Heating device capable of gathering heat and high-temperature and high-pressure diamond anvil cell system

Abstract

The utility model discloses a heating device capable of gathering heat and a high-temperature and high-pressure diamond anvil cell system, which comprise a heating device body, the top of the heating device body is subjected to lower pressure, the bottom of the heating device body is subjected to upper pressure, and the action lines of the lower pressure and the upper pressure coincide. An upper anvil head and a lower anvil head arranged on the diamond anvil assembly can be close to each other under the action of lower pressure and upper pressure; the heating assembly is provided with a ceramic ring, the upper anvil head and the lower anvil head which are close to each other intersect in the central area of the ceramic ring, and the central area can form a high-temperature area. The resistance wire is wound on the ceramic ring to generate heat which is conducted to the central area to form the high-temperature area, so that the experimental environment of the central area can reach a high-temperature and high-pressure environment required by a test sample under the high pressure of the upper anvil head and the lower anvil head and the high temperature of the high-temperature area, and the temperature change rate of the ceramic ring is improved; the physical property of the sample can be conveniently researched.

Description

TECHNICAL FIELD

[0001] The utility model relates to high temperature high pressure under physical quantity in situ measuring device technical field, concretely relates to a kind of heating device and high temperature high pressure diamond anvil cell system that can gather heat. BACKGROUND

[0002] DAC device is diamond anvil cell, a kind of high-pressure experimental device, which is widely used in physics, earth science and material science and other fields, for studying the properties of matter under extremely high pressure conditions.This device mainly includes the following mechanisms: diamond anvil mechanism, pressure mechanism, heating mechanism, its working principle is to use the two or more carefully polished micro diamonds included in the diamond anvil mechanism to apply hydrostatic pressure to the sample, the sample is placed between the tips of the two diamonds, and the pressure mechanism (such as hydraulic pump or screw mechanism) is used to apply pressure to the diamond anvil seat, so as to study the physical phenomena such as high-pressure phase transition of sample material under extreme pressure environment.Secondly, the sample is heated by the heating mechanism, so as to study the physical phenomena such as material structure and superconducting characteristics of sample material under extreme environment of high temperature and high pressure.

[0003] The existing diamond anvil cell heating sample method has laser heating, which uses focused laser beam to directly irradiate the sample to quickly raise its temperature, and the laser beam is divergent after irradiating the sample, so that the heat is radiated to the surrounding, this heating method not only causes serious heat loss, but also increases the floor area and use cost of the equipment; there is also resistance wire heating, which surrounds the upper and lower anvil seats without affecting the pressing of the sample by the upper and lower anvil heads, the resistance wire and the upper and lower anvil seats form a sample cavity, and the heat generated by the resistance wire after being electrified is radiated to the surrounding, part of the heat gradually accumulates in the sample cavity, so that the lowest temperature gradient appears in the middle region of the sample cavity, this heating method not only causes a large amount of heat to be unable to accumulate in the sample cavity, resulting in heat loss, but also makes the environmental temperature of the sample unable to change in time, thereby unable to quickly change the temperature of the sample, which affects the high temperature and high pressure experiment. SUMMARY

[0004] The utility model provides a kind of heating device and high temperature high pressure diamond anvil cell system that can gather heat to solve the existing diamond anvil cell heating sample problem, and the specific technical solutions are as follows:

[0005] A heating device capable of gathering heat, comprising a heating device body, the top of the heating device body is subjected to a vertical downward pressure, the bottom of the heating device body is subjected to a vertical upward pressure, the action lines of the downward pressure and the upward pressure coincide, the heating device body comprises: a diamond anvil assembly, the diamond anvil assembly is provided with an upper anvil head and a lower anvil head, the upper anvil head and the lower anvil head can be close to each other under the action of the downward pressure and the upward pressure; and a heating assembly, the heating assembly is provided with a ceramic ring, the upper anvil head and the lower anvil head close to each other intersect at a central region of the ceramic ring, and the central region can form a high-temperature region.

[0006] Further, the heating assembly further comprises a resistance wire, the resistance wire is uniformly wound on the outer surface of the ceramic ring along the radial direction of the ceramic ring, the heat generated by the resistance wire being electrified is conducted to the ceramic ring, and the heat is radiated by the inner surface of the inner ring of the ceramic ring to gather in the central region of the ceramic ring to form the high-temperature region.

