CN109444191B - Pulse laser heating high-pressure sample testing method - Google Patents
Pulse laser heating high-pressure sample testing method Download PDFInfo
- Publication number
- CN109444191B CN109444191B CN201811501107.9A CN201811501107A CN109444191B CN 109444191 B CN109444191 B CN 109444191B CN 201811501107 A CN201811501107 A CN 201811501107A CN 109444191 B CN109444191 B CN 109444191B
- Authority
- CN
- China
- Prior art keywords
- sample
- anvil
- laser
- light
- spectrometer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/20025—Sample holders or supports therefor
- G01N23/20033—Sample holders or supports therefor provided with temperature control or heating means
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/2005—Preparation of powder samples therefor
Landscapes
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention relates to the field of material property research, in particular to a high-pressure sample testing method heated by pulse laser, which comprises a lower supporting disc, a lower anvil, an upper supporting disc, a gasket, a Teflon ring, a sample, an achromatic lens I, a diaphragm, an achromatic lens II, an optical filter, a beam splitter I, a beam splitter II, a spectrometer, an oscilloscope, a photodiode, a signal generator, a laser, a beam splitter III, a reflecting mirror, a focusing lens, a photomultiplier and a camera.
Description
Technical Field
The invention relates to the field of material property research, in particular to a high-pressure sample testing method capable of carrying out stable heating and spectrum measurement on a sample under a high-pressure condition.
Background
The high pressure spectroscopic measurement technique is a typical research method, such as the technique including X-ray scattering, in which a pressure is applied to a sample of the material to be measured by a pressure applying device such as a anvil and the like, while the material is measured in combination with the spectroscopic technique, and in a general anvil device, the sample is placed in a pressure medium and a gasket, and then the anvil is pressed by a pressing device by applying pressure to the anvil through a support plate. Defect one of the prior art: when a sample under high pressure is subjected to spectrum measurement, particularly X-ray diffraction measurement, the opening of a supporting disc behind a top anvil is small, and the angles of incidence and emergence of X-rays are limited, so that the range of each parameter which can be measured by spectrum can be limited; the defects of the prior art are as follows: the common metal gasket can generate scattering effects such as parasitic Bragg scattering and the like under the X-ray, and attenuate the intensity of the X-ray, especially when the X-ray is incident at a larger angle, the attenuation is more serious, thereby influencing the signal-to-noise ratio of spectrum measurement; defects three in the prior art: some experiments require heating samples to a higher temperature, and the problems of unstable positions, uneven heating, hole burning and the like of the samples possibly occur in the heating method adopted in the prior art because the samples are positioned in gaskets between an upper anvil and a lower anvil and bear high pressure.
Disclosure of Invention
In order to solve the problems, the method adopts a special supporting disc structure to ensure that the incident angle of X-rays is larger, adopts materials with less scattering and absorption of the X-rays to fix the sample in the gasket, increases the stability of the sample and simultaneously can reduce the scattering and attenuation of the X-rays.
The technical scheme adopted by the invention is as follows:
the high-pressure sample testing device heated by the pulse laser comprises a lower supporting disc, a lower anvil, an upper supporting disc, a gasket, a Teflon ring, a sample, an achromatic lens I, a diaphragm, an achromatic lens II, a light filter, a beam splitter I, a beam splitter II, a spectrometer, an oscilloscope, a photodiode, a signal generator, a laser, a beam splitter III, a reflecting mirror, a focusing lens, a photomultiplier and a camera, wherein xyz is a three-dimensional space coordinate system, the output end of the photomultiplier is connected with the input end of the oscilloscope, the output end of the photodiode is connected with the input end of the oscilloscope, and the output end of the signal generator is connected with the trigger end of the laser; the achromatic lens I, the diaphragm, the achromatic lens II, the optical filter, the beam splitter I, the beam splitter II and the spectrometer are sequentially positioned right above the upper anvil and form an imaging light path, light emitted from the sample sequentially passes through the upper anvil, the achromatic lens I, the diaphragm, the achromatic lens II and the optical filter, reaches the beam splitter I and is divided into two identical beams of light, one beam of light enters the photomultiplier after being deflected and is converted into an electric signal to be input into the oscilloscope, the other beam of light propagates along the original path and is split again at the beam splitter II, wherein a part with the wavelength being larger than 760 nanometers enters the spectrometer, and the part with the wavelength being smaller than or equal to 760 nanometers enters the camera for carrying out thermal imaging on the sample; the light inlet of the spectrometer is provided with a shutter and a pinhole, the shutter can be controllably opened or closed, the position and the size of the pinhole can be adjusted to control the quantity of light entering the spectrometer and can be used for collimation of light beams, and the temperature of a sample can be calculated according to the thermal radiation recorded by the spectrometer; the laser, the beam splitter III, the reflecting mirror and the focusing lens form a heating laser light path, laser emitted by the laser is divided into two identical beams by the beam splitter III, one beam sequentially passes through the focusing lens and the upper anvil and is incident on a sample after being reflected by the reflecting mirror, and the other beam is incident on the photodiode after being deflected and is converted into an electric signal to be input into the oscilloscope; the lower anvil is in a decahedron shape and comprises an upper face, a lower face, four upper side faces and