1. A temperature control accessory for an X-ray diffractometer is characterized in that: the device comprises a sample table, wherein a clamping table is arranged on the sample table, a clamping shaft is rotatably connected onto the clamping table, a clamping piece which is horizontally and slidably connected with the clamping table is in threaded connection onto the clamping shaft, and the clamping piece moves in the same direction or in the opposite direction when the clamping shaft rotates;

the sample table is provided with a cavity which is communicated with a first valve, the first valve is communicated with a negative pressure pump, the periphery of the cavity is provided with an annular channel, a plurality of ceramic tubes which are abutted against the clamping table are arranged in the cavity, spiral electric coils are arranged in the ceramic tubes, and two ends of each ceramic tube are communicated with the channel;

the channel is communicated with an inlet pipe and an outlet pipe, the inlet pipe is communicated with a second valve, the outlet pipe is communicated with a third valve, the second valve is communicated with an air path system, and liquid nitrogen or air is input into the second valve through the air path system.

2. The temperature-controlled attachment for an X-ray diffractometer according to claim 1, wherein: the gas path system comprises a reversing valve, the outlet end of the reversing valve is communicated with a second valve, the inlet end of one side of the reversing valve is communicated with a liquid nitrogen tank, and the other inlet end of the reversing valve is communicated with a pump assembly.

3. The temperature-controlled attachment for an X-ray diffractometer according to claim 2, wherein: the clamping table is provided with a temperature sensor which is electrically connected with a controller, and the controller is electrically connected with a display.

4. The temperature-controlled attachment for an X-ray diffractometer according to claim 3, wherein: the sample table is provided with a groove, the groove is internally threaded with a cover body, the cover body is provided with an opening, the opening is provided with a sealing ring, the clamping table is provided with a through hole, and the through hole is communicated with the cavity.

5. The temperature-controlled attachment for an X-ray diffractometer according to claim 4, wherein: and a lead sealing ring is arranged on the sample table, and both the spiral electric ring and the lead of the temperature sensor penetrate through the lead sealing ring.

6. The temperature-control attachment for an X-ray diffractometer according to any one of claims 1 to 5, wherein: the sample table is provided with a flange.

7. The temperature-control attachment for an X-ray diffractometer according to any one of claims 1 to 5, wherein: the bottom of the sample table is provided with a plurality of connecting shafts.

8. The temperature-controlled attachment for an X-ray diffractometer according to claim 1, wherein: the ceramic tube is integrally formed with a throat tube section, the throat tube section is provided with a communicating hole communicated with the cavity, the spiral electric ring is in running fit with the ceramic tube, a heat conducting plate used for sealing the communicating hole is fixed on the spiral electric ring, the spiral electric ring is fixedly connected with the sample feeding tube, and the sample feeding tube is in running connection with the sample table.

9. The temperature-controlled attachment for an X-ray diffractometer according to claim 3, wherein: the controller is electrically connected with a buzzer.

10. The temperature-controlled attachment for an X-ray diffractometer according to claim 1, wherein: both ends of the clamping shaft are provided with circular limiting parts.

Background

The X-ray diffractometer takes a Bragg experimental device as a prototype, integrates the achievements of mechanical and electronic technologies and the like, is a diffraction experimental device which irradiates a polycrystalline sample with characteristic X-rays and records diffraction information with a radiation detector, can analyze the structure and composition of a substance, and can accurately measure the structure of a molecule without damaging the sample. X-ray diffraction methods are ideally very effective for studying materials of structures, and for liquids and amorphous solids, provide a number of essential data, and are therefore considered the most effective tools.

Generally, the measurement of the molecular and compositional structure of a material is performed at normal temperature, and in order to better measure the data of the material, the material needs to be heated or cooled to measure the influence of temperature change on the structure of the material.

Disclosure of Invention

The invention aims to provide a temperature control accessory for an X-ray diffractometer, which is used for heating or cooling a material and is convenient for measuring the influence of temperature change on the structure of the material.

In order to achieve the above object, the basic scheme of the invention is as follows: a temperature control accessory for an X-ray diffractometer comprises a sample table, wherein a clamping table is arranged on the sample table, a clamping shaft is rotatably connected onto the clamping table, a clamping piece which is horizontally and slidably connected with the clamping table is in threaded connection onto the clamping shaft, and the clamping piece moves in the same direction or in the opposite direction when the clamping shaft rotates;

the sample table is provided with a cavity which is communicated with a first valve, the first valve is communicated with a negative pressure pump, the periphery of the cavity is provided with an annular channel, a plurality of ceramic tubes which are abutted against the clamping table are arranged in the cavity, spiral electric coils are arranged in the ceramic tubes, and two ends of each ceramic tube are communicated with the channel;

the channel is communicated with an inlet pipe and an outlet pipe, the inlet pipe is communicated with a second valve, the outlet pipe is communicated with a third valve, the second valve is communicated with an air path system, and liquid nitrogen or air is input into the second valve through the air path system.