[0007] Further, a groove for placing the resistance wire is formed on the outer surface of the ceramic ring along the radial direction of the ceramic ring, and the highest point of the resistance wire arranged in the groove does not exceed the mounting surface of the ceramic ring.

[0008] Preferably, the heating assembly further comprises a heat insulation gasket arranged between the upper anvil head and the ceramic ring, and the heat insulation gasket can completely cover the overlapping region of the ceramic ring and the upper anvil head.

[0009] Preferably, the diamond anvil assembly further comprises an upper shell and a lower shell subjected to the downward pressure and the upward pressure respectively, the upper anvil head is arranged at the bottom center position of the upper shell, the axis of the upper anvil head coincides with the axis of the upper shell, the lower anvil head is arranged at the top center position of the lower shell, the axis of the lower anvil head coincides with the axis of the lower shell, the upper shell and the lower shell drive the upper anvil head and the lower anvil head to be close to each other when they are close to each other, the sample to be measured is fixed at the top center position of the lower anvil head, and the upper anvil head and the lower anvil head close to each other can exert high pressure on the sample to be measured and fix it in the high-temperature region.

[0010] Preferably, the diamond anvil assembly further comprises: an upper anvil seat arranged at the bottom of the upper shell, the top of the upper anvil head is inlaid at the bottom of the upper anvil seat, and the axes of the upper anvil seat, the upper anvil head and the upper shell coincide; a lower anvil seat arranged at the top of the lower shell, the bottom of the lower anvil head is inlaid at the top of the lower anvil seat, and the axes of the lower shell, the lower anvil seat and the lower anvil head coincide; the total distance of the upper anvil head and the lower anvil head moving to be close to each other to extrude the sample to be measured is A; and the upper shell is formed with at least two open grooves in the axial direction, the open grooves are symmetrical about the center line of the upper shell, the length of the open grooves in the axial direction is B, and A≤B.

[0011] Preferably, the heating assembly further comprises a thermocouple passing through the open groove, one end of the thermocouple is connected to the inner surface of the inner ring of the ceramic ring.

[0012] Preferably, comprising: the heating device body as described above; and a pressurizing assembly that applies upper and lower pressures to the bottom and top of the heating device body, respectively.

[0013] From the above technical solution, the utility model has the following beneficial effects:

[0014] The utility model discloses a heating device for diamond anvil cell, which comprises a heating device body and a pressurizing assembly, wherein the heating device body comprises a ceramic ring, a heating assembly and a thermocouple, the ceramic ring is arranged on the upper end of the heating assembly, the heating assembly is arranged on the lower end of the heating device body, and the thermocouple is arranged on the ceramic ring. BRIEF DESCRIPTION OF DRAWINGS

[0015] Figure 1 It is a structural schematic diagram of the utility model embodiment.

[0016] Figure 2 It is Figure 1 Partial enlarged view.

[0017] In the figure: 1, heating device body;2, pressurizing assembly;11, diamond anvil assembly;12, heating assembly;111, upper anvil head;112, upper anvil seat;113, upper shell;114, lower anvil head;115, lower anvil seat;116, lower shell;117, opening groove;121, ceramic ring;122, recess;123, resistance wire;124, thermocouple;125, heat insulation gasket DETAILED DESCRIPTION

[0018] The technical solutions in the utility model embodiments will be clearly and completely described below with reference to the drawings in the utility model embodiments. Obviously, the described embodiments are only part of the embodiments of the utility model, rather than all the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the utility model.

[0019] In the description of the embodiments of the utility model, it needs to be explained that the directions or position relations indicated by the terms "inner", "outer", "upper" and the like are based on the directions or position relations shown in the drawings, or are the directions or position relations in which the utility model product is usually placed during use, which is only for the convenience of describing the utility model and simplifying the description, and does not indicate or imply that the indicated device or element must have a specific direction, be constructed and operated in a specific direction, and therefore cannot be understood as a limitation on the utility model.