four lower side faces, wherein the upper face and the lower face are respectively parallel to a horizontal plane and are formed by cutting and processing a cubic diamond block with the length, the width and the height of 7 mm, 5 mm and 4 mm, the four upper side faces and the four lower side faces form an angle of 45 degrees with the horizontal plane, two lower side faces parallel to an x axis are defined as a lower side face I and a lower side face III, and two lower side faces parallel to a z axis are defined as a lower side face II and a lower side face IV; the upper anvil is in the shape of two upper round tables and lower round tables which are coaxially arranged up and down, and the lower bottom surface of the upper round table is coplanar with the upper bottom surface of the lower round table; the lower supporting disc and the upper supporting disc are hollow cylinders and are provided with an upper opening and a lower opening, the inner side of the lower opening of the upper supporting disc is provided with a truncated cone-shaped chamfer, and the truncated cone-shaped chamfer is contacted with the side surface of an upper truncated cone of the upper anvil; the inner side of the upper opening of the lower supporting disc is provided with two upper-side chamfer surfaces parallel to the x axis, the upper-side chamfer surfaces are respectively contacted with the lower side surface I and the lower side surface III of the lower top anvil, the upper opening of the lower supporting disc is not contacted with the lower side surface II and the lower side surface IV of the lower top anvil, incident light can sequentially pass through the lower opening of the lower supporting disc, the lower side surface II of the lower top anvil and the upper surface of the lower top anvil to shoot a sample, diffracted light formed after the interaction of the incident light and the sample can sequentially pass through the upper surface of the lower top anvil and the lower side surface IV of the lower top anvil and then shoot out from the lower opening of the lower supporting disc, the lower opening of the lower supporting disc is provided with two lower-side chamfer surfaces parallel to the z axis, the included angle between the two lower-side chamfer surfaces is 160 degrees, and the maximum included angle between the diffracted light which can shoot out through the lower opening of the lower supporting disc and the incident light is 160 degrees; the gasket is made of amorphous alloy based on zirconium metal, the Teflon ring is positioned in the gasket, and the sample is positioned in the Teflon ring; the lower support plate and the upper support plate are both made of silicon carbide; the lower anvil and the upper anvil are both made of diamond; the diameter of the upper bottom surface of the upper round table of the upper anvil is 3 mm, the diameter of the lower bottom surface is 4 mm, and the height is 0.5 mm; the diameter of the lower bottom surface of the upper anvil and the lower round table is 1 millimeter, and the height is 0.3 millimeter.
The pulse laser heating high-pressure sample testing method comprises the following steps:
step 1, applying pressure to a lower anvil and an upper anvil by using pressurizing equipment through a lower supporting disc and an upper supporting disc respectively, so that the pressure range of a sample is 2 to 8Gpa;
step 2, the laser emits continuous laser with the power of 0.8 to 2.4 milliwatts, and positions of a beam splitter III, a reflecting mirror and a focusing lens are adjusted so that the continuous laser irradiates the surface of a sample, and an optical image of the sample is recorded by a camera;
step 3, adjusting the laser to increase the power of continuous laser until the temperature change of a heating area on the surface of the sample can be detected through the spectrometer, and then collimating through a pinhole of a light inlet of the spectrometer, wherein a typical value of the temperature of the heating area is 2000K;
step 4, corresponding an optical image of the sample recorded by the camera to a thermal distribution image of the sample recorded by the spectrometer on a spatial scale;
step 5, keeping the collimated laser path unchanged, and adjusting the position of a focusing lens to defocus the laser incident to the sample so as to reduce the temperature gradient in a heating area on the surface of the sample and enable the diameter of the heating area to be 10 microns;
step 6, adjusting the pinhole size of a light inlet of the spectrometer and the position of the achromat I so that light entering the spectrometer is all from the range of 4 microns of the center radius of a heating area of the surface of the sample;
step 7, triggering a laser to emit pulse laser by adjusting a signal generator, wherein the typical value of single pulse time is 25 milliseconds, and setting the shutter opening time of a light inlet of a spectrometer to be 0.5 seconds after the start of the pulse laser so as to record the heat radiation of a sample heated by the single laser pulse and avoid the influence of other stray light;
and 8, carrying out an X-ray diffraction experiment, wherein X-rays are incident to the sample from the lower opening of the lower support disc, diffracted light generated by the sample is emitted from the lower opening of the lower support disc, and the diffracted light is detected by adopting a light detector, so that an X-ray diffraction signal spectrum of the sample is obtained.
The beneficial effects of the invention are as follows:
according to the method, the X-rays can be incident on the sample at a larger angle, and secondly, the Teflon ring is adopted on the outer side of the sample, so that the stability of the sample in the heating process is improved, the scattering and attenuation of nearby substances on the X-rays are reduced, and in addition, the laser pulse is adopted to heat the sample, so that the temperature of the sample can be kept relatively stable in millisecond time, and the signal-to-noise ratio of diffraction signals of the sample in X-ray diffraction measurement is increased.
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 an enlarged schematic view of the lower and upper anvils and lower and upper support plates;
FIG. 3 is a side view of FIG. 2;
FIG. 4 is a bottom view of the lower support plate and lower anvil;
fig. 5 is an enlarged schematic view of the lower anvil and the upper anvil.
