Detection device for measuring sample characteristics of X-ray diffractometer at high temperature
阅读说明：本技术 一种用于x射线衍射仪在高温下测量样品特性的检测装置 (Detection device for measuring sample characteristics of X-ray diffractometer at high temperature ) 是由 张所峰 刘川 王军龙 胡婷婷 于 2020-07-23 设计创作，主要内容包括：本发明公开一种用于X射线衍射仪在高温下测量样品特性的检测装置,包括固定底座、平移底座、中壳、前盖。平移底座上有金属加热丝接线柱及冷却通道、检测温度插座及冷却通道、升降用平移微分头装置。中壳上均匀分布3个螺旋型卡块、X射线进出通道、保护密封膜及中壳冷却通道。多用途样品架内均匀缠绕螺旋状金属加热丝。防辐射弧形板为两个弧形罩。前旋盖通过螺旋型卡块与中壳上的螺旋形卡块相互旋转并锁紧,使其与中壳上密封圈紧密接触。本发明采用多用途样品架内均匀缠绕螺旋状金属加热丝给样品板加热,并通过样品板内温度传感器反馈温度到控制软件来调节并控制对样品的加热温度,使样品板上的样品温度始终稳定在设定温度。(The invention discloses a detection device for measuring sample characteristics of an X-ray diffractometer at high temperature. The translation base is provided with a metal heating wire binding post, a cooling channel, a temperature detection socket, a cooling channel and a translation differential head device for lifting. 3 spiral fixture blocks, an X-ray inlet and outlet channel, a protective sealing film and a middle shell cooling channel are uniformly distributed on the middle shell. Spiral metal heating wires are uniformly wound in the multipurpose sample rack. The radiation-proof arc-shaped plate is two arc-shaped covers. The front rotary cover rotates and is locked with the spiral clamping block on the middle shell through the spiral clamping block, so that the front rotary cover is in close contact with the sealing ring on the middle shell. The invention adopts the multi-purpose sample rack to uniformly wind the spiral metal heating wires to heat the sample plate, and feeds back the temperature to the control software through the temperature sensor in the sample plate to adjust and control the heating temperature of the sample, so that the temperature of the sample on the sample plate is always stabilized at the set temperature.)
1. A test device for measuring properties of a sample at an elevated temperature using an X-ray diffractometer, comprising: comprises a fixed base, a translation base, a middle shell and a front gland;
the fixed base is tightly matched and fixed with a front disc of the diffractometer, and the translation base is installed on the fixed base and can slide relative to the fixed base; the middle shell is fixed on the translation base, a sample rack, a sample plate and a metal heating wire are arranged in a hollow cavity of the middle shell, one end of a binding post of the metal heating wire is connected with a heating cable of a controller through a wiring copper column, the other end of the binding post of the metal heating wire is connected with the metal heating wire in the sample rack, and the metal heating wire conducts heat to the sample plate on the upper part of the sample rack through heat conduction and heats a sample; the front gland is buckled at the front end of the middle shell in a sealing mode.
2. The detecting device for measuring the characteristics of the sample at high temperature by the X-ray diffractometer according to claim 1, characterized in that: the translation base is provided with a guide rail sliding block matched with a linear guide rail on the fixed base, and the translation differential head fixed on the fixed base through manual rotation can realize the lifting motion of the translation base relative to the fixed base; the translation base is provided with two air inlet and outlet connectors, sealing plugs are arranged at the air inlet and outlet connectors, and when inert gas is needed, the sealing plugs on the air inlet and outlet connectors can be detached to fill the middle shell with the inert gas.
3. The detecting device for measuring the characteristics of the sample at high temperature by the X-ray diffractometer according to claim 1, characterized in that: 3 sections of spiral fixture blocks in the shape of external threads are uniformly distributed on the front end of the middle shell; the bottom end of the middle shell is provided with a middle shell sealing ring to realize sealing with the translation base, and the front end of the middle shell is provided with a front gland sealing ring to realize sealing with the front gland; and a middle shell cooling copper pipe is arranged on the outer side of the middle shell sealing ring, and the middle shell sealing ring is cooled through a cooling water nozzle communicated with the cooling copper pipe and the middle shell water pipe in a circulating cooling mode.
4. The detecting device for measuring the characteristics of the sample at high temperature by the X-ray diffractometer according to claim 1, characterized in that: a temperature sensor connected with a temperature detection socket is arranged in the middle shell, the temperature sensor is arranged on the inner side of the sample plate, and the temperature sensor feeds back the temperature of the sample to the controller through a detection cable; the temperature detection socket is provided with a cooling channel, and a sealing ring of the temperature detection socket is cooled through a cooling water nozzle.