[0020] Embodiment one

[0021] As Figure 1 shown, the utility model embodiment includes heating device body 1, the top surface of heating device body 1 is subjected to vertical downward pressure, the bottom surface of heating device body 1 is subjected to vertical upward pressure, the action line of downward pressure and upward pressure coincides, heating device body 1 includes: diamond anvil assembly 11, the diamond anvil assembly 11 is provided with upper anvil head 111 and lower anvil head 114, and upper anvil head 111 and lower anvil head 114 can approach each other under the action of downward pressure and upward pressure, and heating assembly 12 is provided with ceramic ring 121, and upper anvil head 111 and lower anvil head 114 approach each other and intersect at the central region of ceramic ring 121, and the central region can form a high-temperature region.

[0022] Specifically, the downward pressure and upward pressure of heating device body 1 are applied by screw rod feeding mechanism or hydraulic system, which can exert pressure on diamond anvil assembly 11, so that upper anvil head 111 and lower anvil head 114 move, and then upper anvil head 111 and lower anvil head 114 can simultaneously exert high pressure on the sample placed between them and coaxial with them.

[0023] Secondly, the fixing mode of ceramic ring 121 and upper anvil head 111 and lower anvil head 114 has various forms, and in the embodiment, the position of ceramic ring 121 and upper anvil head 111 is fixedly unchanged, and this fixing mode is that the top surface of ceramic ring 121 is fixedly connected with upper anvil head 111, so that ceramic ring 121 moves with the movement of upper anvil head 111, at this time, upper anvil head 111 is always in the central region of ceramic ring 121, and the sample to be measured is placed on the top surface of lower anvil head 114 and coaxial with them, so that when upper anvil head 111 tightly presses lower anvil head 114, both are in the central region of ceramic ring 121.

[0024] In the preferred embodiment, the ceramic ring 121 is in the shape of a circular ring, and the axis of the ceramic ring 121 coincides with the axis of the upper anvil head 111, so that the outer surface of the upper anvil head 111 is equidistant from the inner ring surface of the ceramic ring 121, and the conduction efficiency of the heat generated by the middle region of the ceramic ring 121 to the upper anvil head 111 is the same, and the heating effect of the ceramic ring 121 on each point of the upper anvil head 111 is the same, and the heating effect of the ceramic ring 121 on the sample to be tested is the same.

[0025] The central region of the ceramic ring 121 refers to the region surrounded by the inner ring inner surface and the bottom of the upper anvil head 111 and the top of the lower anvil head 114. A portion of the heat conducted to the ceramic ring 121 is concentrated in the central region, so that the temperature in the central region rises rapidly to form a high-temperature temperature field, and the experimental environment of the sample is high temperature and high pressure, meeting the experimental requirements.

[0026] As shown in Figure 2 Further, the heating assembly 12 further comprises a resistance wire 123, which is uniformly wound on the outer surface of the ceramic ring 121 along the radial direction of the ceramic ring 121. The heat generated by the resistance wire 123 is conducted to the ceramic ring 121, and the heat is radiated to the central region of the ceramic ring 121 through the inner ring inner surface of the ceramic ring 121 to form a high-temperature region.

[0027] Specifically, in the present embodiment, the material of the resistance wire 123 is preferably platinum wire. The platinum wire has a high melting point, good thermal conductivity and good electrical conductivity, so that the platinum wire can continuously generate heat after being electrified, and the highest temperature generated by the platinum wire is about 700 degrees Celsius, which meets the experimental requirements of the sample, and the resistance wire 123 wound on the ceramic ring 121 can conduct the heat to the ceramic ring 121 with low loss, and the temperature of the high-temperature temperature field formed in the central region of the ceramic ring 121 can reach 700 degrees Celsius.

[0028] Secondly, the resistance wire 123 is uniformly wound along the radial direction of the ceramic ring 121, so that the heat conducted by the electrified resistance wire 123 to each point of the ceramic ring 121 is the same, and the heat radiated outward by each point of the ceramic ring 121 is the same. Part of the heat is radiated to the central region along the radial direction of the ceramic ring 121, and the heat in the central region can be concentrated to form a high-temperature temperature field, and the heat radiation values in each direction are equal, so that the temperature of the high-temperature temperature field is distributed in a ring shape, and the temperature decreases step by step from the inside to the outside. The closer to the inner ring inner surface of the ceramic ring 121, the higher the temperature, and the closer to the center line of the ceramic ring 121, the lower the temperature. However, because the volume of the ceramic ring 121 is very small, the temperature in the central region is equal, which meets the experimental requirements.

