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CN109374528B - A spectrum measurement method under high pressure conditions - Google Patents

A spectrum measurement method under high pressure conditions Download PDF

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Publication number
CN109374528B
CN109374528B CN201811476394.2A CN201811476394A CN109374528B CN 109374528 B CN109374528 B CN 109374528B CN 201811476394 A CN201811476394 A CN 201811476394A CN 109374528 B CN109374528 B CN 109374528B
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anvil
pressure
sample
pressure plate
screw
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CN109374528A (en
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方英姿
张向平
方晓华
赵永建
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Jinhua Vocational And Technical University
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Jinhua Vocational And Technical University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65Raman scattering

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  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

本发明涉及材料研究领域,一种高压条件下的光谱测量方法,高压条件下的光谱测量装置包括上压力盘、下压力盘、调平螺丝、压力螺丝、顶砧限位螺丝、上支撑盘、下支撑盘、上顶砧、下顶砧、环形垫圈、压力媒介、样品、限位螺杆、光收集系统和激光器,能够在高压条件下研究样品的光谱特性,采用从上顶砧的冠部斜切面入射激光的方法,使得入射顶砧的激光和经过样品表面反射的激光分别通过顶砧的冠部斜切面进入和离开顶砧,使得激光在样品表面的入射角较大,更有效地过滤顶砧材料的光散射信号,从而使得顶砧的散射光与样品的散射光的分离度更高,样品散射信号的信噪比更大,无导轨结构来对顶砧施压,避免了由于部件松弛而造成的对样品施加压力的偏差。

The invention relates to the field of material research, and is a spectrum measurement method under high pressure conditions. The spectrum measurement device under high pressure conditions comprises an upper pressure plate, a lower pressure plate, a leveling screw, a pressure screw, an anvil limit screw, an upper support plate, a lower support plate, an upper anvil, a lower anvil, an annular gasket, a pressure medium, a sample, a limit screw, a light collection system and a laser. The spectrum characteristics of the sample can be studied under high pressure conditions. The method of incident laser from the crown bevel of the upper anvil is adopted, so that the laser incident on the anvil and the laser reflected by the sample surface enter and leave the anvil through the crown bevel of the anvil respectively, so that the incident angle of the laser on the sample surface is larger, and the light scattering signal of the anvil material is filtered more effectively, so that the separation degree of the scattered light of the anvil and the scattered light of the sample is higher, and the signal-to-noise ratio of the sample scattering signal is larger. There is no guide rail structure to apply pressure to the anvil, and the deviation of applying pressure to the sample caused by loose components is avoided.

Description

Spectrum measurement method under high pressure condition
Technical Field
The invention relates to the field of material research, in particular to a spectrum measuring method under high pressure condition for researching spectrum characteristics of a sample under high pressure condition.
Background
The research of the change of certain characteristics of the material along with the applied pressure has great significance, and the high-pressure spectrum measurement technology is a typical research method, such as the inelastic scattering technology of visible light including Raman scattering, and is very suitable for researching the dependence of the characteristics of the material on photon energy, magnetic interaction, plasma energy, electron energy band structure and superconductive energy gap, and the pressure is applied to a material sample to be measured by adopting a pressure applying device such as a top anvil and the like, and the material is measured by combining the spectrum technology. In particular, the high-pressure light scattering technology is widely adopted, and has the advantages that the solid angle of scattered light emitted from a sample can be collected is large, and the scattered light signal of the sample is strong. However, the prior art devices also suffer from the disadvantage that certain special materials of the prior art that are opaque and have weak scattering signals have difficulty in obtaining clear raman scattering spectra, particularly materials having spectral ranges that overlap with the single photon and two photon raman scattering spectra of the anvil material. The high-pressure spectrum measurement in the prior art generally adopts a supporting table combined with a diamond anvil, the supporting table is pressed along a fixed guide rail to apply pressure to a sample, the relaxation of the guide rail can cause small deviation of displacement, and the pressure deviation between the anvil is caused by uneven distribution of the pressure of the supporting table to the bottom surface of the anvil, so that the problem can be solved by the spectrum measurement method under the high-pressure condition.
Disclosure of Invention
In order to solve the above problems, an object of the present invention is to more effectively filter a light scattering signal of a anvil material, the method of the present invention allows laser light incident to the anvil and laser light reflected by the surface of a sample to enter and leave the anvil through a crown chamfer of the anvil, respectively, and in addition, the present invention applies pressure to the sample using a rail-free structure, thereby avoiding pressure deviation due to aging relaxation of components.