In the figure, 1, lower support plate, 2, lower anvil, 3, upper anvil, 4, upper support plate, 5, gasket, 6, teflon ring, 7, sample, 8, achromatic lens I,9, stop, 10, achromatic lens II,11, filter, 12, beam splitter I,13, beam splitter II,14, spectrometer, 15, oscilloscope, 16, photodiode, 17, signal generator, 18, laser, 19, beam splitter III,20, mirror, 21, focusing lens, 22, photomultiplier, 23, camera.
Detailed Description
As shown in fig. 1, the invention is a schematic diagram, and comprises a lower supporting disc (1), a lower anvil (2), an upper anvil (3), an upper supporting disc (4), a gasket (5), a teflon ring (6), a sample (7), an achromatic lens I (8), a diaphragm (9), an achromatic lens II (10), an optical filter (11), a beam splitter I (12), a beam splitter II (13), a spectrometer (14), an oscilloscope (15), a photodiode (16), a signal generator (17), a laser (18), a beam splitter III (19), a reflecting mirror (20), a focusing lens (21), a photomultiplier tube (22) and a camera (23), wherein xyz is a three-dimensional space coordinate system, the output end of the photomultiplier tube (22) is connected with the input end of the oscilloscope (15), the output end of the photodiode oscilloscope (16) is connected with the input end of the oscilloscope (15), and the output end of the signal generator (17) is connected with the triggering end of the laser (18); the optical imaging device comprises an achromatic lens I (8), a diaphragm (9), an achromatic lens II (10), an optical filter (11), a beam splitter I (12), a beam splitter II (13) and a spectrometer (14), which are sequentially positioned right above an upper anvil (3) and form an imaging optical path, light emitted from a sample (7) sequentially passes through the upper anvil (3), the achromatic lens I (8), the diaphragm (9), the achromatic lens II (10) and the optical filter (11), reaches the beam splitter I (12) and is divided into two identical beams of light, one beam of light enters a photomultiplier (22) after being deflected and is converted into an electric signal to be input into an oscilloscope (15), the other beam of light propagates along an original path and is divided again at the beam splitter II (13), wherein a part with the wavelength longer than 760 nanometers enters the spectrometer (14) and a part with the wavelength less than or equal to 760 nanometers enters a camera (23) for carrying out thermal imaging on the sample (7); the light inlet of the spectrometer (14) is provided with a shutter and a pinhole, the shutter can be controllably opened or closed, the position and the size of the pinhole can be adjusted to control the quantity of light entering the spectrometer (14) and can be used for collimation of light beams, and the temperature of the sample (7) can be calculated according to the thermal radiation recorded by the spectrometer (14); the laser (18), the beam splitter III (19), the reflecting mirror (20) and the focusing lens (21) form a heating laser light path, laser light emitted by the laser (18) is divided into two identical beams by the beam splitter III (19), one beam passes through the focusing lens (21) and the upper anvil (3) in sequence after being reflected by the reflecting mirror (20) and is incident on the sample (7), and the other beam is deflected, then is emitted onto the photodiode (16) and is converted into an electric signal to be input into the oscilloscope (15); the lower supporting disc (1) and the upper supporting disc (4) are made of silicon carbide, the lower top anvil (2) and the upper top anvil (3) are made of diamond, the lower top anvil (2) is in a decahedron shape and comprises an upper face, a lower face, four upper side faces and four lower side faces, the lower top anvil is formed by cutting a cubic diamond block with the length, the width and the height of 7 mm, 5 mm and 4 mm respectively, the upper face and the lower face are parallel to a horizontal plane, the four upper side faces and the four lower side faces form an angle of 45 degrees with the horizontal plane, two lower side faces parallel to an x axis are defined as a lower side face I and a lower side face III, and two lower side faces parallel to a z axis are defined as a lower side face II and a lower side face IV; the upper anvil (3) is in the shape of two upper circular tables and lower circular tables which are coaxially arranged up and down, the lower bottom surface of the upper circular table is coplanar with the upper bottom surface of the lower circular table, the diameter of the upper bottom surface of the upper circular table of the upper anvil (3) is 3 mm, the diameter of the lower bottom surface is 4 mm, and the height is 0.5 mm; the diameter of the lower bottom surface of the lower round table of the upper anvil (3) is 1 mm, and the height is 0.3 mm.
Fig. 2 is an enlarged schematic view of the lower anvil and the upper anvil and the lower support plate and the upper support plate, fig. 3 is a side view of fig. 2, fig. 4 is a bottom view of the lower support plate and the lower anvil, the lower support plate (1) and the upper support plate (4) are hollow cylinders and have an upper opening and a lower opening, the inner side of the lower opening of the upper support plate (4) is provided with a truncated cone-shaped chamfer, and the truncated cone-shaped chamfer is contacted with the side surface of the upper truncated cone of the upper anvil (3); the inside of the upper opening of the lower supporting disc (1) is provided with two upper side chamfer surfaces parallel to the x axis, the upper side chamfer surfaces are respectively contacted with the lower side surface I and the lower side surface III of the lower top anvil (2), the upper opening of the lower supporting disc (1) is not contacted with the lower side surface II and the lower side surface IV of the lower top anvil (2), incident light can sequentially pass through the lower opening of the lower supporting disc (1), the lower side surface II of the lower top anvil (2) and the upper surface of the lower top anvil (2) to shoot a sample (7), diffracted light formed after the interaction of the incident light and the sample (7) can sequentially pass through the upper surface of the lower top anvil (2) and the lower side surface IV of the lower top anvil (2) to be shot from the lower opening of the lower supporting disc (1), the lower opening of the lower supporting disc (1) is provided with two lower side chamfer surfaces parallel to the z axis, an included angle between the two lower chamfer surfaces is 160 degrees, and the maximum incident angle between the diffracted light and the light which can be shot through the lower opening of the lower supporting disc (1) is 160 degrees.