The principle and the beneficial effects of the invention are as follows: (1) in this scheme, rotate the centre gripping axle, can be so that the holding piece syntropy or reverse motion to make the material that the holding piece can the not equidimension of centre gripping, carry out the centre gripping to the material, improve the stability among the measurement process.

(2) In this scheme, to spiral coil circular telegram to heating ceramic tube and centre gripping platform, in order to heat the material, make the material intensification, when needs carry out the low temperature measurement, open first valve, let in the air through the gas circuit system to ceramic tube, in order to lower the temperature to ceramic tube and centre gripping platform, reach the normal atmospheric temperature state (open the third valve with air escape). Then liquid nitrogen is input through the gas path system to cool the ceramic tube, the clamping table and the material so as to achieve the purpose of cooling.

Of course, the application does not necessarily require that all of the above-described technical effects be achieved at the same time.

Further, the gas path system comprises a reversing valve, the outlet end of the reversing valve is communicated with the second valve, the inlet end of one side of the reversing valve is communicated with a liquid nitrogen tank, and the other inlet end of the reversing valve is communicated with a pump assembly.

Has the advantages that: in this scheme, when the switching-over valve communicates second valve and pump package spare, the pump package spare lets in the air to ceramic pipe, utilizes the air cooling, can be so that material temperature variation is not too big, reduces the probability that changes the material structure, reuses the liquid nitrogen and cools down to the material to reach the purpose of cooling down rapidly. Of course, in this scheme, a single process may be performed, that is, only the temperature of the material is raised, or only the temperature of the material is lowered.

Further, a temperature sensor is installed on the clamping table and electrically connected with a controller, and a display is electrically connected with the controller.

Has the advantages that: in this scheme, temperature sensor is in order to detect the temperature of the material that awaits measuring to show specific temperature information through the display, operating personnel adjusts the power of spiral coil according to temperature information, or changes the volume that lets in the liquid nitrogen, so that operating personnel can controllable regulation material temperature.

Furthermore, a groove is formed in the sample table, a cover body is connected with the groove in a threaded mode, an opening is formed in the cover body, a sealing ring is arranged on the opening, a through hole is formed in the clamping table, and the through hole is communicated with the cavity.

Has the advantages that: in this scheme, the utilization cover body covers the material to be measured, stretches into to cover the internal when the X diffraction source through the opening to make the cover body basically sealed, when to the cavity evacuation, through the through-hole to cover internal evacuation, so that the material to be measured is in vacuum environment basically, reaches the purpose of protective material, avoids material temperature variation too fast. Certainly, the ceramic tube is positioned in the cavity, the cavity is vacuumized, the too fast temperature change of the ceramic tube can be reduced, and the purpose of heat preservation is basically achieved.

Furthermore, a lead sealing ring is arranged on the sample table, and both the spiral electric ring and the lead of the temperature sensor penetrate through the lead sealing ring.

Has the advantages that: the lead is led out through the lead sealing ring, and meanwhile, the purpose of sealing the cavity can be achieved.

Furthermore, a flange plate is arranged on the sample table.

Has the advantages that: the sample stage was mounted laterally by a flange plate housing.

Further, the bottom of the sample table is provided with a plurality of connecting shafts.

Has the advantages that: the sample table can be horizontally installed through the connecting shaft.

Further, a throat pipe section is integrally formed on the ceramic pipe, a communicating hole communicated with the cavity is formed in the throat pipe section, a spiral electric ring is in rotating fit with the ceramic pipe, a heat conducting plate used for sealing the communicating hole is fixed on the spiral electric ring, the spiral electric ring is fixedly connected with a feeding pipe, and the feeding pipe is rotatably connected with the sample platform.

Has the advantages that: in this scheme, when letting in the air to ceramic tube, the utilization is advanced the pipe and is rotated, and then advances the pipe and drive the rotation of spiral coil to make intercommunicating pore and cavity intercommunication, during the initial time, the velocity of flow of air is slower, and partial air fills to the cavity, and when gradual air flow rate accelerated, produces certain negative pressure under the effect of larynx pipeline section, takes away the impurity in the cavity, also can blow away the impurity in the ceramic tube, resets the spiral coil at last, is about to the intercommunicating pore and seals. When liquid nitrogen is filled into the ceramic tube, the influence of impurities on the liquid nitrogen is reduced, and the subsequent influence on cavity vacuumizing can also be reduced.