The technical scheme adopted by the invention is as follows:
The spectrum measuring device under the high pressure condition comprises an upper pressure disc, a lower pressure disc, a leveling screw, a pressure screw, an anvil limit screw, an upper support disc, a lower support disc, an upper anvil, a lower anvil, an annular gasket, a pressure medium, a sample, a limit screw, a light collecting system and a laser, wherein xyz is a three-dimensional space coordinate system, the names corresponding to all parts of a diamond standard cutting tool comprise a table top, a crown part, a waist part, a pavilion part and a bottom surface, the bottom surface of the upper anvil is downward, the bottom surface of the lower anvil is upward, the annular gasket is positioned between the bottom surface of the upper anvil and the bottom surface of the lower anvil, the annular gasket is provided with a pressure medium, a sample is positioned in the pressure medium, when high pressure is applied to the sample, the upper anvil and the lower anvil are mutually close, the pressure medium is applied to the sample, the area corresponding to light that can be collected by the light collecting system is called a light collecting area, the upper pressure disc and the lower pressure disc are all made of steel circles with the outer diameter of ten centimeters and are elastic, the upper pressure disc and the lower pressure disc are coaxially arranged in the vertical y direction, the upper pressure disc is provided with three screw holes, the upper pressure disc and the upper screw holes are uniformly distributed with the three screw holes 5M, the upper screw holes M and the lower screw holes M4 are uniformly distributed, the upper screw holes M4 are distributed at the three screw holes M4 are distributed, the upper screw holes M4 are distributed at the upper screw holes M4 and 3, the screw holes M4 are uniformly and 3M 4 are distributed, the screw holes 5, the screw holes are distributed at the upper screw holes 5M and 3M 4 are uniformly and 3, and 3M 4M and 3, 3 screw and 3. The upper surface of the lower pressure disc is provided with three uniformly distributed anvil limiting screws on the circumference of which the distance from the center is two centimeters, the upper support disc and the lower support disc are silicon carbide rings with the outer diameter of three centimeters, the light collecting system is positioned right above the center of the upper support disc, the upper support disc is nested in the upper pressure disc and fixedly connected with the upper support disc, the lower support disc is nested in the lower pressure disc, the lower support disc can be finely adjusted through the three anvil limiting screws, the relative position between the lower support disc and the lower pressure disc in the horizontal plane can be changed, the upper anvil and the lower anvil are processed by adopting diamond standard cutting, the included angle between the crown chamfer and the table surface is 40 degrees, the lower part of the inner side of the upper support disc is provided with a chamfer which is 40 degrees with the horizontal direction, the inner side chamfer of the lower support disc is in contact with the crown chamfer of the lower anvil which is 40 degrees with the horizontal direction, and the upper anvil can sequentially irradiate laser medium and the upper anvil can sequentially irradiate laser on the sample.
The method for spectrum measurement under high pressure comprises the following steps:
Placing an annular gasket on the bottom surface of a lower anvil, placing a pressure medium in the annular gasket, and placing a sample in the pressure medium;
Step two, three leveling screws and three pressure screws are adjusted to change the distance between the upper pressure disc and the lower pressure disc until the distance between the bottom surface of the upper anvil and the pressure medium on the bottom surface of the lower anvil is 100-150 micrometers;
Step three, adjusting three leveling screws to enable an upper pressure disc to be parallel to a lower pressure disc, enabling the bottom surface of an upper anvil and the bottom surface of a lower anvil to be parallel to the upper pressure disc and the lower pressure disc respectively, and fixing the positions of the three leveling screws by adopting limit screws;
Step four, adjusting three pressure screws to enable the central parts of the upper pressure disc and the lower pressure disc to generate slight elastic deflection bending so as to enable the upper anvil and the lower anvil to be continuously close until the pressure medium distance between the bottom surface of the upper anvil and the bottom surface of the lower anvil is 20 micrometers, and then adjusting three anvil limiting screws to enable the lower anvil to be subjected to position adjustment in the horizontal direction so as to enable the bottom surface of the upper anvil to be aligned with the bottom surface of the lower anvil;
fifthly, adjusting three pressure screws to enable the upper pressure disc and the lower pressure disc to be further biased to bend, so that the upper anvil can apply pressure to the sample through a pressure medium, wherein the pressure ranges from 5Gpa to 30Gpa;
step six, adjusting the light collecting system to make the light collecting area of the light collecting system be an inverted cone taking the sample as a vertex, wherein the typical value of the solid angle range is 10-30 degrees;
step seven, laser emitted by the laser enters from the crown oblique surface of the upper anvil at normal direction, and enters the sample after refraction is generated at the interface of the upper anvil and the pressure medium;
Step eight, part of scattered light generated by the sample under the action of laser and located in a light collecting area of the light collecting system enters the light collecting system;
and step nine, analyzing scattered light information of the sample acquired by the light collecting system for material characteristic research.