As fig. 5 is an enlarged schematic view of the lower anvil and the upper anvil, the gasket (5) is made of amorphous alloy based on zirconium metal, the teflon ring (6) is located inside the gasket (5), and the sample (7) is located inside the teflon ring (6).
The high-pressure sample testing device heated by the pulse laser comprises a lower supporting disc (1), a lower anvil (2), an upper anvil (3), an upper supporting disc (4), a gasket (5), a Teflon ring (6), a sample (7), an achromatic lens I (8), a diaphragm (9), an achromatic lens II (10), an optical filter (11), a beam splitter I (12), a beam splitter II (13), a spectrometer (14), an oscilloscope (15), a photodiode (16), a signal generator (17), a laser (18), a beam splitter III (19), a reflecting mirror (20), a focusing lens (21), a photomultiplier tube (22) and a camera (23), wherein xyz is a three-dimensional space coordinate system, the output end of the photomultiplier tube (22) is connected with the input end of the oscilloscope (15), the output end of the photodiode (16) is connected with the input end of the oscilloscope (15), and the output end of the signal generator (17) is connected with the trigger end of the laser (18); the optical imaging device comprises an achromatic lens I (8), a diaphragm (9), an achromatic lens II (10), an optical filter (11), a beam splitter I (12), a beam splitter II (13) and a spectrometer (14), which are sequentially positioned right above an upper anvil (3) and form an imaging optical path, light emitted from a sample (7) sequentially passes through the upper anvil (3), the achromatic lens I (8), the diaphragm (9), the achromatic lens II (10) and the optical filter (11), reaches the beam splitter I (12) and is divided into two identical beams of light, one beam of light enters a photomultiplier (22) after being deflected and is converted into an electric signal to be input into an oscilloscope (15), the other beam of light propagates along an original path and is divided again at the beam splitter II (13), wherein a part with the wavelength longer than 760 nanometers enters the spectrometer (14) and a part with the wavelength less than or equal to 760 nanometers enters a camera (23) for carrying out thermal imaging on the sample (7); the light inlet of the spectrometer (14) is provided with a shutter and a pinhole, the shutter can be controllably opened or closed, the position and the size of the pinhole can be adjusted to control the quantity of light entering the spectrometer (14) and can be used for collimation of light beams, and the temperature of the sample (7) can be calculated according to the thermal radiation recorded by the spectrometer (14); the laser (18), the beam splitter III (19), the reflecting mirror (20) and the focusing lens (21) form a heating laser light path, laser light emitted by the laser (18) is divided into two identical beams by the beam splitter III (19), one beam passes through the focusing lens (21) and the upper anvil (3) in sequence after being reflected by the reflecting mirror (20) and is incident on the sample (7), and the other beam is deflected, then is emitted onto the photodiode (16) and is converted into an electric signal to be input into the oscilloscope (15); the lower anvil (2) is in a decahedron shape and comprises an upper surface, a lower surface, four upper side surfaces and four lower side surfaces, wherein the upper surface and the lower surface are parallel to a horizontal plane and are respectively formed by cutting and processing a cubic diamond block with the length, the width and the height of 7 mm, 5 mm and 4 mm, the four upper side surfaces and the four lower side surfaces form an angle of 45 degrees with the horizontal plane, two lower side surfaces parallel to an x axis are defined as a lower side surface I and a lower side surface III, and two lower side surfaces parallel to a z axis are defined as a lower side surface II and a lower side surface IV; the upper anvil (3) is in the shape of two upper round tables and lower round tables which are coaxially arranged up and down, and the lower bottom surface of the upper round table is coplanar with the upper bottom surface of the lower round table; the lower supporting disc (1) and the upper supporting disc (4) are hollow cylinders and are provided with an upper opening and a lower opening, the inner side of the lower opening of the upper supporting disc (4) is provided with a truncated cone-shaped chamfer, and the truncated cone-shaped chamfer is contacted with the side surface of the upper truncated cone of the upper anvil (3); the inner side of the upper opening of the lower supporting disc (1) is provided with two upper-side chamfer surfaces parallel to the x axis, the upper-side chamfer surfaces are respectively contacted with the lower side surface I and the lower side surface III of the lower top anvil (2), the upper opening of the lower supporting disc (1) is not contacted with the lower side surface II and the lower side surface IV of the lower top anvil (2), incident light can sequentially pass through the lower opening of the lower supporting disc (1), the lower side surface II of the lower top anvil (2) and the upper surface of the lower top anvil (2) to shoot a sample (7), diffracted light formed after the interaction of the incident light and the sample (7) can sequentially pass through the upper surface of the lower top anvil (2) and the lower side surface IV of the lower top anvil (2) to shoot out from the lower opening of the lower supporting disc (1), the lower opening of the lower supporting disc (1) is provided with two lower-side chamfer surfaces parallel to the z axis, the included angle between the two lower-side chamfer surfaces is 160 degrees, and the maximum incident angle between the diffracted light which can shoot out through the lower opening of the lower supporting disc (1) is 160 degrees; the gasket (5) is made of amorphous alloy based on zirconium metal, the Teflon ring (6) is positioned in the gasket (5), and the sample (7) is positioned in the Teflon ring (6); the lower support disc (1) and the upper support disc (4) are both made of silicon carbide; the lower anvil (2) and the upper anvil (3) are both made of diamond; the diameter of the upper bottom surface of the upper round table of the upper anvil (3) is 3 mm, the diameter of the lower bottom surface is 4 mm, and the height is 0.5 mm; the diameter of the lower bottom surface of the lower round table of the upper anvil (3) is 1 mm, and the height is 0.3 mm.
