阅读说明：本技术 一种用于流体微观结构联用测量的温度压力控制样品腔 (Temperature and pressure control sample cavity for combined measurement of fluid microstructure ) 是由 缪夏然 周平 宋良益 杨春明 田丰 马静远 边风刚 黄宇营 李见 于 2020-12-15 设计创作，主要内容包括：本发明提供一种用于流体微光结构联用测量的温度压力控制样品腔,包括：密闭腔体；流体样品池,其设置于密闭腔体的中间密闭空间；加压套管,其与所述流体样品池连通,并与所述密闭腔体外部的一液压装置相连；加热模块,其埋设于所述密闭腔体中,并通过线缆和密闭腔体上的小孔与密闭腔体外部的控温装置连接；以及两个光学窗口,其位于所述流体样品池的上下两侧且彼此相对。本发明的用于流体微观结构联用测量的温度压力控制样品腔可以通过加热模块对流体样品池中的样品进行变温,既保证了样品的均匀变温,同时通过加压套管对内部流体进行加压,以保证控制样品所处的环境,提高了实验的可靠性。(The invention provides a temperature and pressure control sample cavity for the combined measurement of a fluid micro-optical structure, which comprises: sealing the cavity; the fluid sample cell is arranged in the middle closed space of the closed cavity; the pressurizing sleeve is communicated with the fluid sample cell and is connected with a hydraulic device outside the closed cavity; the heating module is embedded in the closed cavity and is connected with a temperature control device outside the closed cavity through a cable and a small hole in the closed cavity; and two optical windows located at upper and lower sides of the fluid sample cell and opposite to each other. The temperature and pressure control sample cavity for the combined measurement of the fluid microstructure can change the temperature of the sample in the fluid sample pool through the heating module, so that the uniform temperature change of the sample is ensured, and meanwhile, the internal fluid is pressurized through the pressurizing sleeve, so that the environment of the sample is ensured to be controlled, and the reliability of the experiment is improved.)

1. A temperature and pressure controlled sample chamber for use in conjunction with measurements of fluid microstructures, comprising:

a closed cavity (1);

a fluid sample cell (2) disposed in the middle enclosed space of the enclosed chamber (1);

the pressurizing sleeve (3) is communicated with the fluid sample cell (2) and is connected with a sample feeding pressurizing device (31) outside the closed cavity (1);

the heating module is embedded in the sealed cavity (1) and is connected with a temperature control device outside the sealed cavity (1) through a small hole in the sealed cavity (1) and a cable; and two optical windows (5) located on upper and lower sides of the fluid sample cell (2) and facing each other.

2. The temperature-pressure control sample chamber for use in the measurement of a combination of fluid microstructures according to claim 1, wherein the thickness of the fluid sample cell (2) is 1.0 to 1.5 mm.

3. Temperature-pressure control sample chamber for the joint measurement of fluidic microstructures according to claim 1, characterized in that the number of said pressurizing sleeves (3) is 2, which are inserted in the closed chamber (1).

4. The temperature and pressure control sample chamber for the measurement of the combination of microstructure of fluid according to claim 1, wherein the closed chamber (1) is fixed in a pressing housing (6), the pressing housing (6) comprises two pressing parts, each pressing part is distributed with a plurality of angle positioning holes (61) with central symmetry, and the angle positioning holes (61) are matched with the angles of the concave screw heads.

5. The temperature-pressure controlled sample chamber for the co-usage of fluidic microstructures according to claim 4, wherein the closed chamber body (1) and the pressure housing (6) are provided with a conical opening at a side of each optical window (5) away from the fluidic sample cell (2), and the size of the opening gradually increases in a direction away from the fluidic sample cell (2).

6. The temperature-pressure control sample chamber for the measurement of the combination of fluid microstructures according to claim 5, wherein the periphery of the optical window (5) is fixed to the position of the closed cavity (1) where the opening is formed by welding to achieve sealing.

7. The temperature-pressure controlled sample chamber for use in conjunction with measurements of fluid microstructures according to claim 5, wherein an opening angle of said opening is at least 65 °.

8. The temperature-pressure control sample chamber for the joint measurement of fluid microstructures according to claim 4, wherein the closed chamber (1) comprises two sealing covers (11) fitted to each other and a sealing cover base (12) disposed between the sealing cover (11) and the pressing housing (6), and two optical windows (5) are respectively disposed at axial centers of the sealing cover (11) and the sealing cover base (12).

9. Temperature-pressure controlled sample chamber for the joint measurement of fluidic microstructures according to claim 1, wherein the optical window (5) is made of single crystal diamond and has a diameter of at least 2.5 mm.

10. The temperature-pressure control sample chamber for the joint measurement of fluid microstructures according to claim 1, wherein the material of the closed chamber body (1) is copper.

Technical Field

The invention belongs to the field of material structure measurement, and particularly relates to a temperature and pressure control sample cavity for combined measurement of a fluid microstructure.