The beneficial effects of the invention are as follows:
The method can effectively and spatially separate the scattered light of the anvil from the scattered light of the sample, and can increase the signal to noise ratio of the scattered signal of the sample, so that the sufficiently strong scattered signal of the sample can be obtained without focusing laser on a smaller area on the sample, and the damage to the sample caused by the heat generation on the surface of the sample due to local laser can be avoided.
Drawings
The following is further described in connection with the figures of the present invention:
FIG. 1 is a schematic illustration of the present invention;
FIG. 2 is a schematic top view of an upper pressure plate;
FIG. 3 is an enlarged schematic view of the upper and lower anvils;
Fig. 4 is a schematic diagram of a diamond standard cut.
In the figure, 1, an upper pressure disk, 2, a lower pressure disk, 3, leveling screws, 4, pressure screws, 5, a top anvil limit screw, 6, an upper support disk, 7, a lower support disk, 8, an upper top anvil, 8-1, a table top, 8-2, a crown, 8-3, a lumbar plane, 8-4, a pavilion, 8-5, a bottom surface, 9, a lower top anvil, 10, an annular gasket, 11, a pressure medium, 12, a sample, 13, a limit screw, 14, a light collecting system, 15, and a laser.
Detailed Description
Fig. 1 is a schematic diagram of the invention, fig. 2 is a schematic diagram of an upper pressure plate in plan view, which comprises an upper pressure plate (1), a lower pressure plate (2), leveling screws (3), pressure screws (4), anvil limiting screws (5), an upper supporting plate (6), a lower supporting plate (7), an upper anvil (8), a lower anvil (9), an annular gasket (10), a pressure medium (11), a sample (12), a limiting screw (13), a light collecting system (14) and a laser (15), xyz is a three-dimensional space coordinate system, the upper pressure plate (1) and the lower pressure plate (2) are made of steel with ten cm outer diameter and are elastic, the upper pressure plate (1) and the lower pressure plate (2) are coaxially arranged in the vertical y direction, three uniformly distributed M5 screw holes are formed on the circumference of the upper pressure plate (1) with three uniformly distributed screw holes on the circumference of the center of three screw holes, limit screws (13) are formed on the side surfaces of each M4 screw hole, the lower pressure plate (2) is provided with three M5 screw holes corresponding to the three M5 screw holes, the upper pressure plate (1) and the lower pressure plate (2) are uniformly distributed on the circumference of the upper pressure plate (1) with three screw holes (4), the pressure screw (4) connects the lower pressure disc (2) with the upper pressure disc (1) through an M5 screw hole, the leveling screw (3) is an M4 screw and the top end of the leveling screw is conical, the leveling screw (3) passes through the M4 screw hole of the upper pressure disc (1) and the top end of the leveling screw is positioned in a conical groove of the lower pressure disc (2), three uniformly distributed anvil limiting screws (5) are arranged on the circumference of the upper surface of the lower pressure disc (2) which is two centimeters away from the center, the upper supporting disc (6) and the lower supporting disc (7) are silicon carbide circular rings with the outer diameter of three centimeters, the light collecting system (14) is positioned right above the center of the upper supporting disc (6), the area corresponding to the light which can be collected by the light collecting system (14) is called a light collecting area, the upper supporting disc (6) is nested in the upper pressure disc (1) and fixedly connected, the lower supporting disc (7) is nested in the lower pressure disc (2), the lower supporting disc (7) can be finely adjusted by three anvil limiting screws (5), the relative position between the lower supporting disc (7) and the lower pressure disc (2) in a horizontal plane can be changed, the upper anvil (8) and the lower anvil (9) are processed by adopting diamond standard cutting, and the upper supporting disc is provided with a table top (8-1), a crown (8-2), a waist surface (8-3), a pavilion (8-4) and a bottom surface (8-5), the included angle between the crown chamfer and the table top (8-1) is 40 degrees, the lower part of the inner side of the upper supporting disk (6) is provided with a chamfer which is 40 degrees with the horizontal direction, the inner side chamfer of the upper supporting disk (6) is contacted with the crown chamfer of the upper anvil (8), the upper part of the inner side of the lower supporting disk (7) is provided with a chamfer which is 40 degrees with the horizontal direction, the inner side chamfer of the lower supporting disk (7) is contacted with the crown chamfer of the lower anvil (9), and laser emitted by the laser (15) can be normally incident to the crown chamfer of the upper anvil (8) and sequentially enter the sample (12) through the upper anvil (8) and the pressure medium (11).