5. The detecting device for measuring the characteristics of the sample at high temperature by the X-ray diffractometer according to claim 1, characterized in that: the spiral metal heating wire is uniformly wound in the sample rack, and the extending parts at the two ends of the metal heating wire are used as a positive electrode terminal and a negative electrode terminal of the metal heating wire and are respectively connected with the positive electrode terminal and the negative electrode terminal in the metal heating wire terminal.
6. The detecting device for measuring the characteristics of the sample at high temperature by the X-ray diffractometer according to claim 1, characterized in that: the bottom of the sample rack is hermetically connected with a flow guide cavity, and the flow guide cavity is in a vacuum state; the top of the sample plate is oppositely provided with two arc-shaped radiation-proof arc plates, and when the detection device works, the sample plate is coated by the two radiation-proof arc plates.
7. The detecting device for measuring the characteristics of the sample at high temperature by the X-ray diffractometer according to claim 1, characterized in that: all there is cooling channel on the positive and negative terminal of metal heater strip terminal, gives the cooling of metal heater strip terminal sealing washer through the cooling water injection well choke, still is equipped with a temperature switch on the metal heater strip terminal, with temperature switch self-closing heating system after the temperature of metal heater strip terminal reaches temperature switch's settlement temperature.
8. The detecting device for measuring the characteristics of the sample at high temperature by the X-ray diffractometer according to claim 7, wherein: the cooling system is characterized by also comprising a cooling water inlet pipe and a cooling water outlet pipe which are connected into the cooling system of the X-ray diffractometer; the cooling water enters the temperature detection socket through the cooling water inlet pipe, enters the metal heating wire binding post through the cooling channel and then enters the other metal heating wire binding post through the metal heating wire binding post water pipe, enters the mesochite cooling copper pipe through the cooling channel and then enters the front gland cooling copper pipe through the front gland water pipe, and finally returns to the X-ray diffractometer cooling system through the cooling water outlet pipe.
9. The detecting device for measuring the characteristics of the sample at high temperature by the X-ray diffractometer according to claim 1, characterized in that: a front screw cap is arranged at the front gland, and the front screw cap is rotationally connected with the front screw cap and then is mutually rotated and locked with 3 sections of spiral clamping blocks in the shape of external threads uniformly distributed on the middle shell through 3 sections of spiral clamping blocks in the shape of internal threads uniformly distributed; the outside of preceding gland is provided with preceding radiating cover, evenly distributed multilayer annular fin on the preceding radiating cover.
10. The detecting device for measuring the characteristics of the sample at high temperature by the X-ray diffractometer according to claim 1, characterized in that: and a front gland cooling copper pipe is arranged on the front gland and is used for cooling a front gland sealing ring on the middle shell through circulating cooling with a cooling water nozzle and a front gland water pipe.
Technical Field
The invention relates to the technical field of high-temperature detection devices, in particular to a detection device for measuring sample characteristics of an X-ray diffractometer at high temperature.
Background
The X-ray diffractometer takes a Bragg experimental device as a prototype, integrates the achievements of mechanical and electronic technologies and the like, and is a diffraction experimental device which irradiates a polycrystalline sample with characteristic X-rays and records diffraction information with a radiation detector. The X-ray diffractometer can analyze the structure and composition of a substance, and can accurately measure the structure of a molecule without destroying a sample. X-ray diffraction methods are ideally very efficient for studying materials of structures, and provide a number of essential data for liquids and amorphous solids. X-ray diffraction is considered to be the most effective tool.
The conventional X-ray diffractometer can only detect a sample in normal-temperature air when testing the sample, can only measure the structure and the composition of molecules of the sample at normal temperature, can not measure the crystal structure change of the sample in high-temperature heating or the mutual dissolution change of various substances, and needs a detection device capable of detecting the crystal sample under the high-temperature condition.
Disclosure of Invention
Aiming at the problem that the crystal structure change of a sample or the mutual dissolution change of various substances in high-temperature heating cannot be measured, the invention provides a detection device for an X-ray diffractometer to measure the characteristics of the sample at high temperature.
In order to achieve the purpose, the invention provides the following scheme: the invention provides a detection device for measuring sample characteristics of an X-ray diffractometer at high temperature, which comprises a fixed base, a translation base, a middle shell and a front gland, wherein the fixed base is fixed on the middle shell; the fixed base is tightly matched and fixed with a front disc of the diffractometer, and the translation base is installed on the fixed base and can slide relative to the fixed base; the middle shell is fixed on the translation base, a sample rack, a sample plate and a metal heating wire are arranged in a hollow cavity of the middle shell, one end of a binding post of the metal heating wire is connected with a heating cable of a controller through a wiring copper column, the other end of the binding post of the metal heating wire is connected with the metal heating wire in the sample rack, and the metal heating wire conducts heat to the sample plate on the upper part of the sample rack through heat conduction and heats a sample; the front gland is buckled at the front end of the middle shell in a sealing mode.
