30 | 2016-12-07 | 中国科学院苏州纳米技术与纳米仿生研究所 | Spectrum scan test device and method of testing thereof |
| CN106940311A (en) * | 2017-05-03 | 2017-07-11 | 重庆大学 | The in-situ detection method of fault characteristic gases is dissolved in a kind of transformer oil |
| CN109425572A (en) * | 2017-08-30 | 2019-03-05 | 三星电子株式会社 | Collection optical system and Raman spectrum system for spectrometer |
| CN109596598A (en) * | 2019-01-07 | 2019-04-09 | 武汉大学 | A kind of portable mono wavelength Raman photometer based on SERS |
| CN112834480A (en) * | 2020-12-31 | 2021-05-25 | 中国科学院合肥物质科学研究院 | Confocal Raman system for high-pressure normal-temperature and low-temperature experiments and measurement method thereof |
| CN112945927A (en) * | 2021-01-18 | 2021-06-11 | 吉林大学 | In-situ high-pressure confocal Raman spectrum measurement system |
| CN114279836A (en) * | 2021-12-14 | 2022-04-05 | 北京高压科学研究中心 | Physical property characterization system and method based on dynamic loading |
-
2011
- 2011-01-06 CN CN 201110001677 patent/CN102162793A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 《中国优秀硕士学位论文全文数据库》 20080715 郝苇苇 《玻璃基微流控芯片的制作及原位拉曼检测》 第59-76页 1-3 , 第7期 * |
| 《光散射学报》 20080930 贾茹等 《一套高温高压原位拉曼散射_布里渊散射测量系统》 第213-214页 1-3 第20卷, 第3期 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507529A (en) * | 2011-09-26 | 2012-06-20 | 中国科学院半导体研究所 | Microscopic confocal Raman spectrometer |
| CN104316507A (en) * | 2014-10-14 | 2015-01-28 | 上海交通大学 | Raman signal detection system and method |
| CN106198463A (en) * | 2015-04-30 | 2016-12-07 | 中国科学院苏州纳米技术与纳米仿生研究所 | Spectrum scan test device and method of testing thereof |
| CN106940311A (en) * | 2017-05-03 | 2017-07-11 | 重庆大学 | The in-situ detection method of fault characteristic gases is dissolved in a kind of transformer oil |
| CN109425572A (en) * | 2017-08-30 | 2019-03-05 | 三星电子株式会社 | Collection optical system and Raman spectrum system for spectrometer |
| CN109596598A (en) * | 2019-01-07 | 2019-04-09 | 武汉大学 | A kind of portable mono wavelength Raman photometer based on SERS |
| CN112834480A (en) * | 2020-12-31 | 2021-05-25 | 中国科学院合肥物质科学研究院 | Confocal Raman system for high-pressure normal-temperature and low-temperature experiments and measurement method thereof |
| CN112834480B (en) * | 2020-12-31 | 2023-02-03 | 中国科学院合肥物质科学研究院 | Confocal Raman system for high-pressure normal-temperature and low-temperature experiments and measurement method thereof |
| CN112945927A (en) * | 2021-01-18 | 2021-06-11 | 吉林大学 | In-situ high-pressure confocal Raman spectrum measurement system |
| CN114279836A (en) * | 2021-12-14 | 2022-04-05 | 北京高压科学研究中心 | Physical property characterization system and method based on dynamic loading |
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Application publication date: 20110824 |