As shown in fig. 3, which is an enlarged schematic view of the upper anvil and the lower anvil, the bottom surface of the upper anvil (8) is downward, the bottom surface of the lower anvil (9) is upward, the ring gasket (10) is located between the bottom surface of the upper anvil (8) and the bottom surface of the lower anvil (9), the ring gasket (10) has a pressure medium (11), the sample (12) is located in the pressure medium (11), when a high pressure is applied to the sample (12), the upper anvil (8) and the lower anvil (9) are close to each other, and the pressure is applied to the sample (12) through the pressure medium (11), the high pressure range is 5GPa to 30GPa, and the area corresponding to the light that can be collected by the light collecting system (14) is called a light collecting area.
As shown in FIG. 4, the standard diamond cutter is schematically shown, and the names of each part of the standard diamond cutter are a table top (8-1), a crown (8-2), a waist (8-3), a pavilion (8-4) and a bottom (8-5).
The spectrum measuring device under the high pressure condition comprises an upper pressure disc (1), a lower pressure disc (2), a leveling screw (3), a pressure screw (4), a top anvil limit screw (5), an upper support disc (6), a lower support disc (7), an upper top anvil (8), a lower top anvil (9), an annular gasket (10), a pressure medium (11), a sample (12), a limit screw (13), a light collecting system (14) and a laser (15), xyz is a three-dimensional space coordinate system, and names corresponding to all parts of diamond standard cutting comprise a table top (8-1), a crown (8-2), a waist (8-3), a waist surface (8-3), The upper anvil (8-4) and the lower anvil (8-5) are arranged at the bottom surface of the upper anvil (8) downwards, the bottom surface of the lower anvil (9) is upwards, the bottom surface of the upper anvil (8) is downwards, the bottom surface of the lower anvil (9) is upwards, the annular gasket (10) is arranged between the bottom surface of the upper anvil (8) and the bottom surface of the lower anvil (9), the annular gasket (10) is provided with a pressure medium (11), the sample (12) is arranged in the pressure medium (11), when high pressure is applied to the sample (12), the upper anvil (8) and the lower anvil (9) are mutually close, the pressure is applied to the sample (12) through the pressure medium (11), the high pressure range is 5GPa to 30GPa, the area corresponding to the light which can be collected by the light collecting system (14) is called the light collecting area, the upper pressure disc (1) and the lower pressure disc (2) are all made of steel circular with the outer diameter of ten centimeters, the upper pressure disc (1) and the lower pressure disc (2) are coaxially arranged in the vertical y direction, the upper pressure disc (1) is provided with three screw holes (M) with three screw holes (5) which are uniformly distributed at the circumference (M) and three screw holes (5M) are distributed at the center (5M) and four sides (4) are distributed at the center (5M) of the screw holes (5M) are distributed uniformly and correspond with the M5 screw hole of the upper pressure disc (1), the upper surface of the lower pressure disc (2) is provided with three conical grooves which are uniformly distributed and correspond with the M4 screw hole of the upper pressure disc (1), the pressure screw (4) is an M5 screw, the pressure screw (4) connects the lower pressure disc (2) with the upper pressure disc (1) through the M5 screw hole, the leveling screw (3) is an M4 screw and the top end of the leveling screw is conical, and the leveling screw (3) is connected with the upper pressure disc (1) through the M4 screw hole of the upper pressure disc (1), The top end of the upper supporting disc is positioned in a conical groove of the lower pressure disc (2), three anvil limiting screws (5) which are uniformly distributed are arranged on the circumference of the upper surface of the lower pressure disc (2) which is two centimeters away from the center, the upper supporting disc (6) and the lower supporting disc (7) are all silicon carbide rings with the outer diameter of three centimeters, the light collecting system (14) is positioned right above the center of the upper supporting disc (6), the upper supporting disc (6) is nested in the upper pressure disc (1) and connected and fixed, the lower supporting disc (7) is nested in the lower pressure disc (2), the lower supporting disc (7) can be finely adjusted through the three anvil limiting screws (5), the relative position between the lower supporting disc (7) and the lower pressure disc (2) in the horizontal plane can be changed, and the upper anvil (8) and the lower anvil (9) are formed by diamond standard cutting, And has a table top (8-1), a crown (8-2), a waist surface (8-3), Pavilion (8-4) and bottom surface (8-5), the contained angle of crown chamfer and mesa (8-1) is 40 degrees, the inboard lower part of last supporting disk (6) has the chamfer that is 40 degrees with the horizontal direction, the inboard chamfer of last supporting disk (6) and the crown chamfer contact of last anvil (8), the inboard upper portion of lower supporting disk (7) has the chamfer that is 40 degrees with the horizontal direction, the inboard chamfer of lower supporting disk (7) and the crown chamfer contact of lower anvil (9), the laser beam that laser instrument (15) launched can be with normal incidence crown chamfer of last anvil (8) to through last anvil (8) and pressure medium (11) incident to sample (12) in proper order.