Background

Synchrotron radiation X-ray small angle scattering (SAXS) is sensitive to electron cloud distribution of materials, typically collecting scattering signals at angles less than 5 °, and is used to study the nanoscale structure of new materials in complex fluids. The synchrotron radiation X-ray wide angle diffraction (WAXS) is sensitive to the periodic structure of the material, and the relevant parameters such as the crystal form of the material can be obtained by collecting diffraction signals of which the angle is more than 5 degrees. Raman scattering is an inelastic scattering used to study vibrational modes of molecules and can probe the backbone structure of the molecule. The complex fluid can show special properties at high temperature and high pressure, and the SAXS, the WAXS and the Raman can be used for researching the microstructure information of the complex fluid in different scales at high temperature and high pressure, so that the analysis of the relationship between the structure and the performance of the complex fluid at high temperature and high pressure is facilitated.

However, no high-temperature high-pressure sample cavity which simultaneously meets the combined measurement of complex fluids SAXS, WAXS and Raman exists in the market at present.

Therefore, a temperature and pressure control sample cavity which can simultaneously reach the pressure of 15MPa and the temperature of 700K is urgently needed to meet the sample requirement of complex fluid.

Disclosure of Invention

The invention aims to provide a temperature and pressure control sample cavity for the combined measurement of a fluid microstructure so as to simultaneously meet the requirements of the combined measurement of in-situ synchrotron radiation X-ray scattering, X-ray diffraction and Raman scattering of complex fluids.

In order to achieve the above object, the present invention provides a temperature-pressure controlled sample chamber for measurement in combination with a fluid microstructure, comprising: sealing the cavity; the fluid sample cell is arranged in the middle closed space of the closed cavity; the pressurizing sleeve is communicated with the fluid sample cell and is connected with a sample introduction pressurizing device outside the closed cavity; the heating module is embedded in the closed cavity and is connected with a temperature control device outside the closed cavity through a cable and a small hole in the closed cavity; and two optical windows located at upper and lower sides of the fluid sample cell and opposite to each other.

The thickness of the fluid sample cell is 1.0-1.5 mm.

The number of the pressurizing sleeves is 2, and the pressurizing sleeves are inserted into the closed cavity.

The closed cavity is fixed in a pressing shell, the pressing shell comprises two pressing parts, a plurality of angle positioning holes which are centrosymmetric are distributed on each pressing part, and the angle positioning holes are matched with the angles of the concave screw heads.

The closed cavity and the pressing shell are provided with a conical opening at one side of each optical window, which is far away from the fluid sample cell, and the size of the opening is gradually increased along the direction far away from the fluid sample cell.

The periphery of the optical window is fixed at the position of the closed cavity body, which is provided with the opening, in a welding mode so as to realize sealing.

The opening angle of the opening is at least 65 °.

The sealed cavity comprises two sealing covers matched with each other and a sealing cover base arranged between the sealing covers and the pressing shell, and the two optical windows are respectively arranged at the axes of the sealing covers and the sealing cover base.

The optical window is made of single crystal diamond and has a diameter of at least 2.5 mm.

The closed cavity is made of copper.

The temperature and pressure control sample cavity for the complex fluid microstructure combined measurement performs temperature change on a sample in the fluid sample pool through the temperature change block in the heating module, so that the uniform temperature change of the sample is ensured; meanwhile, the internal fluid is pressurized through the pressurizing sleeve, so that the environment of the sample is guaranteed to be controlled, the reliability of the experiment is improved, the temperature can reach 700K, and the pressure can reach 15 MPa. In addition, the window material of the invention selects the single crystal diamond with high transmittance to rays, thereby reducing stray signals and ensuring the atmosphere environment, the maximum scattering angle can reach 65 degrees, the diameter of the optical path window is at least 2.5mm, and the requirements of WAXS signal collection on the scattering angle and the spot size requirements of X rays and Raman laser are met.

Drawings

FIG. 1 is a schematic side view of a temperature pressure control sample chamber for use in measurements of fluid microstructure in accordance with an embodiment of the invention.

Fig. 2 is a schematic top view of the temperature and pressure control sample chamber for measurement in conjunction with fluid microstructure shown in fig. 1.

Detailed Description

The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.

Fig. 1 shows a temperature and pressure controlled sample chamber for use in conjunction with measurements of fluid microstructures for use in situ and in conjunction with measurements of synchrotron radiation X-ray scattering, X-ray diffraction, and raman scattering of a fluid sample, according to one embodiment of the present invention. The device comprises a closed cavity 1, a fluid sample cell 2 arranged in the middle closed space of the closed cavity 1, a pressurizing sleeve 3 communicated with the fluid sample cell 2, a heating module (not shown) embedded in the closed cavity 1, and two optical windows 5 which are positioned at the upper side and the lower side of the fluid sample cell 2 and are opposite to each other. The closed cavity 1 is fixed in the pressing shell 6.