The device has the principle of larger diffraction light angle detection range in the X-ray diffraction experiment:
in the process of carrying out an X-ray diffraction experiment, X-rays are incident to a sample (7) from a lower opening of a lower supporting disc (1), a light detector detects diffraction light generated by the sample (7) emitted from the lower opening of the lower supporting disc (1), particularly, under the condition that the X-rays sequentially pass through the lower opening of the lower supporting disc (1), the lower side face II of a lower top anvil (2) and the upper face of the lower top anvil (2) to be emitted to the sample (7), the diffraction light formed after the incident X-rays interact with the sample (7) sequentially passes through the upper face of the lower top anvil (2) and the lower side face IV of the lower top anvil (2) and then is emitted from the lower opening of the lower supporting disc (1), and the included angle between two lower side inclined planes of the lower top anvil (2) is 160 degrees, so that the maximum included angle between the diffraction light emitted through the lower opening of the lower supporting disc (1) and the light detector and the incident light is 160 degrees by adjusting the incident position of the X-rays. Thereby solving the first disadvantage of the prior art.
Principle of the device of the invention for reducing scattering and attenuation of X-rays:
the Teflon material has weaker scattering of X rays and higher transmittance of the X rays, so that the Teflon ring (6) in the gasket (5) can greatly reduce scattering and attenuation of the incident X rays by elements around the sample in an X-ray diffraction experiment, on one hand, the signal of the scattering of the X rays acquired by the detector is reduced, and on the other hand, the X-ray diffraction signal of the sample is increased, and therefore the signal to noise ratio is greatly increased. Thereby solving the second drawback of the prior art.
The principle that the stability of the sample (7) is higher in the heating process of the device under the high pressure condition is as follows:
the Teflon material has good processability, the Teflon ring (6) can be tightly combined with the sample (7) and the gasket (5), the gasket (5) is made of amorphous alloy based on zirconium metal, so that the Teflon material has good plasticity and high tensile strength, the gasket (5) can be integrally deformed under high pressure, the sample (7) is not easy to be punched out of the gasket (5) in the process of pressure or temperature change, and the stability of the sample (7) in the experimental process is increased. In addition, the device adopts pulse laser to heat the sample (7), so that the temperature of the sample (7) can be kept relatively stable in millisecond time. Thereby solving the third disadvantage of the prior art.
The pulse laser heating high-pressure sample testing method comprises the following steps:
step 1, a pressurizing device is adopted to respectively apply pressure to a lower anvil (2) and an upper anvil (3) through a lower supporting disc (1) and an upper supporting disc (4), so that the pressure range of a sample (7) is 2 to 8Gpa;
step 2. A laser (18) emits a continuous laser with a power of 0.8 to 2.4 milliwatts and adjusts the positions of a beam splitter III (19), a mirror (20) and a focusing lens (21) so that the continuous laser irradiates the surface of the sample (7) and an optical image of the sample (7) is recorded by a camera (23);
step 3, adjusting the laser (18) to increase the power of the continuous laser until the temperature change of a heating area on the surface of the sample (7) can be detected by the spectrometer (14), and then collimating the sample through a pinhole of a light inlet of the spectrometer (14), wherein a typical value of the temperature of the heating area is 2000K;
step 4, corresponding an optical image recorded by a camera (23) on a spatial scale to a thermal distribution image recorded by a spectrometer (14) of the sample (7);
step 5, keeping the collimated laser path unchanged, and adjusting the position of a focusing lens (21) to defocus laser incident to the sample (7) so as to reduce the temperature gradient in a heating area on the surface of the sample (7) and make the diameter of the heating area be 10 microns;
step 6, adjusting the pinhole size of the light inlet of the spectrometer (14) and the position of the achromat I (8) so that the light entering the spectrometer (14) comes from the range that the center radius of the heating area of the surface of the sample (7) is 4 microns;
step 7, triggering a laser (18) by adjusting a signal generator (17) to emit pulse laser, wherein the typical value of single pulse time is 25 milliseconds, and setting the shutter opening time of a light inlet of a spectrometer (14) to be 0.5 seconds after the start of the pulse laser so as to record the heat radiation of a sample (7) heated by single laser pulse and avoid the influence of other stray light;
and 8, performing an X-ray diffraction experiment, wherein X-rays are incident to the sample (7) from the lower opening of the lower support disc (1), diffraction light generated by the sample (7) is emitted from the lower opening of the lower support disc (1), and the diffraction light is detected by adopting a light detector, so that an X-ray diffraction signal spectrum of the sample (7) is obtained.