The invention relates to a principle of spatially separating scattered light of a diamond anvil and scattered light of a sample, which comprises the following steps:
The scattered light of the sample is mainly located in a range of about 45 degrees of solid angle perpendicular to the surface of the sample, while the scattered light of the diamond anvil is mainly concentrated in the light path of the laser entering the anvil and the vicinity of the light path of the laser in the anvil after being reflected by the surface of the sample, the laser enters from the crown chamfer of the diamond anvil, the incident angle on the surface of the sample is larger, the corresponding reflection angle is also larger, so that the scattered light and fluorescence of the diamond can be better separated from the scattered light of the sample, the refractive index of the pressure medium between the anvil and the sample is lower than that of the diamond, the refractive index of the laser beam in the process of leaving the anvil and entering the pressure medium is stronger, and the refractive angle is larger, as shown in fig. 3, so that the spatial separation between the scattered light of the diamond and the scattered light of the sample can be further increased.
It should be noted that since the angle at which the laser beam enters the diamond anvil and impinges on the diamond-pressure medium interface is greater than the critical angle of the diamond-air interface, the refractive index n p of the pressure medium cannot be too small, otherwise the laser beam will be totally reflected back into the anvil, on the other hand, in order to have a larger angle of refraction when the laser beam enters the pressure medium from the diamond, and to ensure that n p cannot be too large, a suitable value of n p needs to be chosen, n p typically being 1.4.
The method for spectrum measurement under high pressure comprises the following steps:
Firstly, placing an annular gasket (10) on the bottom surface of a lower anvil (9), placing a pressure medium (11) in the annular gasket (10), and placing a sample (12) in the pressure medium (11);
Step two, three leveling screws (3) and three pressure screws (4) are adjusted to change the distance between the upper pressure disc (1) and the lower pressure disc (2) until the distance between the bottom surface of the upper anvil (8) and the pressure medium (11) on the bottom surface of the lower anvil (9) is 100-150 micrometers;
Step three, adjusting three leveling screws (3) to enable an upper pressure disc (1) to be parallel to a lower pressure disc (2), enabling the bottom surface of an upper anvil (8) and the bottom surface of a lower anvil (9) to be parallel to the upper pressure disc (1) and the lower pressure disc (2) respectively, and fixing the positions of the three leveling screws (3) by adopting limit screws (13);
Step four, adjusting three pressure screws (4) to enable the central parts of the upper pressure disc (1) and the lower pressure disc (2) to generate slight elastic deflection bending so as to enable the upper top anvil (8) to be continuously close to the lower top anvil (9) until the distance between the bottom surface of the upper top anvil (8) and a pressure medium (11) on the bottom surface of the lower top anvil (9) is 20 micrometers, and then adjusting three top anvil limit screws (5) to adjust the position of the lower top anvil (9) in the horizontal direction so as to enable the bottom surface of the upper top anvil (8) to be aligned with the bottom surface of the lower top anvil (9);
Fifthly, adjusting three pressure screws (4) to enable the upper pressure disc (1) and the lower pressure disc (2) to be further biased to bend, so that the upper anvil (8) can apply pressure to the sample (12) through a pressure medium (11), wherein the pressure ranges from 5Gpa to 30Gpa;
Step six, adjusting the light collection system (14) so that the light collection area is an inverted cone with the sample as a vertex, and the typical value of the solid angle range is 10 to 30 degrees;
step seven, laser emitted by a laser (15) enters from a crown chamfer of the upper anvil (8) in normal direction, and enters the sample (12) after refraction is generated at the interface of the upper anvil (8) and the pressure medium (11);
step eight, a part of scattered light generated by the sample (12) under the action of laser light, which is positioned in a light collecting area of the light collecting system (14), enters the light collecting system (14);
And step nine, analyzing scattered light information of the sample (12) acquired by the light collecting system (14) for material characteristic research.