Preferably, a guide rail sliding block matched with a linear guide rail on the fixed base is arranged on the translation base, and the translation base can move up and down relative to the fixed base by manually rotating a translation differential head fixed on the fixed base; the translation base is provided with two air inlet and outlet connectors, sealing plugs are arranged at the air inlet and outlet connectors, and when inert gas is needed, the sealing plugs on the air inlet and outlet connectors can be detached to fill the middle shell with the inert gas.
Preferably, 3 sections of spiral fixture blocks in the shape of external threads are uniformly distributed on the front end of the middle shell; the bottom end of the middle shell is provided with a middle shell sealing ring to realize sealing with the translation base, and the front end of the middle shell is provided with a front gland sealing ring to realize sealing with the front gland; and a middle shell cooling copper pipe is arranged on the outer side of the middle shell sealing ring, and the middle shell sealing ring is cooled through a cooling water nozzle communicated with the cooling copper pipe and the middle shell water pipe in a circulating cooling mode.
Preferably, a temperature sensor connected with a socket for detecting temperature is arranged inside the middle shell, the temperature sensor is arranged on the inner side of the sample plate, and the temperature sensor feeds back the temperature of the sample to the controller through a detection cable; the temperature detection socket is provided with a cooling channel, and a sealing ring of the temperature detection socket is cooled through a cooling water nozzle.
Preferably, the spiral metal heating wire is uniformly wound in the sample rack, and the extending parts at two ends of the metal heating wire are used as the positive electrode and the negative electrode of the metal heating wire and are respectively connected with the positive terminal and the negative terminal in the terminals of the metal heating wire.
Preferably, the bottom of the sample holder is hermetically connected with a flow guide cavity, and the flow guide cavity is in a vacuum state; the top of the sample plate is oppositely provided with two arc-shaped radiation-proof arc plates, and when the detection device works, the sample plate is coated by the two radiation-proof arc plates.
Preferably, all there is cooling channel on the positive and negative terminal of metal heater strip terminal, gives the cooling of metal heater strip terminal sealing washer through the cooling water injection well choke, still is equipped with a temperature switch on the metal heater strip terminal, with temperature switch self-closing heating system after the temperature of metal heater strip terminal reaches temperature switch's settlement temperature.
Preferably, the X-ray diffractometer further comprises a cooling system, wherein a cooling water inlet pipe and a cooling water outlet pipe of the cooling system are connected into the cooling system of the X-ray diffractometer; the cooling water enters the temperature detection socket through the cooling water inlet pipe, enters the metal heating wire binding post through the cooling channel and then enters the other metal heating wire binding post through the metal heating wire binding post water pipe, enters the mesochite cooling copper pipe through the cooling channel and then enters the front gland cooling copper pipe through the front gland water pipe, and finally returns to the X-ray diffractometer cooling system through the cooling water outlet pipe.
Preferably, a front screw cap is arranged at the front gland, and the front screw cap is rotationally connected with the front screw cap and then is mutually rotated and locked with 3 sections of spiral fixture blocks in the shape of external threads uniformly distributed on the middle shell through 3 sections of spiral fixture blocks in the shape of internal threads uniformly distributed on the front screw cap; the outside of preceding gland is provided with preceding radiating cover, evenly distributed multilayer annular fin on the preceding radiating cover.
Preferably, a front gland cooling copper pipe is mounted on the front gland, and the front gland cooling copper pipe cools the front gland sealing ring on the middle shell through circulating cooling with the cooling water nozzle and the front gland water pipe.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention adopts the multi-purpose sample rack to uniformly wind the spiral metal heating wires to heat the sample plate, and feeds back the temperature to the control software through the temperature sensor in the sample plate to adjust and control the heating temperature of the sample, so that the temperature of the sample on the sample plate is always stabilized at the set temperature.
The invention is provided with circulating cooling channels on the metal heating wire binding post, the temperature detection socket, the middle shell and the front gland, and the circulating cooling channels are mutually connected in series in the cooling system of the X-ray diffractometer.
The anti-radiation arc plate coats the sample plate, so that the temperature of the sample can be effectively prevented from being lost, the temperature of the sample can be kept, and the sample can be protected from being influenced by air flow when the sample is vacuumized or filled with inert gas.