The method adopts the supporting disc with a special structure to press the anvil, so that X rays can enter the sample at a larger angle, teflon is added between the gasket and the sample, the stability of the sample is improved, the scattering and attenuation of other substances near the sample to the X rays are reduced, and the signal to noise ratio of an X-ray diffraction signal of the sample is increased.
Claims (1)
1. The high-pressure sample testing device for pulse laser heating comprises a lower supporting disc (1), a lower top anvil (2), an upper top anvil (3), an upper supporting disc (4), a gasket (5), a Teflon ring (6), a sample (7), an achromatic lens I (8), a diaphragm (9), an achromatic lens II (10), a filter (11), a beam splitter I (12), a beam splitter II (13), a spectrometer (14), an oscilloscope (15), a photodiode (16), a signal generator (17), a laser (18), a beam splitter III (19), a reflecting mirror (20), a focusing lens (21), a photomultiplier (22) and a camera (23), wherein xyz is a three-dimensional space coordinate system, the output end of the photomultiplier (22) is connected with the input end of the oscilloscope (15), the output end of the photodiode (16) is connected with the input end of the oscilloscope (15), and the output end of the signal generator (17) is connected with the triggering end of the laser (18); the optical imaging device comprises an achromatic lens I (8), a diaphragm (9), an achromatic lens II (10), an optical filter (11), a beam splitter I (12), a beam splitter II (13) and a spectrometer (14), which are sequentially positioned right above an upper anvil (3) and form an imaging optical path, light emitted from a sample (7) sequentially passes through the upper anvil (3), the achromatic lens I (8), the diaphragm (9), the achromatic lens II (10) and the optical filter (11), reaches the beam splitter I (12) and is divided into two identical beams of light, one beam of light enters a photomultiplier (22) after being deflected and is converted into an electric signal to be input into an oscilloscope (15), the other beam of light propagates along an original path and is divided again at the beam splitter II (13), wherein a part with the wavelength longer than 760 nanometers enters the spectrometer (14) and a part with the wavelength less than or equal to 760 nanometers enters a camera (23) for carrying out thermal imaging on the sample (7); the light inlet of the spectrometer (14) is provided with a shutter and a pinhole, the shutter can be controllably opened or closed, the position and the size of the pinhole can be adjusted to control the quantity of light entering the spectrometer (14) and can be used for collimation of light beams, and the temperature of the sample (7) can be calculated according to the thermal radiation recorded by the spectrometer (14); the laser (18), the beam splitter III (19), the reflecting mirror (20) and the focusing lens (21) form a heating laser light path, laser light emitted by the laser (18) is divided into two identical beams by the beam splitter III (19), one beam passes through the focusing lens (21) and the upper anvil (3) in sequence after being reflected by the reflecting mirror (20) and is incident on the sample (7), and the other beam is deflected, then is emitted onto the photodiode (16) and is converted into an electric signal to be input into the oscilloscope (15); the lower anvil (2) is in a decahedron shape and comprises an upper surface, a lower surface, four upper side surfaces and four lower side surfaces, wherein the upper surface and the lower surface are parallel to a horizontal plane and are respectively formed by cutting and processing a cubic diamond block with the length, the width and the height of 7 mm, 5 mm and 4 mm, the four upper side surfaces and the four lower side surfaces form an angle of 45 degrees with the horizontal plane, two lower side surfaces parallel to an x axis are defined as a lower side surface I and a lower side surface III, and two lower side surfaces parallel to a z axis are defined as a lower side surface II and a lower side surface IV; the upper anvil (3) is in the shape of two upper round tables and lower round tables which are coaxially arranged up and down, and the lower bottom surface of the upper round table is coplanar with the upper bottom surface of the lower round table; the lower supporting disc (1) and the upper supporting disc (4) are hollow cylinders and are provided with an upper opening and a lower opening, the inner side of the lower opening of the upper supporting disc (4) is provided with a truncated cone-shaped chamfer, and the truncated cone-shaped chamfer is contacted with the side surface of the upper truncated cone of the upper anvil (3); the inner side of the upper opening of the lower supporting disc (1) is provided with two upper-side chamfer surfaces parallel to the x axis, the upper-side chamfer surfaces are respectively contacted with the lower side surface I and the lower side surface III of the lower top anvil (2), the upper opening of the lower supporting disc (1) is not contacted with the lower side surface II and the lower side surface IV of the lower top anvil (2), incident light can sequentially pass through the lower opening of the lower supporting disc (1), the lower side surface II of the lower top anvil (2) and the upper surface of the lower top anvil (2) to shoot a sample (7), diffracted light formed after the interaction of the incident light and the sample (7) can sequentially pass through the upper surface of the lower top anvil (2) and the lower side