The invention adopts the method of incidence laser from the crown chamfer of the upper anvil, so that the incidence angle of the laser on the surface of the sample is larger, the separation degree of the scattered light of the anvil and the scattered light of the sample is higher, and the signal to noise ratio of the scattered signal of the sample is larger.

Claims (1)

1.一种高压条件下的光谱测量方法,高压条件下的光谱测量装置包括上压力盘(1)、下压力盘(2)、调平螺丝(3)、压力螺丝(4)、顶砧限位螺丝(5)、上支撑盘(6)、下支撑盘(7)、上顶砧(8)、下顶砧(9)、环形垫圈(10)、压力媒介(11)、样品(12)、限位螺杆(13)、光收集系统(14)和激光器(15),xyz为三维空间坐标系,金刚石标准切工的各部分对应的名称包括台面(8-1)、冠部(8-2)、腰面(8-3)、亭部(8-4)和底面(8-5),上顶砧(8)的底面向下,下顶砧(9)的底面向上,环形垫圈(10)位于上顶砧(8)的底面和下顶砧(9)的底面之间,环形垫圈(10)中具有压力媒介(11),样品(12)位于压力媒介(11)内,对样品(12)施加高压时,上顶砧(8)和下顶砧(9)相互靠近,并通过压力媒介(11)将压力施加到样品(12)上,高压范围5GPa到30GPa,光收集系统(14)能够收集的光对应的区域称为光收集区域;上压力盘(1)和下压力盘(2)均是外径为十厘米的钢制圆环形且具有弹性,上压力盘(1)与下压力盘(2)在竖直y方向同轴排列,上压力盘(1)距中心为三厘米的圆周上具有三个均布的M5螺孔,上压力盘(1)距中心为四厘米的圆周上具有三个均布的M4螺孔,每个所述M4螺孔的侧面均具有限位螺杆(13),下压力盘(2)具有三个均布的M5螺孔、且与上压力盘(1)的所述M5螺孔对应,下压力盘(2)上面具有三个均布的圆锥形凹槽、且与上压力盘(1)的所述M4螺孔对应,压力螺丝(4)为M5螺丝,压力螺丝(4)通过M5螺孔将下压力盘(2)与上压力盘(1)相连接,调平螺丝(3)为M4螺丝且其顶端为圆锥形,调平螺丝(3)通过上压力盘(1)的M4螺孔、且顶端位于下压力盘(2)的圆锥形凹槽内,在下压力盘(2)的上表面距中心为二厘米的圆周上安装有三个均布的顶砧限位螺丝(5),上支撑盘(6)和下支撑盘(7)均是外径为三厘米的碳化硅圆环,光收集系统(14)位于上支撑盘(6)中心的正上方,上支撑盘(6)嵌套于上压力盘(1)内并连接固定,下支撑盘(7)嵌套于下压力盘(2)内,下支撑盘(7)能够通过三个顶砧限位螺丝(5)来微调,能够改变下支撑盘(7)与下压力盘(2)之间在水平面内的相对位置,上顶砧(8)和下顶砧(9)均采用金刚石标准切工加工而成、且具有台面(8-1)、冠部(8-2)、腰面(8-3)、亭部(8-4)和底面(8-5),冠部斜切面与台面(8-1)的夹角为40度,上支撑盘(6)的内侧下部具有与水平方向呈40度的斜切面,上支撑盘(6)的内侧斜切面与上顶砧(8)的冠部斜切面接触,下支撑盘(7)的内侧上部具有与水平方向呈40度的斜切面,下支撑盘(7)的内侧斜切面与下顶砧(9)的冠部斜切面接触,激光器(15)发射的激光能够以法向入射上顶砧(8)冠部斜切面,并依次通过上顶砧(8)和压力媒介(11)入射到样品(12),压力媒介的折射率为1.4,1. A spectrum measurement method under high pressure conditions, wherein the spectrum measurement device under high pressure conditions comprises an upper pressure plate (1), a lower pressure plate (2), a leveling screw (3), a pressure screw (4), an anvil limit screw (5), an upper support plate (6), a lower support plate (7), an upper anvil (8), a lower anvil (9), an annular gasket (10), a pressure medium (11), a sample (12), a limit screw (13), a light collection system (14) and a laser (15), wherein xyz is a three-dimensional space coordinate system, and the names corresponding to the various parts of the diamond standard cut include a table (8-1), a crown (8-2), a girdle (8-3), a pavilion (8-4) and a bottom surface (8-5), the bottom surface of the upper anvil (8) is downward, and the bottom surface of the lower anvil (9) is upward, the annular gasket (10) is located between the bottom surface of the upper anvil (8) and the bottom surface of the lower anvil (9), and the annular gasket (10) contains the pressure medium (11), the sample (12) ) is located in the pressure medium (11). When high pressure is applied to the sample (12), the upper anvil (8) and the lower anvil (9) are close to each other and pressure is applied to the sample (12) through the pressure medium (11). The high pressure range is 5GPa to 30GPa. The area corresponding to the light that can be collected by the light collection system (14) is called the light collection area. The upper pressure plate (1) and the lower pressure plate (2) are both steel annular rings with an outer diameter of ten centimeters and are elastic. The upper pressure