[0029] Further, the outer surface of the ceramic ring 121 is formed with grooves 122 for placing the resistance wire 123 along the radial direction of the ceramic ring 121, and the highest point of the resistance wire 123 arranged in the grooves 122 does not exceed the mounting surface of the ceramic ring 121.

[0030] Specifically, the number of the grooves 122 in the preferred embodiment is 21. When the number of the grooves 122 is small, the total length of the resistance wire 123 wound on the ceramic ring 121 is short, so that the total resistance of the resistance wire 123 is small, and when the total voltage applied to the resistance wire 123 is unchanged, the total current of the resistance wire 123 is large, thus generating more heat, which makes the platinum wire easy to be burnt out. When the number of the grooves 122 is large, the resistance wire 123 gathered on the inner surface of the inner ring of the ceramic ring 121 is large, thus the gathered heat is large, and the platinum wire is easy to be burnt out.

[0031] Secondly, the resistance wire 123 is completely placed in the grooves 122, so that the heat conducted by the resistance wire 123 to the ceramic ring 121 is as little as possible, thus accelerating the heat gathering speed of the ceramic ring 121 and improving the experimental efficiency. Secondly, the complete placement of the resistance wire 123 in the grooves 122 also makes there be no gap between the mounting surface of the ceramic ring 121 and the contact surface of the upper anvil head 111, thus preventing the heat from gathering and burning out the platinum wire.

[0032] Further, the heating assembly 12 further comprises a heat insulation gasket 125 arranged between the upper anvil head 111 and the ceramic ring 121, which can completely cover the overlapping area of the ceramic ring 121 and the upper anvil head 111.

[0033] Specifically, the upper and lower surfaces of the heat insulation gasket 125 are fixedly connected with the upper anvil head 111 and the ceramic ring 121 by high-temperature cement, so that the movement state of the ceramic ring 121 is the same as that of the upper anvil head 111, and the heat of the ceramic ring 121 cannot be conducted to the upper anvil head 111, thus avoiding the reduction of the service life of the upper anvil head 111 due to heating. Therefore, the heat insulation gasket 125 needs to completely separate the ceramic ring 121 and the upper anvil head 111, so as to ensure that the heat of the ceramic ring 121 cannot be conducted to the upper anvil head 111, and improve the heat insulation effect of the heat insulation gasket 125.

[0034] Further, the diamond anvil assembly 11 further comprises an upper shell 113 and a lower shell 116 subjected to the upper pressure and the lower pressure respectively, the upper anvil head 111 is arranged at the bottom center of the upper shell 113, the axis of the upper anvil head 111 coincides with the axis of the upper shell 113, the lower anvil head 114 is arranged at the top center of the lower shell 116, the axis of the lower anvil head 114 coincides with the axis of the lower shell 116, the upper shell 113 and the lower shell 116 are close to each other to drive the upper anvil head 111 and the lower anvil head 114 to be close to each other, the sample to be measured is fixed at the top center of the lower anvil head 114, and the upper anvil head 111 and the lower anvil head 114 close to each other can apply high pressure to the sample to be measured and fix it in a high temperature area.

[0035] Specifically, the upper shell 113 and the lower shell 116 are connected by a bolt with a spring, when the pressing assembly 2 presses the upper shell 113 downward, the upper shell 113 moves downward along the bolt, the upper anvil head 111 connected at the bottom center of the upper shell 113 moves downward to press the lower anvil head 114, as known, the contact parts of the upper anvil head 111 and the lower anvil head 114 are the top surfaces of the two, the sample is placed at the center of the top surface, and the upper anvil head 111 and the lower anvil head 114 press the sample to make the sample in a high temperature and high pressure environment.

