CN202101940U - High-pressure in-situ measurement Raman system - Google Patents

High-pressure in-situ measurement Raman system Download PDF

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Publication number
CN202101940U
CN202101940U CN 201120002347 CN201120002347U CN202101940U CN 202101940 U CN202101940 U CN 202101940U CN 201120002347 CN201120002347 CN 201120002347 CN 201120002347 U CN201120002347 U CN 201120002347U CN 202101940 U CN202101940 U CN 202101940U
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China
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raman
pressure
laser
high pressure
utility
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Expired - Fee Related
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CN 201120002347
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Chinese (zh)
Inventor
刘景�
蒋升
李晓东
李延春
沈国寅
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Institute of High Energy Physics of CAS
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Institute of High Energy Physics of CAS
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Abstract

The utility model discloses a simple and effective high-pressure in-situ measurement Raman system, which comprises a laser light source, a laser transmission optical path, a Raman signal exciting, a collecting and transmitting optical path, a microexamination optical path, and a Raman signal detection and processing device. The system provided by the utility model solves the problems in a high-pressure Raman test environment, such as large disturbance caused by spurious signals, strong fluorescence background and difficulty in measuring low-wave-number signals, not only expanding a path for the application Raman spectrum to high-pressure science, but also providing a test measure for analyzing stratified samples. The system has a good application prospect.

Description

A kind of situ high pressure is measured raman system
Technical field
The utility model relates to a kind of raman system, relates in particular to a kind of raman system that is used for carrying out at adamas opposed anvils (DAC) the situ high pressure measurement.
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 the measurement of obtaining Raman spectrum under sample high pressure difficulty very.
The utility model content
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 utility model provides a kind of simple and effective situ high pressure to measure raman system; It comprises the detection and the treatment facility of the exciting of LASER Light Source, Laser Transmission light path, Raman signal, collection and delivery optics, microexamination light path and Raman signal; Wherein, usage space wave filter and holographic notch filters in the exciting of Raman signal, collection and delivery optics.In the system, high-tension unit is the adamas opposed anvils; LASER Light Source is to send the Argon ion laser that wavelength is 488 nanometers or 514.5 nanometer lasers; Spatial filter comprises the achromat and the confocal pinhole that places their centers of two same model; 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.
The situ high pressure of the utility model is measured raman system and is had very high three-dimensional resolution characteristic, can do optical section to some samples.The utility model be not merely Raman spectrum in high-pressure science application extension channel, and a kind of means of testing of analyzing the stratiform sample is provided, have good application prospects.
Description of drawings
Fig. 1 is the principle chart of the raman system of the utility model.
Fig. 2 is the principle chart of the raman system spatial filter of the utility model.
The HfO that Fig. 3 obtains for the raman system of using the utility model 2The high pressure Raman spectrum.
The Gd that Fig. 4 obtains for the raman system of using the utility model 2O 3Raman spectrum.
Fig. 5 obtains Dy for the raman system of using the utility model 2O 3Raman spectrum.
Nd under the different pressures that Fig. 6 obtains for the raman system of using the utility model 2O 3Raman spectrum.
Embodiment
In order to make those skilled in the art can clearer understanding the utility model, through embodiment the utility model be further specified 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 utility model provides a kind of situ high pressure raman spectroscopy measurement appearance; The detection and the treatment facility that comprise the exciting of Laser Transmission light path, Raman signal, collection and delivery optics, micro-imaging observation optical path and Raman signal; Wherein in the collection of Raman signal and delivery optics, 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, the situ high pressure raman system 1 of the utility model 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, excitation wavelength 488 nanometers or 514.5 nanometers.Laser beam expands bundle through beam expander 3, and the angle of divergence is reduced, and spot diameter increases, and through catoptron 4 break-in vertical incidence forward (FWD) bandpass filters (band pass filter) 5, shoot laser focuses on the sample in the high-tension unit 7 through complex objective lens 6 then.
2. the exciting of Raman signal, collection and delivery optics
The exciting of Raman signal, collection and delivery optics are meant this a part of light path of complex objective lens 6 to spectrometer entrance slit, comprising complex objective lens 6, spatial filter 8 and holographic notch filter plate 9.Laser focuses on the sample in the high-tension unit 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; As long as choose the size of aperture be slightly larger than sample at the aperture place picture point size; Just can guarantee only to come from signal that object focal point place sample produces fully through aperture, and before the focus and the signal and the parasitic light signal of sample generation afterwards can not pass through aperture.Therefore, through 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, the spectral measurement system of design 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 sample state at any time.Because laser facula is very little, want to find the sample well of 7 li tens microns sizes of high-tension unit, 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).By the 1800g/mm grating beam splitting, then received behind the collimator objective collimation of the Raman diffused light process spectrometer inside of entering spectrometer 11 entrance slits 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 that Fig. 3 obtains for the raman system of using the utility model 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 that Fig. 4 obtains for the raman system of using the utility model 2O 3Raman spectrum, show that device can survey minimum wave number to 90cm -1Fig. 5 obtains Dy for the raman system of using the utility model 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.Nd under the different pressures that Fig. 6 obtains for the raman system of using the utility model 2O 3Raman spectrum, can see when pressure reaches 400,000 atmospheric pressure, utilize this device still can obtain good Raman spectrum.
The situ high pressure of the utility model is measured raman system and is had very high three-dimensional resolution characteristic, can do optical section to some samples.This utility model be not merely Raman spectrum in high-pressure science application extension channel, and a kind of means of testing of analyzing the stratiform sample is provided, 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 the detection and the treatment facility of the exciting of LASER Light Source, Laser Transmission light path, Raman signal, collection and delivery optics, microexamination light path and Raman signal; It is characterized in that; Usage space wave filter and holographic notch filters in the exciting of said Raman signal, collection and delivery optics; Said LASER Light Source is to send the Argon ion laser that wavelength is 488 nanometers or 514.5 nanometer lasers; Said spatial filter comprises the achromat and the confocal pinhole that places their centers of two same model, and said microexamination light path comprises white light source, semi-transparent semi-reflecting lens, collector lens, camera and display screen, and the detection of said Raman signal and treatment facility 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 said 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 said high-tension unit is the adamas opposed anvils.
CN 201120002347 2011-01-06 2011-01-06 High-pressure in-situ measurement Raman system Expired - Fee Related CN202101940U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103592284A (en) * 2013-11-25 2014-02-19 电子科技大学 Online real-time representation device for film epitaxial growth
CN103674926A (en) * 2012-08-29 2014-03-26 日立视听媒体股份有限公司 Optical device

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103674926A (en) * 2012-08-29 2014-03-26 日立视听媒体股份有限公司 Optical device
CN103674926B (en) * 2012-08-29 2016-01-20 日立乐金光科技株式会社 Optical devices
US9297980B2 (en) 2012-08-29 2016-03-29 Hitachi-Lg Data Storage, Inc. Optical device for transmission-type scanning by moving scanning beam without moving observation sample
CN103592284A (en) * 2013-11-25 2014-02-19 电子科技大学 Online real-time representation device for film epitaxial growth
CN103592284B (en) * 2013-11-25 2015-08-26 电子科技大学 The online real-time characterization device of a kind of thin film epitaxial growth

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Granted publication date: 20120104

Termination date: 20140106