plate (1) and the lower pressure plate (2) are coaxially arranged in the vertical y direction. The upper pressure plate (1) has three evenly distributed M5 screw holes on a circumference three centimeters from the center. The upper pressure plate (1) has three evenly distributed M4 screw holes on a circumference four centimeters from the center. The side of each of the M4 screw holes has a limiting screw (13). The lower pressure plate (2) has three evenly distributed M5 screw holes corresponding to the M5 screw holes of the upper pressure plate (1). The lower pressure plate (2) has three The conical grooves are evenly distributed and correspond to the M4 screw holes of the upper pressure plate (1). The pressure screw (4) is an M5 screw. The pressure screw (4) connects the lower pressure plate (2) to the upper pressure plate (1) through the M5 screw holes. The leveling screw (3) is an M4 screw and its top end is conical. The leveling screw (3) passes through the M4 screw hole of the upper pressure plate (1) and its top end is located in the conical groove of the lower pressure plate (2). The upper surface of the lower pressure plate (2) is 1/8 of the distance from the center Three evenly spaced anvil limit screws (5) are installed on a 2 cm circumference. The upper support plate (6) and the lower support plate (7) are both silicon carbide rings with an outer diameter of 3 cm. The light collection system (14) is located directly above the center of the upper support plate (6). The upper support plate (6) is nested in the upper pressure plate (1) and connected and fixed. The lower support plate (7) is nested in the lower pressure plate (2). The lower support plate (7) can be fine-tuned by the three anvil limit screws (5) to change the lower pressure plate (2). The support plate (7) and the lower pressure plate (2) are in relative position in a horizontal plane. The upper anvil (8) and the lower anvil (9) are both made of diamond standard cutting and have a table (8-1), a crown (8-2), a waist (8-3), a pavilion (8-4) and a bottom (8-5). The angle between the crown bevel and the table (8-1) is 40 degrees. The inner lower part of the upper support plate (6) has a bevel at 40 degrees to the horizontal direction. The upper support plate (6) ) is in contact with the crown bevel of the upper anvil (8), the inner upper portion of the lower support plate (7) has a bevel at an angle of 40 degrees to the horizontal direction, the inner bevel of the lower support plate (7) is in contact with the crown bevel of the lower anvil (9), the laser emitted by the laser (15) can be incident on the crown bevel of the upper anvil (8) in a normal direction, and is incident on the sample (12) through the upper anvil (8) and the pressure medium (11) in turn, the refractive index of the pressure medium is 1.4, 其特征是:所述一种高压条件下的光谱测量方法的步骤:The characteristic is that: the steps of the spectrum measurement method under high pressure conditions are: 步骤一,将环形垫圈(10)置于下顶砧(9)的底面上,将压力媒介(11)置于环形垫圈(10)中,将样品(12)置于压力媒介(11)内;Step 1: placing an annular gasket (10) on the bottom surface of the lower anvil (9), placing a pressure medium (11) in the annular gasket (10), and placing a sample (12) in the pressure medium (11); 