Further, the controller is electrically connected with a buzzer.

Has the advantages that: if the temperature is too high, the controller gives an alarm through the buzzer.

Furthermore, both ends of the clamping shaft are provided with limiting parts which are circular.

Has the advantages that: the limiting piece limits the clamping piece to prevent the limiting piece from sliding out of the clamping shaft.

Drawings

FIG. 1 is an isometric view of a temperature-controlled attachment for an X-ray diffractometer in accordance with one embodiment of the present invention;

FIG. 2 is a top view of a temperature-controlled attachment for an X-ray diffractometer in accordance with one embodiment of the present invention;

FIG. 3 is a sectional view taken along line A-A of FIG. 2;

FIG. 4 is a sectional view taken along line B-B of FIG. 2;

FIG. 5 is a schematic diagram of a gas circuit system of a temperature control accessory for an X-ray diffractometer according to an embodiment of the present invention;

fig. 6 is a schematic structural view of a ceramic tube in the temperature control attachment for an X-ray diffractometer according to the second embodiment of the present invention.

Detailed Description

In the following, the technical solutions in the embodiments of the present invention will be clearly and completely described with reference to the accompanying 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 embodiments.

In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.

Reference numerals in the drawings of the specification include: the device comprises a sample table 11, a channel 111, a groove 12, a cover body 121, a clamping table 13, a through hole 131, a clamping shaft 14, a clamping piece 15, a flange 16, an inlet pipe 17, a second valve 171, a temperature sensor 18, an outlet pipe 19, a third valve 191, a ceramic pipe 21, a spiral coil 22, a first valve 23, a cavity 24, a connecting shaft 25, a lead sealing ring 26, a communication hole 27, a heat conducting piece 28, a liquid nitrogen tank 31, an air pump 32 and a reversing valve 33.

The first embodiment is as follows:

substantially as shown in figures 1, 2, 3, 4 and 5: the utility model provides a accuse temperature annex that X ray diffractometer was used, includes sample platform 11, and the bolt fastening has the faraday dish on sample platform 11, and the bottom of sample platform 11 is provided with connecting axle 25, and connecting axle 25 is the screw rod, in this embodiment, can transversely install sample platform 11 on the diffractometer through ring flange 16, can be with sample platform 11 vertical connection on the diffractometer through the screw rod.

A circular clamping table 13 is detachably connected to the sample table 11, a clamping shaft 14 is rotatably connected to the clamping table 13, and limiting pieces are fixed to two ends of the clamping shaft 14 and are nuts; the division of centre gripping axle 14 both sides has the opposite screw thread of direction of rotation, and the equal threaded connection in both ends of centre gripping axle 14 has holding piece 15, and when centre gripping axle 14 forward rotation, holding piece 15 syntropy motion, when centre gripping axle 14 antiport, holding piece 15 antiport. In this way, materials to be tested of different sizes can be clamped. The clamping table 13 is provided with a through hole 131, and the temperature sensor 18 is fixed on the clamping table 13 through screws. The sample stage 11 is provided with a groove 12, the groove 12 is connected with an arc-shaped cover body 121 in a threaded manner, the cover body 121 is made of a transparent glass material, the cover body 121 is provided with an opening, and a sealing ring is installed on the opening.

The sample table 11 is provided with a cavity 24 communicated with the through hole 131, the cavity 24 is communicated with a first valve 23, the first valve 23 is communicated with a negative pressure pump, an annular passage 111 is formed in the periphery of the cavity 24, a plurality of ceramic tubes 21 are installed in the cavity 24, the ceramic tubes 21 are abutted to the clamping table 13, the clamping table 13 is made of ceramic materials, and two ends of each ceramic tube 21 are communicated with the passage 111. In this embodiment, a spiral coil 22 is installed in a ceramic tube 21, a lead of the spiral coil 22 penetrates through the ceramic tube 21, a lead sealing ring 26 is fixed on a sample stage 11, both the lead of the spiral coil 22 and a temperature sensor 18 penetrate through the lead sealing ring 26, the lead of the spiral coil 22 is connected with a power supply, the lead of the temperature sensor 18 is connected with a controller, and the controller is electrically connected with a display and a buzzer.

In this embodiment, one side of the sample stage 11 is communicated with an inlet pipe 17, the inlet pipe 17 is communicated with the channel 111, the inlet pipe 17 is communicated with the second valve 171, the other side of the sample stage 11 is provided with an outlet pipe 19, the outlet pipe 19 is communicated with the channel 111, the outlet pipe 19 is communicated with a third valve 191, and the third valve 191 is communicated with a waste recovery device. The second valve 171 is communicated with an air path system, the air path system in this embodiment includes a reversing valve 33, an outlet end of the reversing valve 33 is communicated with the second valve 171, one inlet end of the reversing valve 33 is communicated with the liquid nitrogen tank 31, the other inlet end of the reversing valve 33 is communicated with a pump assembly, and the pump assembly is an air pump 32.