Wherein, the thickness of the fluid sample cell 2 is 1.0-1.5 mm. The number of the pressurizing sleeves 3 is 2, and the pressurizing sleeves are inserted into the closed cavity 1; one of the pressurizing sleeves 3 is connected with a sample injection pressurizing device 31 outside the closed cavity 1, so that a fluid sample is injected into the sample cell 2 through the sample injection pressurizing device 31 and the pressure environment of the sample is changed; the other pressurizing cannula 3 is connected to a sample outlet valve 32 to control the discharge and pressure environment of the fluid sample. The heating modules are preferably heating pipes, the heating modules are embedded in a sealing cover base 12 of the sealed cavity 1 in an array mode, the array is preferably a circumferential array, the number of the heating modules is preferably 2-4, and the heating modules are connected with a temperature control device outside the sealed cavity 1 through cables and small holes reserved in the sealed cavity 1 so as to change the temperature condition of the fluid sample. Therefore, different pressure and temperature conditions are changed through the pressurizing sleeve 3 and the heating module, and the synchrotron radiation X-ray scattering, diffraction and Raman combined experiment of the experimental sample is completed. The temperature and pressure control sample cavity for the combined measurement of the fluid microstructure can simultaneously reach the pressure of 15MPa and the temperature of 700K.

The closed cavity 1 is made of copper and is a cylindrical cavity and comprises two sealing covers 11 (comprising an upper sealing cover and a lower sealing cover) which are matched with each other and two sealing cover bases 12 arranged between the sealing covers and the pressing shell, a heat insulation cushion layer is arranged between the sealing covers 11 and the sealing cover bases 12 to prevent high temperature from being conducted to the pressing shell 6, and two optical windows 5 are respectively arranged in the centers of the sealing covers 11 and the sealing cover bases 12 of the closed cavity 1. Therefore, X-rays and laser can enter from the optical window 5 of the sealing cover 11 of the sealed cavity 1 and irradiate on the fluid sample in the fluid sample cell 2, the X-rays interact with electrons in the sample to generate a scattering signal, and the scattering signal passes through the optical window 5 on the other side and then enters an X-ray detector; the laser-excited reflected raman spectrum signal is returned in the original path and collected by an external optical device such as a raman light probe. In this embodiment, the optical window 5 is made of single crystal diamond, and has a diameter of at least 2.5mm and a thickness of 300 to 500 μm. Therefore, the X-ray penetrates through the window of the single crystal diamond to irradiate on the fluid sample, the single crystal diamond absorbs less X-ray, and therefore the accuracy of the experiment is improved.

The closed cavity 1 and the pressing shell 6 are provided with a conical opening on the side of each optical window 5 far from the fluid sample cell 2, the size of the opening is gradually increased along the direction far from the fluid sample cell 2, and the opening angle of the opening is at least 65 degrees, so that the scattering opening angle at two ends of each optical window 5 can reach 65 degrees at most. The periphery of the optical window 5 is fixed at the position of the closed cavity 1, which is provided with the opening, in a welding mode so as to realize sealing.

The pressing housing 6 is located on a coaxial optical path of the X-ray and the raman laser, that is, on a coaxial optical path for combined measurement of synchrotron radiation X-ray scattering, X-ray diffraction, and raman scattering, and includes two pressing members (i.e., an upper pressing member and a lower pressing member). The pressing shell 6 is fixed on a three-dimensional displacement table so as to move the closed cavity 1 to the coaxial light path through the three-axis displacement table, and ensure that X rays and Raman laser irradiate on a sample through the optical window 5 at the maximum intensity during testing, so that the X rays penetrate through the sample to form a scattering signal on the other side, and the Raman laser irradiates on the sample to excite the sample to reflect the Raman signal and return the Raman signal in the original path. The positioning repeatability requirement of the three-dimensional translation stage is better than 1 micrometer.

As shown in fig. 2, a plurality of angle positioning holes 61 with symmetrical centers are distributed on each pressing part of the pressing shell 6, the angle positioning holes 61 are matched with the angles of the concave screw heads, and the angle positioning holes 61 are matched with the angles of the concave screw heads to press the pressing shell 6, so that the pressing shell 6 presses the sealing cover 11 and the sealing cover base 12 of the sealed cavity 1 after being screwed by the concave screw heads.

Thus, the temperature and pressure control sample chamber for the measurement of the combination of fluid microstructures of the present invention satisfies the following requirements: the opening angle of the front window and the rear window of the temperature and pressure control sample cavity is at least 65 degrees, so that the requirements of WAXS signal collection on the scattering angle and the requirements of Raman signal strength on the collected scattering angle are met. Secondly, the sizes of the front window and the rear window of the temperature pressure control sample cavity are not less than 2.5mm, so that the spot size requirements of X-rays and Raman laser are met. And the front and rear window materials need to be single crystal diamond, so that the requirement of X-ray transmission performance is met. And fourthly, the pressurizing mode of the temperature and pressure control sample cavity is hydraulic pressure, so that the requirement that the experimental sample is fluid is met.

In conclusion, the temperature and pressure control sample cavity heats and pressurizes the internal fluid through the temperature control device and the pressurizing sleeve, so that the environment of the sample can be ensured to be controlled, X rays, Raman scattering and the like can pass through the temperature and pressure control sample cavity, and in-situ temperature and pressure changing experiments can be completed as required.

The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not intended to limit the scope of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present application fall within the scope of the claims of the present patent application. The invention has not been described in detail in order to avoid obscuring the invention.