步骤二,调节三个调平螺丝(3)以及三个压力螺丝(4),以改变上压力盘(1)与下压力盘(2)之间的距离,直到上顶砧(8)的底面与下顶砧(9)底面上的压力媒介(11)之间距离为100至150微米;Step 2: Adjust the three leveling screws (3) and the three pressure screws (4) to change the distance between the upper pressure plate (1) and the lower pressure plate (2) until the distance between the bottom surface of the upper anvil (8) and the pressure medium (11) on the bottom surface of the lower anvil (9) is 100 to 150 microns; 步骤三,调节三个调平螺丝(3)使得上压力盘(1)与下压力盘(2)平行,且上顶砧(8)的底面及下顶砧(9)的底面也分别与上压力盘(1)及下压力盘(2)平行,然后采用限位螺杆(13)固定三个调平螺丝(3)的位置;Step 3: Adjust the three leveling screws (3) so that the upper pressure plate (1) is parallel to the lower pressure plate (2), and the bottom surface of the upper anvil (8) and the bottom surface of the lower anvil (9) are also parallel to the upper pressure plate (1) and the lower pressure plate (2), respectively, and then use the limit screw (13) to fix the position of the three leveling screws (3); 步骤四,调节三个压力螺丝(4)使得上压力盘(1)与下压力盘(2)的中心部分产生微小的弹性偏向弯曲,以使得上顶砧(8)与下顶砧(9)继续接近,直到上顶砧(8)底面与下顶砧(9)底面上的压力媒介(11)距离为20微米,然后调节三个顶砧限位螺丝(5)以在水平方向对下顶砧(9)进行位置调节,使得上顶砧(8)的底面与下顶砧(9)的底面对准;Step 4: Adjust the three pressure screws (4) so that the central parts of the upper pressure plate (1) and the lower pressure plate (2) produce a slight elastic deflection bend, so that the upper anvil (8) and the lower anvil (9) continue to approach each other, until the distance between the pressure medium (11) on the bottom surface of the upper anvil (8) and the bottom surface of the lower anvil (9) is 20 microns, and then adjust the three anvil limit screws (5) to adjust the position of the lower anvil (9) in the horizontal direction, so that the bottom surface of the upper anvil (8) is aligned with the bottom surface of the lower anvil (9); 步骤五,调节三个压力螺丝(4)使得上压力盘(1)与下压力盘(2)进一步偏向弯曲,使得上顶砧(8)能够通过压力媒介(11)对样品(12)施加压力,压力的范围为5Gpa到30Gpa;Step 5, adjusting the three pressure screws (4) to make the upper pressure plate (1) and the lower pressure plate (2) further deflect and bend, so that the upper anvil (8) can apply pressure to the sample (12) through the pressure medium (11), and the pressure range is 5 GPa to 30 GPa; 步骤六,调节光收集系统(14)使得其光收集区域是以样品为顶点的倒置圆锥体,立体角范围典型值为10到30度;Step 6, adjusting the light collection system (14) so that its light collection area is an inverted cone with the sample as the vertex, and the solid angle range is typically 10 to 30 degrees; 步骤七,激光器(15)发射的激光从上顶砧(8)的冠部斜切面以法向入射,并在上顶砧(8)与压力媒介(11)的界面产生折射后入射到样品(12);Step 7, the laser light emitted by the laser (15) is incident from the crown bevel surface of the upper anvil (8) in a normal direction, and is incident on the sample (12) after being refracted at the interface between the upper anvil (8) and the pressure medium (11); 步骤八,样品(12)在激光作用下产生的散射光中的位于光收集系统(14)的光收集区域中的部分进入光收集系统(14);Step eight, a portion of the scattered light generated by the sample (12) under the action of the laser and located in the light collection area of the light collection system (14) enters the light collection system (14); 步骤九,分析光收集系统(14)采集得到的样品(12)的散射光信息,用于材料特性研究。Step nine, analyzing the scattered light information of the sample (12) collected by the light collection system (14) for material property research.
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