The specific implementation process is as follows:

in this embodiment, the clamping table 13 can be detached from the sample table 11, then the material to be tested is placed on the clamping table 13, and the clamping shaft 14 is rotated forward or backward, so that the clamping plate moves towards the material to be tested or away from the material to be tested, and the material to be tested with different sizes is clamped.

After the clamping is completed, the holding stage 13 is placed on the sample stage 11, and the holding stage 13 abuts against the ceramic tube 21 (the holding stage 13 is sufficiently in contact with the ceramic tube 21). The cover body 121 is installed in the groove 12 to cover the material to be measured, the emission head of the diffractometer extends into the cover body 121 through the opening and aligns to the material to be measured, and at the moment, the cover body 121 is basically in a sealed state.

When heating is needed, the cavity 24 is vacuumized in advance through the negative pressure pump, the cavity 24 is vacuumized through the through hole 131, so that the material to be measured and the ceramic tube 21 are basically in a vacuum state, the spiral electric coil 22 is started, the spiral electric coil 22 heats the ceramic tube 21, and the ceramic tube 21 conducts heat transfer on the clamping table 13 until the material to be measured is heated to a certain temperature. The temperature sensor 18 transmits the temperature signal of the material to be measured to the controller, the controller obtains the temperature information and displays the temperature information through the display, and when the temperature is too high or too low, the power of the spiral coil 22 is adjusted to achieve the purpose of temperature regulation. The ceramic tube 21 is in the vacuum cavity 24, so that the temperature of the ceramic tube 21 can be prevented from changing too fast.

When needing to cool down, close spiral electric circle 22, open second valve 171 and third valve 191, communicate second valve 171 and air pump 32 through switching-over valve 33, air pump 32 lets in the air to passageway 111 and ceramic tube 21, utilize the air to cool down ceramic tube 21 and grip slipper 13, until cooling to the material to be measured, utilize the air to cool down, can be unlikely to the temperature variation of the material to be measured too fast, when the display shows that the temperature is the normal atmospheric temperature, seal third valve 191, rethread switching-over valve 33 communicates second valve 171 with liquid nitrogen container 31, pour into the liquid nitrogen into ceramic tube 21 through liquid nitrogen container 31, carry out rapid cooling to the material to be measured through the liquid nitrogen. The process is a continuous temperature change process, can effectively raise or lower the temperature, and improves the temperature control efficiency of the whole process.

In this embodiment, can utilize spiral coil 22 alone to heat up, also can utilize the liquid nitrogen alone to cool down, two systems can be independent to reach the purpose of accuse temperature.

Example two:

the difference between the second embodiment and the first embodiment is that, as shown in fig. 6, a plurality of throat sections are integrally formed on the ceramic tube 21, a communication hole 27 communicated with the cavity 24 is formed on the throat sections, a heat conducting fin 28 for closing the communication hole 27 is fixed on the spiral electric coil 22, the spiral electric coil 22 is fixedly connected with the sample inlet tube 17, and the sample inlet tube 17 is rotatably connected with the sample stage 11.

The specific implementation process is as follows:

in this embodiment, the cavity 24 and the ceramic tube 21 may be cleaned to some extent, specifically: when the clamping piece 15 clamps the material to be tested, some powder may be caused to be on the clamping table 13 or in the cavity 24. When impurities such as dust need to be cleaned, an operator rotates the inlet pipe 17, and the inlet pipe 17 drives the spiral coil 22 to rotate, so that the heat conducting plate and the communication hole 27 are staggered.

A certain amount of air is fed into the ceramic tube 21 through the air pump 32, part of the air enters the cavity 24, negative pressure in the cavity 24 and the cover body 121 is lost, then the feeding amount of the air pump 32 is increased, the flow rate of the air in the ceramic tube 21 is increased, negative pressure is formed at the throat section, and under the action of the negative pressure, dust and the like enter the ceramic tube 21 along with air flow and are discharged through the outlet tube 19. And impurities are discharged, and the influence of the impurities on temperature rise and temperature reduction is reduced.

When letting in liquid nitrogen, reset spiral coil 22 again and make ceramic tube 21 seal, carry out the evacuation to cavity 24 again, also can discharge powder etc. certainly during the evacuation, this embodiment uses the cooperation of two kinds of modes, the residue of minimize powder.

The foregoing is merely an example of the present invention and common general knowledge in the art of specific structures and/or features of the invention has not been set forth herein in any way. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.