[0036] Further, the diamond anvil assembly 11 further comprises: an upper anvil seat 112 arranged at the bottom of the upper shell 113, the top of the upper anvil head 111 is inlaid at the bottom of the upper anvil seat 112, the axes of the upper anvil seat 112, the upper anvil head 111 and the upper shell 113 coincide; a lower anvil seat 115 arranged at the top of the lower shell 116, the bottom of the lower anvil head 114 is inlaid at the top of the lower anvil seat 115, the axes of the lower anvil seat 115, the lower anvil head 114 and the lower shell 116 coincide; the total distance of the movement of the upper anvil head 111 and the lower anvil head 114 close to each other to press the sample to be measured is A; and the upper shell 113 forms at least two open grooves 117 in the axial direction, the open grooves 117 are symmetrical about the center line of the upper shell 113, the length of the open grooves 117 in the axial direction is B, and A≤B.

[0037] Specifically, the top surface of the upper shell 113 is formed with a conical upper cavity for placing the pressing assembly 2, and the bottom of the upper shell 113 is fixedly connected with an upper anvil seat 112 corresponding to the upper cavity, the bottom of the upper anvil seat 112 is fixedly connected with an upper anvil head 111, the center lines of the upper anvil seat 112, the upper cavity and the upper anvil head 111 coincide, so that the pressure action line of the pressing assembly 2 on the upper anvil head 111 through the upper cavity and the upper anvil seat 112 coincides with the center line, and then the pressure of the upper anvil head 111 on the sample is vertically downward.

[0038] Meanwhile, the bottom of the lower shell 116 is formed with a conical lower cavity for placing the pressing assembly 2, and the top of the lower shell 116 is fixedly connected with a lower anvil seat 115 corresponding to the lower cavity, the top of the lower anvil seat 115 is fixedly connected with a lower anvil head 114, the center lines of the lower anvil seat 115, the lower cavity and the lower anvil head 114 coincide, so that the pressure action line of the pressing assembly 2 on the lower anvil head 114 through the lower cavity and the lower anvil seat 115 coincides with the center line, and then the pressure of the lower anvil head 114 on the sample is vertically upward.

[0039] Secondly, the total distance of the movement of the upper anvil head 111 and the lower anvil head 114 close to each other to extrude the sample to be tested is A, which is the distance of the movement of the upper anvil head 111 along the screw to press the lower anvil head 114, so that there is a space between the upper anvil head 111 and the lower anvil head 114 before moving for operating the sample. Figure 1 It can be seen that the outer surface of the upper shell 113 moves up and down along the inner surface of the lower shell 116, the resistance wire 123 connected with the ceramic ring 121 is connected with the external power source through the open slot 117, under the pressure of the pressing assembly 2, the vertical pressure received by the lower shell 116 and the upper shell 113 is very large, and the symmetrically formed open slot 117 can reduce the stress deformation of the lower shell 116 and ensure the service life of the equipment; A≤B makes the open slot 117 not hinder the movement of the upper shell 113 to the lower shell 116, and then hinder the extrusion of the sample by the upper anvil head 111 and the lower anvil head 114.

[0040] Further, the heating assembly 12 further comprises a thermocouple 124 passing through the open slot 117, one end of the thermocouple 124 is connected with the inner surface of the ceramic ring 121.

[0041] Specifically, the thermocouple 124 is usually composed of two conductors or semiconductors of different materials, and the two conductors are welded together at one end to form a working end, and the other end is kept at a known temperature, called the reference end, in this embodiment, the working end of the thermocouple 124 is connected to the inner surface of the inner ring of the ceramic ring 121, and the temperature of the high-temperature temperature field of the central area is measured, due to the temperature difference between the two ends, a electromotive force proportional to the temperature difference will be generated in the thermocouple 124 loop, which is firm and durable, fast response, wide measurement range, so that it can obtain the temperature of the high-temperature temperature field in real time, and further stabilize the temperature of the experimental environment of the sample, and carry out sample experiments under high pressure and high temperature conditions.

[0042] Embodiment two

[0043] The second embodiment includes the heating device body 1 in the first embodiment; and a pressurizing assembly 2, which respectively applies upper pressure and lower pressure to the bottom and top of the heating device body 1.

[0044] Specifically, the pressurizing assembly 2 applies upper pressure and lower pressure to the bottom and top of the heating device body 1 through a screw feeding mechanism or a hydraulic system, respectively, wherein the action lines of the upper pressure and the lower pressure coincide, so that the heating device body 1 can do telescopic motion under the action of the pressurizing assembly 2, so that the upper anvil head 111 and the lower anvil head 114 can reach the required pressure value of the experimental pressure on the sample to be measured, thereby meeting the experimental requirements.