The front screw cap can rotate for a certain angle on the front press cap, and then mutually rotates and locks through the 3 sections of spiral fixture blocks in the shape of internal threads which are uniformly distributed and the 3 sections of spiral fixture blocks in the shape of external threads which are uniformly distributed on the middle shell, so that the front screw cap is tightly contacted with the sealing ring on the middle shell.
According to the invention, the guide rail and the sliding block are arranged between the translation base and the fixed base, and the translation differential head fixed on the fixed base can be manually rotated to realize the lifting motion of the translation base, so that the height of the position of the middle shell fixed on the translation base can be adjusted, and the X-ray can be ensured to irradiate on the surface of the sample plate.
The invention reserves an air inlet and outlet joint and a sealing plug on the translation base. If special requirement for using inert gas exists, the sealing plug on the air inlet and outlet joint can be removed to fill inert gas into the middle shell to protect the sample from being oxidized.
According to the invention, the front heat-radiating cover is provided with the vacuum pumping hole which is a national standard KF16 vacuum connecting piece, and when a sample is detected, the middle shell can be vacuumized by the vacuum pump, so that the sample temperature is prevented from being influenced by heat loss in the air.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic structural view of the present invention;
in fig. 2, 2a is a structural schematic diagram of the translation base, and 2b is a side sectional view of the translation base;
in FIG. 3, 3a is a schematic view of the sealing and cooling structure of the middle shell, and 3b is a layout view of the sealing and cooling structure of the middle shell;
in fig. 4, 4a is a schematic diagram of a cooling structure of the front gland, and 4b is a side sectional view of the cooling structure of the front gland;
in fig. 5, 5a is a cooling cross-sectional view of the metal heating wire binding post and the temperature detection socket, 5b is a cooling side view of the metal heating wire binding post and the temperature detection socket, and 5c is a cooling connection view of the metal heating wire binding post and the temperature detection socket; 5d is a schematic cooling structure diagram of the metal heating wire binding post and the temperature detection socket;
FIG. 6 is a schematic view of the cooling water pipe connection of the detection device;
FIG. 7 is a schematic winding diagram of a metal heating wire;
in fig. 8, 8a is a schematic structural view of the front screw cap and the front gland, and 8b is a side sectional view of the front screw cap and the front gland;
fig. 9 is a schematic view of a fitting structure of the latch between the front screw cap and the middle shell.
Wherein, 1 is a fixed base, 2 is a translation base, 3 is an air inlet and outlet joint and a sealing plug, 4 is a metal heating wire binding post, 5 is a metal heating wire binding post water pipe, 6 is a temperature detection socket, 7 is a temperature detection socket water pipe, 8 is a translation differential head, 9 is a middle shell water pipe, 10 is a middle shell cooling copper pipe, 11 is a middle shell, 12 is a middle shell blocking cover, 13 is a diversion cavity, 14 is a fixed back plate, 15 is a multipurpose sample rack, 16 is a sample plate, 17 is a protective sealing film, 18 is an anti-radiation arc plate, 19 is a front gland sealing ring, 20 is a front gland, 21 is a front gland cooling copper pipe, 22 is a front heat dissipation cover, 23 is a vacuum air pumping hole, 24 is a front screw cap, 25 is a metal heating wire, 26 is a temperature sensor, 27 is a goniometer front disc, 28 is a front gland water pipe, 29 is a front heat dissipation cover sealing ring, 30 is a, 36 wiring copper columns, 37 metal heating wire wiring terminal sealing rings, 38 detection temperature socket sealing rings, 39 detection temperature sockets, 40 temperature switches, 41 cooling water inlet pipes, 42 cooling water outlet pipes and 43 front gland blocks; 44 spiral-shaped fixture block.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Aiming at the problem that the crystal structure change of a sample or the mutual dissolution change of various substances in high-temperature heating cannot be measured, the invention provides a detection device for an X-ray diffractometer to measure the characteristics of the sample at high temperature.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
As shown in fig. 1 to 9, the present embodiment provides a detection apparatus for measuring sample characteristics at high temperature by an X-ray diffractometer, which comprises a fixed base 1, a translation base 2, a middle shell 11 and a front cover. X-ray access windows are processed on two sides of the middle shell 11, a protective sealing film 17 covers the windows, and 3 spiral clamping blocks and a cooling channel of the middle shell 11 are uniformly distributed at the front end of the middle shell 11. The device comprises a translation base 2 arranged on a fixed base 1, a middle shell 11 arranged on the translation base 2, a multipurpose sample rack 15 arranged in the middle shell 11, a diversion cavity 13, a sample plate 16, a radiation-proof arc-shaped plate 18 arranged on the multipurpose sample rack 15, a
Specifically, the fixed base 1 is tightly fitted and fixed with the goniometer front disc 27, ensuring that the detection device is at the center of the optical path of the goniometer. 4 guide rail sliders 33 are arranged on the translation base 2 and are matched with linear guide rails 32 fixed on the fixed base 1, the translation differential head 8 fixed on the fixed base 1 through manual rotation can realize the lifting motion of the translation base 2, the height of the position of the middle shell 11 fixed on the translation base 2 is adjusted, and the X-ray can be irradiated on the surface of the sample plate 16.