surface IV of the lower top anvil (2) to shoot out from the lower opening of the lower supporting disc (1), the lower opening of the lower supporting disc (1) is provided with two lower-side chamfer surfaces parallel to the z axis, the included angle between the two lower-side chamfer surfaces is 160 degrees, and the maximum incident angle between the diffracted light which can shoot out through the lower opening of the lower supporting disc (1) is 160 degrees; the gasket (5) is made of amorphous alloy based on zirconium metal, the Teflon ring (6) is positioned in the gasket (5), and the sample (7) is positioned in the Teflon ring (6); the lower support disc (1) and the upper support disc (4) are both made of silicon carbide; the lower anvil (2) and the upper anvil (3) are both made of diamond; the diameter of the upper bottom surface of the upper round table of the upper anvil (3) is 3 mm, the diameter of the lower bottom surface is 4 mm, and the height is 0.5 mm; the diameter of the lower bottom surface of the lower round table of the upper anvil (3) is 1 mm, the height is 0.3 mm,
the method is characterized in that: the pulse laser heating high-pressure sample testing method comprises the following steps:
step 1, a pressurizing device is adopted to respectively apply pressure to a lower anvil (2) and an upper anvil (3) through a lower supporting disc (1) and an upper supporting disc (4), so that the pressure range of a sample (7) is 2 to 8Gpa;
step 2. A laser (18) emits a continuous laser with a power of 0.8 to 2.4 milliwatts and adjusts the positions of a beam splitter III (19), a mirror (20) and a focusing lens (21) so that the continuous laser irradiates the surface of the sample (7) and an optical image of the sample (7) is recorded by a camera (23);
step 3, adjusting the laser (18) to increase the power of the continuous laser until the temperature change of a heating area on the surface of the sample (7) can be detected by the spectrometer (14), and then collimating the sample through a pinhole of a light inlet of the spectrometer (14), wherein a typical value of the temperature of the heating area is 2000K;
step 4, corresponding an optical image recorded by a camera (23) on a spatial scale to a thermal distribution image recorded by a spectrometer (14) of the sample (7);
step 5, keeping the collimated laser path unchanged, and adjusting the position of a focusing lens (21) to defocus laser incident to the sample (7) so as to reduce the temperature gradient in a heating area on the surface of the sample (7) and make the diameter of the heating area be 10 microns;
step 6, adjusting the pinhole size of the light inlet of the spectrometer (14) and the position of the achromat I (8) so that the light entering the spectrometer (14) comes from the range that the center radius of the heating area of the surface of the sample (7) is 4 microns;
step 7, triggering a laser (18) by adjusting a signal generator (17) to emit pulse laser, wherein the typical value of single pulse time is 25 milliseconds, and setting the shutter opening time of a light inlet of a spectrometer (14) to be 0.5 seconds after the start of the pulse laser so as to record the heat radiation of a sample (7) heated by single laser pulse and avoid the influence of other stray light;
and 8, performing an X-ray diffraction experiment, wherein X-rays are incident to the sample (7) from the lower opening of the lower support disc (1), diffraction light generated by the sample (7) is emitted from the lower opening of the lower support disc (1), and the diffraction light is detected by adopting a light detector, so that an X-ray diffraction signal spectrum of the sample (7) is obtained.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811501107.9A CN109444191B (en) | 2018-11-27 | 2018-11-27 | Pulse laser heating high-pressure sample testing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811501107.9A CN109444191B (en) | 2018-11-27 | 2018-11-27 | Pulse laser heating high-pressure sample testing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109444191A CN109444191A (en) | 2019-03-08 |
| CN109444191B true CN109444191B (en) | 2023-08-11 |
Family
ID=65558460
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811501107.9A Active CN109444191B (en) | 2018-11-27 | 2018-11-27 | Pulse laser heating high-pressure sample testing method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109444191B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110361405A (en) * | 2019-07-02 | 2019-10-22 | 南方科技大学 | Diffraction device and diffraction measurement method |
| CN113567400A (en) * | 2021-07-16 | 2021-10-29 | 北京高压科学研究中心 | Device capable of measuring second harmonic of substance under ultrahigh pressure condition and application thereof |
| CN114279836B (en) * | 2021-12-14 | 2024-07-09 | 北京高压科学研究中心 | Physical property characterization system and method based on dynamic loading |
| CN114563358A (en) * | 2022-02-15 | 2022-05-31 | 北京理工大学 | Double-sided laser heating equipment for researching high-temperature and high-pressure response of material |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003205233A (en) * | 2001-10-31 | 2003-07-22 | Tokai Univ | Ultrahigh pressure producing method and apparatus |
| RU95400U1 (en) * | 2010-02-04 | 2010-06-27 | Учреждение Российской академии наук Институт кристаллографии им. А.В. Шубникова РАН | HIGH PRESSURE SYMMETRIC NON-MAGNETIC CAMERA WITH DIAMOND ANVIL |
| CN104142316A (en) * | 2014-08-15 | 2014-11-12 | 中国科学院上海技术物理研究所 | Pre-ablation and reheating combined triple-pulse LIBS (laser-induced breakdown spectroscopy) detection system |
