阅读说明：本技术 一种耐腐蚀原位高温微型衍射仪 (Corrosion-resistant in-situ high-temperature miniature diffractometer ) 是由 高梅 文闻 张兴民 雷琦 周兴泰 高兴宇 黄宇营 于 2019-10-23 设计创作，主要内容包括：本发明提供一种耐腐蚀原位高温微型衍射仪,包括：样品毛细管,旋转轴,第一联轴器,变速马达,滑动轴,主丝杆,以及加热组件；其中,样品毛细管的第一端与旋转轴连接,旋转轴又通过第一联轴器与变速马达连接,通过变速马达驱动实现样品毛细管的旋转运动；滑动轴套设于旋转轴的外侧,滑动轴与主丝杆螺纹连接,通过旋转主丝杆实现样品毛细管在水平方向上的运动；样品毛细管的第二端与加热组件连接实现样品加热。根据本发明,提供了一种可多维度调节的、整体结构紧凑的、既可以安装到上海光源BL14B1衍射光束线实验站,也可以安装到其它线站进行原位表征的耐腐蚀原位高温微型衍射仪。(The invention provides a corrosion-resistant in-situ high-temperature micro diffractometer, which comprises: the device comprises a sample capillary tube, a rotating shaft, a first coupler, a variable speed motor, a sliding shaft, a main screw rod and a heating assembly; the first end of the sample capillary is connected with a rotating shaft, the rotating shaft is connected with a variable speed motor through a first coupler, and the rotating motion of the sample capillary is realized through the driving of the variable speed motor; the sliding shaft is sleeved on the outer side of the rotating shaft and is in threaded connection with the main screw rod, and the sample capillary tube moves in the horizontal direction by rotating the main screw rod; and the second end of the sample capillary is connected with the heating component to realize sample heating. According to the invention, the corrosion-resistant in-situ high-temperature micro diffractometer can be adjusted in multiple dimensions, is compact in overall structure, and can be mounted to a Shanghai light source BL14B1 diffraction beam line experiment station and other line stations for in-situ characterization.)

1. A corrosion-resistant in-situ high temperature micro diffractometer, comprising: the device comprises a sample capillary tube, a rotating shaft, a first coupler, a variable speed motor, a sliding shaft, a main screw rod and a heating assembly;

the first end of the sample capillary is connected with the rotating shaft, the rotating shaft is connected with the variable speed motor through the first coupler, and the rotating motion of the sample capillary is realized through the driving of the variable speed motor;

the sliding shaft is sleeved on the outer side of the rotating shaft, a connecting block is arranged on the sliding shaft and is in threaded connection with the main screw rod through the connecting block, and the sample capillary tube moves in the horizontal direction by rotating the main screw rod;

the second end of the sample capillary is connected with the heating component, the sample in the sample capillary is heated by the heating component, and the heating component is provided with an X-ray transmission hole for transmitting the X-ray.

2. The corrosion-resistant in-situ high temperature micro-diffractometer according to claim 1, wherein the connection of the first end of the sample capillary to the rotating shaft is performed by: the first end of sample capillary is connected with a capillary protective housing, the capillary protective housing is installed in a capillary mounting disc through lock nut again, the capillary mounting disc is fixed in through the screw again the rotating shaft end cover on the tip of rotation axis.

3. The corrosion-resistant in-situ high-temperature micro diffractometer according to claim 2, wherein the first end of the sample capillary is flexibly connected with the capillary protective shell by inserting plasticine, and the concentricity of the sample capillary and the rotating shaft is realized by adjusting a screw on the capillary mounting plate.

4. The corrosion-resistant in-situ high temperature micro-diffractometer according to claim 1, wherein the heating assembly comprises: platinum wire heating furnace, heating furnace thermocouple and heating furnace electrode.

5. The corrosion-resistant in-situ high temperature micro-diffractometer of claim 4, wherein the heating assembly further comprises: the fine adjustment device comprises a heating furnace fine adjustment supporting plate for supporting the platinum wire heating furnace, and a fine adjustment screw rod connected with the heating furnace fine adjustment supporting plate and used for realizing the displacement of the heating assembly in the horizontal direction.

6. The corrosion-resistant in-situ high temperature micro-diffractometer according to claim 1, wherein the sample capillary is made of quartz or graphite.

7. The corrosion-resistant in-situ high temperature micro-diffractometer according to claim 1, wherein the rotating shaft is in interference fit with an outer sliding shaft through a rolling bearing for rotation and support.

8. The corrosion-resistant in-situ high-temperature micro-diffractometer according to claim 1, wherein the corrosion-resistant in-situ high-temperature micro-diffractometer can be mounted on a diffraction beam line experiment station for in-situ high-temperature XRD phase change test, and can also be independently fixed on an electric tripod component for characterization test.

9. The corrosion-resistant in situ high temperature micro diffractometer of claim 8, wherein said motorized tripod assembly comprises: the tripod support is installed in proper order from bottom to top install in step motor, second shaft coupling, rotatory lead screw and the perpendicular sliding disk that connects gradually on the tripod support, through step motor's drive realizes the motion of perpendicular sliding disk along vertical direction.

10. The corrosion-resistant in-situ high-temperature micro-diffractometer according to claim 9, wherein the vertical sliding disk is connected to a rotating disk with an adjustable inclination angle through a transition disk, and the corrosion-resistant in-situ high-temperature micro-diffractometer is connected to the rotating disk through a main mounting table, so as to adjust the inclination of the sample capillary.

Technical Field

The invention relates to the field of rotary capillary devices, in particular to a corrosion-resistant in-situ high-temperature micro diffractometer.

Background

In recent years, the fourth generation advanced nuclear reactor is actively developed in all countries in the world, the thorium-based molten salt reactor nuclear energy system is mainly developed in China, high-temperature molten liquid flows in a molten salt reactor, the molten salt has strong chemical corrosivity, the interaction process of reactor engineering materials and the molten salt under high temperature needs to be observed in situ by comprehensive synchrotron radiation X-ray diffraction, absorption, scattering, imaging and other characterization technologies, and the microstructure evolution mechanism of the reactor engineering materials under the strong corrosion environment of the molten salt is researched, but no device capable of applying a synchrotron radiation light source to carry out such experiments exists at present.

Disclosure of Invention

The invention aims to provide a corrosion-resistant in-situ high-temperature micro diffractometer, so that the problem that a device capable of applying a synchrotron radiation light source to research high-temperature strong-corrosion molten salt is lacked in the prior art is solved.

In order to solve the technical problems, the invention adopts the following technical scheme:

provided is a corrosion-resistant in-situ high-temperature micro diffractometer, comprising: the device comprises a sample capillary tube, a rotating shaft, a first coupler, a variable speed motor, a sliding shaft, a main screw rod and a heating assembly; the first end of the sample capillary is connected with the rotating shaft, the rotating shaft is connected with the variable speed motor through the first coupler, and the rotating motion of the sample capillary is realized through the driving of the variable speed motor; the sliding shaft is sleeved on the outer side of the rotating shaft, a connecting block is arranged on the sliding shaft and is in threaded connection with the main screw rod through the connecting block, and the sample capillary tube moves in the horizontal direction by rotating the main screw rod; the second end of the sample capillary is connected with the heating component, and the sample in the sample capillary is heated by the heating component, and the heating component is provided with an X-ray transmission hole for transmitting X-ray; the corrosion-resistant in-situ high-temperature micro diffractometer is installed through the main installation platform, so that in-situ observation research of the reaction process of the molten salt and the reactor engineering material at high temperature is realized.

Preferably, the connection of the first end of the sample capillary to the rotation axis is performed by: the first end of sample capillary is connected with a capillary protective housing, the capillary protective housing is installed in a capillary mounting disc through lock nut again, the capillary mounting disc is fixed in through the screw again the rotating shaft end cover on the tip of rotation axis.

Preferably, the first end of the sample capillary is flexibly connected with the capillary protective shell through rubber mud stuffing, and the concentricity of the sample capillary and the rotating shaft is realized by adjusting a screw on the capillary mounting plate.

Preferably, the heating assembly comprises: platinum wire heating furnace, heating furnace thermocouple and heating furnace electrode.

Preferably, the heating assembly further comprises: the fine adjustment device comprises a heating furnace fine adjustment supporting plate for supporting the platinum wire heating furnace, and a fine adjustment screw rod connected with the heating furnace fine adjustment supporting plate and used for realizing the displacement of the heating assembly in the horizontal direction.

Preferably, the sample capillary is made of quartz or graphite.

Preferably, the rotating shaft is interference-fitted with an outer sliding shaft through a rolling bearing for rotation and support.

According to the invention, the corrosion-resistant in-situ high-temperature micro-diffractometer can be arranged on a Huber5021 type diffractometer of a Shanghai light source BL14B1 diffraction beam line experimental station to perform in-situ high-temperature XRD phase change test, and can also be independently fixed on an electric tripod component to perform characterization test.

The electric tripod assembly comprises: the tripod support is installed in proper order from bottom to top install in step motor, second shaft coupling, rotatory lead screw and the perpendicular sliding disk that connects gradually on the tripod support, through step motor's drive realizes the motion of perpendicular sliding disk along vertical direction.

Preferably, the vertical sliding disc is connected with a rotating disc with an adjustable inclination angle through a transition disc, and the corrosion-resistant in-situ high-temperature micro diffractometer is connected with the rotating disc through a main mounting table to realize the adjustment of the inclination of the sample capillary.

The corrosion-resistant in-situ high-temperature micro diffractometer provided by the invention has the beneficial effects that the sample capillary tube packaged with a sample to be detected can be adjusted in the horizontal direction and the vertical direction so that the sample can be aligned with X-ray, the sample capillary tube can be precisely heated and heated by the heating component while rotating, and the heating component can be finely adjusted in the horizontal direction relative to the sample capillary tube. The corrosion-resistant in-situ high-temperature micro-diffractometer provided by the invention has a compact integral structure, is small and light, meets the requirements of a narrow space and small load-bearing environment of a Huber5021 type diffractometer sample stage of a Shanghai light source BL14B1 diffraction beam line experiment station, and can be mounted on the Shanghai light source BL14B1 diffraction beam line experiment station and other line stations for in-situ characterization.

In summary, the key points of the invention are as follows: 1. the first international corrosion-resistant in-situ high-temperature micro diffractometer is developed; 2. the micro diffractometer can simultaneously meet the research requirements of static/dynamic high-temperature powder diffraction; 3. the micro diffractometer is the first diffractometer suitable for the research of high-temperature strong-corrosion environment in the world; 4. the X light spot size of the diffraction line station of the Shanghai light source 14B1 is small (0.2mm X0.3 mm), in order to ensure that a sample always aims at X light in the rotating process, the micro diffractometer is provided with a mechanism for adjusting the left and right positions, the vertical height and the concentricity of the sample in the horizontal direction, and through ingenious design, the whole structure is compact and small while the requirement of multi-dimensional adjustability is met, and the limit of limited bearing and narrow space of the Huber5021 type diffractometer sample platform of the Shanghai light source 14B1 is met; 5. the sample capillary in the micro diffractometer can rotate at variable speed, the rotation not only can improve the heating uniformity of a sample, but also can eliminate the orientation of the sample, and the speed change function can select proper rotating speed according to different samples and exposure duration; 6. the micro diffractometer can support capillaries with multiple sizes and different materials and a heating furnace with multiple sizes, and is convenient to select proper capillaries according to the size of sample particles, sample diffraction signals and the required temperature; 7. the sample capillary of the micro diffractometer can be heated in a large temperature area by a heating furnace while rotating, and the heating furnace with matched size can be selected according to the size of the capillary, so that the thermal efficiency is fully exerted.

In a word, the invention provides the corrosion-resistant in-situ high-temperature micro diffractometer which can be adjusted in multiple dimensions, has a compact overall structure and can be used for researching high-temperature strong-corrosion molten salt by using a synchrotron radiation light source.

Drawings

FIG. 1 is a schematic diagram of the overall structure of a corrosion-resistant in-situ high-temperature micro-diffractometer provided in accordance with a preferred embodiment of the present invention;

FIG. 2 is a schematic view of the corrosion-resistant in-situ high temperature micro-diffractometer shown in FIG. 1, taken from another perspective;

FIG. 3 is a schematic view of the internal structure of the corrosion-resistant in-situ high temperature micro-diffractometer shown in FIG. 1 after hiding the main mounting stage;

FIG. 4 is a schematic view of the internal structure of FIG. 3 after further concealing the sliding shaft;

FIG. 5 is a schematic structural view of a motorized tripod assembly for use with a corrosion-resistant in-situ high temperature micro-diffractometer;

FIG. 6 is a schematic view of the structure of the corrosion-resistant in-situ high temperature micro diffractometer mounted on the electric tripod assembly together with the water inlet and outlet pipes.

Detailed Description

The present invention will be further described with reference to the following specific examples. It should be understood that the following examples are illustrative only and are not intended to limit the scope of the present invention.

Referring to fig. 1 to 4, a corrosion-resistant in-situ high-temperature micro-diffractometer 100 is provided according to a preferred embodiment of the present invention. The device includes: the device comprises a main mounting table 1, a limiting screw 2, a sliding shaft 3, a main screw rod 4, a variable speed motor 5, a rotating shaft end cover 6, a capillary mounting disc 7, a locking nut 8, a capillary protection shell 9, a sample capillary 10, an X-ray transmission hole 11, a platinum wire heating furnace 12, a heating furnace thermocouple 13, a heating furnace electrode 14, a heating furnace fine adjustment supporting plate 15, a fine adjustment screw rod 16, a connecting block 28, a first coupler 29, a rotating shaft 30 and a rolling bearing 31.

The main mounting platform 1 is a bearing platform of the whole device, is mainly used for mounting the sliding shaft 3 and the main screw rod 4, and is also a platform connected with an external device, and plays a most key role in connection. The first end of the sample capillary 10 is connected with a rotating shaft 30, the rotating shaft 30 is connected with a variable speed motor 5 through a first coupler 29, and the rotating motion of the sample capillary 10 can be realized through the driving of the variable speed motor 5; the sliding shaft 3 is sleeved outside the rotating shaft 30, and the sliding shaft 3 is in threaded connection with the main screw rod 4 through the connecting block 28, so that the sample capillary 10 can move left and right in the horizontal direction by rotating the main screw rod 4; the second end of the sample capillary 10 is connected with a heating component formed by a platinum wire heating furnace 12, a heating furnace thermocouple 13 and a heating furnace electrode 14, and the sample in the sample capillary is heated by the heating component, and the heating component is provided with an X-ray transmission hole 11 for transmitting the X-ray.

In view of the fragility and the varying diameter of the sample capillary 10, according to the preferred embodiment, the connection of the first end of the sample capillary 10 to the rotation axis 30 is performed by: the first end of the sample capillary 10 is connected with a capillary protection shell 9, plasticine is filled in a gap between the capillary protection shell and the capillary protection shell 9, the capillary protection shell 9 is arranged on a capillary installation plate 7 through a locking nut 8, and the capillary installation plate 7 is fixed on a rotating shaft end cover 6 on one end part of a rotating shaft 30 through a screw.

Because plasticine is filled between the sample capillary 10 and the sample protective shell 9, after the sample capillary is inserted into the sample protective shell, the sample center can not be ensured to be vertical to the sample mounting disc 7, when the sample mounting disc 7 is fixed on the rotating shaft end cover 6 by utilizing four surrounding screws, the aim of concentricity of the sample capillary 10 and the rotating shaft 30 can be achieved by finely adjusting different precession depths of the four screws, and therefore the X-ray can be ensured to be always irradiated on the sample and uniformly heated in the rotating process of the sample capillary 10.

According to the preferred embodiment, as shown in fig. 1 and 3, the side wall of the sliding shaft 3 is provided with the elongated groove structure 24 extending along the horizontal direction, and the main mounting table 1 is provided with two limit screws 2 inserted into the elongated groove structure 24, so that the moving distance of the sliding shaft 3 in the horizontal direction can be limited to prevent the sliding shaft from being out of alignment, and the sliding shaft 3 can be prevented from rolling along the circumferential direction.

According to the preferred embodiment, the sample capillary 10 is made of quartz or graphite, and the sample capillary made of graphite or quartz has high X-ray transmission property and is preferably 0.5mm to 4mm in outer diameter and 50mm in length. The diameter of the quartz tube can be 0.5mm, 1mm and 2mm respectively, certain pressure can be borne, the wall thickness is 0.01-0.1 mm, the absorption of X-rays (the energy is 18KeV) can be ignored, and a sample can be sealed in the quartz tube in advance; the size of the graphite pipe is 1.5mm in inner diameter and 4mm in outer diameter, the opening of the pipe is tightly sealed after being screwed in through the graphite plug, and the graphite has high X-ray transmission performance and good chemical stability, can resist corrosion of acid, alkali and organic solvents, can in situ study the microstructure evolution law of the molten salt reactor material in a high-temperature environment, clearly defines the degradation and failure mechanism of the molten salt reactor material in the high-temperature environment, and determines the performance optimization scheme of the molten salt reactor material.

According to the preferred embodiment, in order to match the size of the sample capillary 10 and sufficiently exert thermal efficiency, the platinum wire heating furnace 12 for providing a heating function to the sample capillary 10 may be used in two sizes, and when the outer diameter of the sample capillary 10 is less than or equal to 2mm, the platinum wire heating furnace 12 having an inner diameter of 3mm is preferably used, and when the outer diameter of the sample capillary 10 is 3 to 4mm, the platinum wire heating furnace 12 having an inner diameter of 5mm is preferably used, so that the sample packed in the sample capillary 10 is heated from room temperature to 1000 ℃.

According to the preferred embodiment, a platinum heating wire is uniformly wound spirally between two layers of ceramic sleeves (two tubes with different outer diameters are bonded by high temperature glue), and the X-ray transmitting hole 11 is preferably 1mm wide by 1.5mm high, opened at the central position of the upper half of the ceramic tube, as shown in fig. 1, and used for the incident and emergent X-rays (spot size 0.2mm (h) X0.3 mm (v)) to pass through.

According to the preferred embodiment, the heating assembly further comprises a heating furnace fine adjustment support plate 15 used for supporting the platinum wire heating furnace 12 and a fine adjustment screw rod 16 connected with the heating furnace fine adjustment support plate 15, the whole heating assembly can be adjusted by-3 mm in the left and right direction along the horizontal direction through manually adjusting the fine adjustment screw rod 16, and the X-ray transmission hole 11 is aligned to the X-ray.

According to the preferred embodiment, the heating assembly further preferably comprises a set of temperature control system, current is introduced through the heating furnace electrode 14, normal regulation of the temperature is controlled through a lead-out line of the heating furnace thermocouple 13, a whole set of automatic temperature control system such as a platinum rhodium-platinum thermocouple sensor, a temperature transmitter, a regulator and a display instrument is arranged outside the whole device, the temperature control precision of the system is 1 ℃, and the maximum temperature rise rate is 50 ℃/min.

According to the preferred embodiment, the rotary shaft 30 is also interference-fitted with the outside sliding shaft 3 through the rolling bearing 31 for rotation and support.

The corrosion-resistant in-situ high-temperature micro-diffractometer 100 provided according to the above preferred embodiment works according to the following principle:

when the main screw rod 4 starts to be manually rotated, the sliding shaft 3 moves left and right along the horizontal direction, namely the rotating shaft 30 in the sliding shaft is driven to move together, the sample capillary tube 10 is naturally driven to move left and right along the horizontal direction (the stroke is-10-15 mm), and the X-ray energy is ensured to accurately irradiate on a sample packaged in the sample capillary tube 10;

the variable speed motor 5 is started, the rotating shaft 30 is driven to rotate through the first coupler 29 in the sliding shaft 3, the sample capillary 10 can be driven to rotate in the platinum wire heating furnace 12, the rotating speed of the sample capillary 10 is adjustable, the rotating speed is preferably 20-100 rpm, the samples packaged in the sample capillary 10 can be uniformly mixed, and meanwhile, the heating uniformity is guaranteed.

According to the preferred embodiment of the invention, the corrosion-resistant in-situ high-temperature micro-diffractometer 100 is provided, and the device mainly has two installation modes, wherein one mode is that when the Shanghai light source BL14B1 diffraction beam line experiment station is used, the whole device is fixed on a Phi circular table of a Huber5021 type diffractometer through the main installation table 1, and the other mode is that when the other line stations are used, the whole device can be fixed on the electric triangle frame assembly 200 through the main installation table 1.

Referring to fig. 3 and 4, the present invention further provides an electric tripod assembly 200 for use with a corrosion-resistant in-situ high-temperature micro-diffractometer, comprising: tripod support 17, step motor 18, second coupling 19, rotatory lead screw 20, rotary disk 21, transition dish 22, vertical sliding disk 23.

The stepping motor 18, the coupler 19, the rotary screw rod 20 and the vertical sliding disc 23 are sequentially mounted on the tripod support 17 from bottom to top and are sequentially connected, and the vertical sliding disc 23 can move in the vertical direction by being driven by the stepping motor 18.

According to the preferred embodiment, the rotating disc 21 is connected to the vertical sliding disc 23 through the transition disc 22, and the rotating disc 21 is preferably adjustable within the inclination angle range of 0-10 degrees, so that when the corrosion-resistant in-situ high-temperature micro diffractometer 100 is connected with the rotating disc 21 through the main mounting table 1, the micro adjustment of the inclination of the sample capillary can be realized by operating the rotating disc 21, and the liquid sample is prevented from flowing out.

When the corrosion-resistant in-situ high-temperature micro diffractometer 100 is fixed to the electric triangular frame assembly 200 through the main mounting table 1, in order to prevent the temperature of the hot table from being too high during heating, a water cooling system is preferably configured, as shown in fig. 6, the corrosion-resistant in-situ high-temperature micro diffractometer 100 is respectively connected with a heat radiation water inlet pipe 26 and a water outlet pipe 27, and thus the construction of the whole working mode is completed.

The electric tripod assembly 200 according to the above preferred embodiment operates as follows:

the stepping motor 18 on the tripod support 17 is electrified to start working (stroke is 30mm), the rotating screw rod 20 is driven by the second coupler 19 to drive the vertical sliding disc 23 to move up and down to adjust the height of the sample capillary 10, so that the sample capillary and the X-ray are in the same horizontal plane, and in addition, the inclination of the sample capillary 10 can be adjusted by rotating the rotating disc 21, so that the liquid sample in the sample capillary 10 cannot flow out.

The invention focuses on the operation mode of the whole device on the electric tripod component, when the electric tripod is cancelled and is directly installed on the Huber5021 diffractometer of the Shanghai light source BL14B1 diffraction beam line experiment station, except that the up-and-down movement driven by the stepping motor 18 and the rotation driven by the rotating disc 21 are replaced by the diffractometer, other operation modes are the same as the above embodiment, and are not repeated.

The above embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and various changes may be made in the above embodiments 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.