The translation base 2 is provided with two air inlet and outlet connectors and a sealing plug 3, and if inert gas is used according to special requirements, the sealing plug 3 on the air inlet and outlet connectors can be detached to fill the inert gas into the middle shell 11 to protect the sample from being oxidized. One end of the metal heating
The multipurpose sample rack 15 is fixed on the fixed back plate 14, the spiral metal heating wire 25 is uniformly wound in the multipurpose sample rack 15, the sample is heated on the heat conduction sample plate 16 through heat conduction, and the temperature sensor 26 can accurately sense the actual temperature of the sample on the inner side of the sample plate 16. The diversion cavity 13 is hermetically connected with the multipurpose sample rack 15, and the diversion cavity 13 is in a vacuum state to prevent the heat loss of the metal heating wire 25 during heating and ensure the heating efficiency. The radiation-proof arc-shaped plates 18 are two arc-shaped covers which coat the sample plate 16 when in use, so that the heat loss of the metal heating wires 25 during heating is prevented, and the heating efficiency is ensured.
The front screw cap can rotate for a certain angle on the front press cap and then mutually rotate and lock with 3 sections of spiral fixture blocks 44 with the shape of the external thread which are uniformly distributed on the middle shell through 3 sections of spiral fixture blocks with the shape of the internal thread which are uniformly distributed, so that the front screw cap is tightly contacted with the upper sealing ring of the middle shell. The front heat radiating cover 22 is uniformly distributed with a plurality of layers of annular heat radiating fins to radiate redundant heat to ensure the temperature of the front press cover 24 and ensure the personal safety of operators. The vacuum pumping hole 23 is a standard KF16 vacuum connector and is connected with a vacuum pump for use during vacuum pumping.
As shown in fig. 2, 4 guide sliders 33 mounted on the translation base 2 are matched with the linear guide 32 fixed on the fixed base 1, and the translation base 2 can be lifted and lowered by manually rotating the translation differential head 8 fixed on the fixed base 1, so as to adjust the height of the position of the middle shell 11 fixed on the translation base 2 and ensure that the X-ray can irradiate on the surface of the sample plate 16.
As shown in fig. 3, the middle shell 11 is provided with 3 segments of spiral blocks 44 with external thread shape at the front end. The bottom end of the middle shell 11 is provided with a middle shell sealing ring 30 to realize sealing with the translation base 2, and the front end is provided with a front gland sealing ring 19 to realize sealing with the
As shown in fig. 4, the
As shown in fig. 5, the metal
As shown in fig. 6, a cooling water inlet pipe 41 and a cooling water outlet pipe 42 are connected to the cooling system of the X-ray diffractometer. The cooling water enters the
As shown in fig. 7, the metal heating wire 25 is spirally wound in the multifunctional sample holder 15, and the two ends of the metal heating wire 25 are extended to serve as the positive and negative electrodes of the metal heating wire 25 and are connected to the metal
As shown in fig. 8, 3 segments of spiral blocks 44 with internal thread shapes are uniformly distributed on the front screw cap 24. A front gland block 43 fixed by an inner hexagon screw is arranged between the spiral blocks 44,
the front gland stop 43 front section is inserted into a groove on the
As shown in fig. 9, the 3 segments of the spiral fixture blocks 44 with the shape of the internal threads uniformly distributed on the front screw cap 24 and the 3 segments of the spiral fixture blocks 44 with the shape of the external threads uniformly distributed on the middle shell 11 rotate with each other, so that the
The invention adopts the spiral metal heating wire 25 uniformly wound in the multipurpose sample rack 15 to heat the sample plate 16, and feeds back the temperature to the control software through the temperature sensor 26 in the sample plate 16 to adjust and control the heating temperature of the sample, so that the temperature of the sample on the sample plate 16 is always stabilized at the set temperature.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any reference signs in the claims are not intended to be construed as limiting the claim concerned.
The principle and the implementation mode of the invention are explained by applying a specific example, and the description of the embodiment is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
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