[0045] Although the embodiments of the utility model have been shown and described, it can be understood by those skilled in the art that various changes, modifications, replacements and variations can be made to these embodiments without departing from the principles and spirits of the utility model, and the scope of the utility model is defined by the appended claims and their equivalents.

[0046] The technical, shape and structure parts not described in detail in the utility model are well-known technologies.

Claims

1. A heating device capable of gathering heat, comprising a heating device body (1), the top of the heating device body (1) is subjected to a vertical downward pressing force, the bottom of the heating device body (1) is subjected to a vertical upward pressing force, the action lines of the downward pressing force and the upward pressing force coincide, characterized in that, The heating device body (1) comprises: a diamond anvil assembly (11) provided with an upper anvil head (111) and a lower anvil head (114) capable of approaching each other under the action of the lower pressure and the upper pressure; and a heating assembly (12) provided with a ceramic ring (121), the upper anvil head (111) and the lower anvil head (114) approaching each other intersect at the central region of the ceramic ring (121), and the central region can form a high-temperature region.

2. The heating device of claim 1, wherein: The heating assembly (12) further comprises a resistance wire (123) uniformly wound on the outer surface of the ceramic ring (121) along the radial direction of the ceramic ring (121), and the heat generated by the resistance wire (123) is conducted to the ceramic ring (121), and the heat is radiated through the inner surface of the inner ring of the ceramic ring (121) to gather in the central region of the ceramic ring (121) to form the high-temperature region.

3. The heating device of claim 2, wherein: A groove (122) for placing the resistance wire (123) is formed on the outer surface of the ceramic ring (121) along the radial direction of the ceramic ring (121), and the highest point of the resistance wire (123) arranged in the groove (122) does not exceed the mounting surface of the ceramic ring (121).

4. The heating device of claim 3, wherein: The heating assembly (12) further comprises a heat insulation gasket (125) arranged between the upper anvil head (111) and the ceramic ring (121), which can completely cover the overlapping region of the ceramic ring (121) and the upper anvil head (111).

5. The heating device of claim 4, wherein: The diamond anvil assembly (11) further comprises an upper shell (113) and a lower shell (116) respectively subjected to the lower pressure and the upper pressure, the upper anvil head (111) is arranged at the bottom center position of the upper shell (113), the axis of the upper anvil head (111) coincides with the axis of the upper shell (113), the lower anvil head (114) is arranged at the top center position of the lower shell (116), the axis of the lower anvil head (114) coincides with the axis of the lower shell (116), and the upper shell (113) and the lower shell (116) drive the upper anvil head (111) and the lower anvil head (114) to approach each other when they approach each other, the sample to be tested is fixed at the top center position of the lower anvil head (114), and the upper anvil head (111) and the lower anvil head (114) approaching each other can apply high pressure to the sample to be tested and fix it in the high-temperature region.

6. The heating device of claim 5, wherein: The diamond anvil assembly (11) further comprises: an upper anvil seat (112) arranged at the bottom of the upper shell (113), the top of the upper anvil head (111) is inlaid at the bottom of the upper anvil seat (112), and the axes of the upper anvil seat (112), the upper anvil head (111) and the upper shell (113) coincide; A lower anvil head (114) is set on the top of the lower shell (116), the bottom of the lower anvil head (114) is inlaid on the top of the lower anvil seat (115), the axis of the lower shell (116), the lower anvil seat (115) and the lower anvil head (114) coincide; The total distance of the movement of the upper anvil head (111) and the lower anvil head (114) to each other to extrude the sample to be tested is A; and the upper shell (113) is formed with at least two open grooves (117) in the axial direction, the open grooves (117) are symmetrical about the center line of the upper shell (113), the length of the axial direction of the open grooves (117) is B, A≤B.

7. The heating device of claim 6, wherein: The heating assembly (12) further comprises a thermocouple (124) passing through the open groove (117), one end of the thermocouple (124) is connected to the inner surface of the inner ring of the ceramic ring (121).

8. A high pressure high temperature diamond anvil cell system, characterized by, Comprise: The heating device body (1) according to claim 7; and a pressurizing assembly (2) for applying upper pressure and lower pressure to the bottom and top of the heating device body (1) respectively.

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