| US9194824B1 (en) * | 2011-03-28 | 2015-11-24 | Us Synthetic Corporation | Anvils and ultra-high pressure apparatuses using the same |
| CN106525884A (en) * | 2016-11-15 | 2017-03-22 | 中国科学院高能物理研究所 | Optical system and fluorescence measurement and pre-positioning method thereof |
| CN107044995A (en) * | 2017-01-12 | 2017-08-15 | 吉林大学 | The measuring system and measuring method of material Curie temperature under high pressure |
| CN107715798A (en) * | 2017-10-20 | 2018-02-23 | 金华职业技术学院 | The device of gas polymerisation is carried out under the conditions of a kind of cryogenic high pressure |
| CN107884728A (en) * | 2017-10-20 | 2018-04-06 | 金华职业技术学院 | A kind of method that magnet-optical medium film physical property is measured under the conditions of cryogenic high pressure |
| CN107884260A (en) * | 2017-10-20 | 2018-04-06 | 金华职业技术学院 | A kind of method of material property under measurement high-temperature and high-pressure conditions |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7736472B2 (en) * | 2001-10-31 | 2010-06-15 | Tokai University Educational System | Method and device for generating ultra-high pressure |
-
2018
- 2018-11-27 CN CN201811501107.9A patent/CN109444191B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003205233A (en) * | 2001-10-31 | 2003-07-22 | Tokai Univ | Ultrahigh pressure producing method and apparatus |
| RU95400U1 (en) * | 2010-02-04 | 2010-06-27 | Учреждение Российской академии наук Институт кристаллографии им. А.В. Шубникова РАН | HIGH PRESSURE SYMMETRIC NON-MAGNETIC CAMERA WITH DIAMOND ANVIL |
| US9194824B1 (en) * | 2011-03-28 | 2015-11-24 | Us Synthetic Corporation | Anvils and ultra-high pressure apparatuses using the same |
| CN104142316A (en) * | 2014-08-15 | 2014-11-12 | 中国科学院上海技术物理研究所 | Pre-ablation and reheating combined triple-pulse LIBS (laser-induced breakdown spectroscopy) detection system |
| CN106525884A (en) * | 2016-11-15 | 2017-03-22 | 中国科学院高能物理研究所 | Optical system and fluorescence measurement and pre-positioning method thereof |
| CN107044995A (en) * | 2017-01-12 | 2017-08-15 | 吉林大学 | The measuring system and measuring method of material Curie temperature under high pressure |
| CN107715798A (en) * | 2017-10-20 | 2018-02-23 | 金华职业技术学院 | The device of gas polymerisation is carried out under the conditions of a kind of cryogenic high pressure |
| CN107884728A (en) * | 2017-10-20 | 2018-04-06 | 金华职业技术学院 | A kind of method that magnet-optical medium film physical property is measured under the conditions of cryogenic high pressure |
| CN107884260A (en) * | 2017-10-20 | 2018-04-06 | 金华职业技术学院 | A kind of method of material property under measurement high-temperature and high-pressure conditions |
Non-Patent Citations (1)
| Title |
|---|
| 周强.激光加热原位高温高压拉曼、布里渊散射研究.《中国博士学位论文全文数据库 基础科学专辑》.2007,2007年(第05期),A005-4. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109444191A (en) | 2019-03-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109444191B (en) | Pulse laser heating high-pressure sample testing method | |
| EP2677301B1 (en) | Method and system for improving precision of element measurement based on laser-induced breakdown spectroscopy | |
| CN105807305B (en) | A kind of double-wavelength pulse laser radiation dose rate effect analog system | |
| CN111060516B (en) | Multi-channel in-situ detection device and method for subsurface defects of optical element | |
| RU2249813C2 (en) | Device for taking elementary analysis by means of spectrometry of optical emission on laser-generated plasma | |
| JPH034151A (en) | Light and heat type inspection method and device for executing said method | |
| CN109444111B (en) | Optical fiber LIBS detection system and method capable of selecting double-pulse mode | |
| CN108563034B (en) | Reflective spatial filter debugging device and method | |
| CN105928906B (en) | A kind of material reflectance dynamic measurement system varied with temperature and measurement method | |
| CN111443062B (en) | Device and method for detecting transient refractive index ultrafast of semiconductor material | |
| CN107356407A (en) | The device of synchro measure high-capacity optical fiber laser power, spectrum and beam quality | |
| CN111122599A (en) | Method for quickly imaging absorption type defects of large-caliber reflective film element | |
| CN114839145A (en) | Laser damage analysis test instrument | |
| CN209387559U (en) | A kind of high pressure sample test device of pulsed laser heating | |
| CN109444192B (en) | High-pressure sample testing device heated by pulse laser | |
| CN111175328A (en) | Real-time detection device and method for material structure | |
| CN109884032A (en) | The pinpoint laser induced breakdown spectroscopy detection system of ablation point and method | |
| CN111122397B (en) | Optical material performance detection device | |
| CN112595493A (en) | Common target surface measuring device and method for laser damage threshold and nonlinear absorption | |
| CN107886820B (en) | Integrated double-light-path laser ionization effect simulation system | |
| CN109358004A (en) | The method and apparatus of dual-wavelength difference non-marked micro-imaging | |
| US20150323431A1 (en) | 3d laser ablation tomography and spectrographic analysis | |
| CN110966931B (en) | Femtosecond laser processing morphological parameter time-resolved confocal measurement method and device | |
| JPWO2019038823A1 (en) | Far-infrared spectrometer and far-infrared spectroscopy method | |
| CN109613048B (en) | Method for researching phase change of sample under high pressure |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |