Multi-sample cell hanging and high temperature resistant fuse electrode device

Abstract

The present application relates to the field of calorimetric device, specifically to a kind of multi-sample cell hanging and high-temperature-resistant fuse electrode device, including electrode plug, electrode stick component and sample cell, wherein electrode plug includes electrode column, electrode cap and electrode sleeve, each electrode column is arranged in electrode sleeve, electrode cap is arranged on the upper end of electrode sleeve, and the part exposed after the upper end of electrode column passes through the electrode sleeve forms electrode joint, the electrode stick component includes multiple electrode sticks, and the lower end of the electrode column is connected with corresponding electrode stick, electrode stick with same length forms a group of electrode stick groups, and sample cell is hung at the lower end of corresponding electrode stick group by fuse wire.The present application can simultaneously hang multiple sample cells, realize fast and convenient replacement of sample cell in high-temperature furnace, greatly improve experimental efficiency, and can work at a maximum of 1800K high temperature.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of calorimetric device, in particular to a multi-sample cell hanging and high-temperature-resistant fuse electrode device. BACKGROUND

[0002] Heat capacity is the sum of the energy contribution of the lattice, electrons and other forms of motion inside the material system, which is a basic thermophysical parameter of the material. Through the accurate determination of heat capacity, the basic thermodynamic data such as enthalpy, entropy, Gibbs free energy of the material can be obtained, and then the structure and phase transition of the material can be understood. In addition, it is also a method to obtain the lattice vibration of the microstructure of the material, the electronic energy level transition, and to understand the superconducting phenomenon, the mechanism of magnetic action, and the structural distortion. Therefore, obtaining accurate data of high-temperature heat capacity of the material is of great significance for exploring and designing new materials, optimizing the preparation process of materials, promoting the understanding and development of material science, etc.

[0003] Drop calorimetry is one of the most accurate and reliable methods for determining the heat capacity of a material at high temperatures. However, this method has some drawbacks such as long testing time, high temperature, sample changing difficulty, sample dropping inconvenience, and the need for operators to have certain professional knowledge. These limitations restrict its development and use. Therefore, it is particularly important to develop a drop calorimetry device that is simple to operate, easy to change samples, stable in performance, has a high and wide working temperature range, and high accuracy. One of the most critical aspects is the optimization of the sample cell dropping method and structure to ensure good stability, fast sample dropping, easy sample changing, and long-term repeated use of the fuse electrode in high-temperature environments.

[0004] Currently, the representative high-temperature calorimetric systems in the field of drop calorimetry include ice calorimeter, water calorimeter, and copper block calorimeter. However, the fuse electrode of these drop calorimetric devices can only hang one sample cell at a time. After each experiment, the temperature needs to be lowered and raised again, which is time-consuming and inefficient. Moreover, the repeatability and reliability are poor at high temperatures, which is not conducive to controlling the experimental time in high-temperature environments. Long-term opening of the furnace cover also leads to large heat leakage, making the furnace chamber susceptible to sudden cooling, reducing the accuracy of the instrument. In addition, the maximum temperature of the fuse electrode of these three calorimetric devices does not exceed 1000K, which seriously affects their application. SUMMARY

[0005] The purpose of the present application is to provide a multi-sample cell hanging and high-temperature-resistant fuse electrode device that can simultaneously hang multiple sample cells, achieve fast and convenient sample cell replacement in a high-temperature furnace, greatly improve experimental efficiency, and work at a maximum temperature of 1800K. At the same time, it effectively ensures the accuracy of the drop tube calorimeter, allowing the sample cell to be conveniently positioned at the center of the tube-type high-temperature furnace.

[0006] The purpose of the present application is achieved by the following technical solutions:

[0007] A high-temperature-resistant fuse electrode device for suspending multiple sample cells comprises electrode plugs, electrode rod assemblies and sample cells, wherein the electrode plug comprises electrode columns, an electrode cap and an electrode sleeve, each electrode column is arranged in the electrode sleeve, the electrode cap is arranged at the upper end of the electrode sleeve, and the exposed part of the upper end of the electrode column after passing through the electrode sleeve forms an electrode joint, the electrode rod assembly comprises multiple electrode rods, and the lower end of the electrode column is connected with the corresponding electrode rod, the electrode rods with the same length form a group of electrode rod assemblies, and the sample cell is suspended at the lower end of the corresponding electrode rod assembly through a fuse wire.

[0008] The electrode sleeve and the electrode cap are both provided with through holes for the electrode column to pass through, and the outer side of the electrode column is wrapped with an insulating ceramic layer.

[0009] The exposed metal at the top of the electrode column forms an electrode joint.

[0010] The lower end of the electrode column forms a first connecting end, the upper end of the electrode rod forms a second connecting end, and the first connecting end is threadedly connected with the corresponding second connecting end.

[0011] The first connecting end is an internally threaded end provided with an internally threaded hole, and the second connecting end is an externally threaded column end.

[0012] The electrode cap is provided with clamping grooves on both sides.

[0013] As viewed along the axial direction of the electrode column, each electrode column is uniformly distributed along the circumferential direction, and two electrode rods belonging to the same electrode rod assembly are symmetrically arranged.

[0014] The lower end of the electrode rod is provided with a hook, the two ends of the fuse wire are respectively hung on the hooks at the lower ends of different electrode rods in the corresponding electrode rod assembly, and the upper end of the sample cell is provided with a hanging ring hung on the fuse wire.

[0015] Each sample cell is sequentially arranged along the vertical direction.

[0016] During testing, the electrode sleeve is butt-jointed and inserted into the furnace mouth of the tubular high-temperature furnace.

[0017] The advantages and positive effects of the present application are as follows:

[0018] 1. The design of the fuse wire and multiple electrode rod assemblies can realize the suspension of multiple sample cells, the fuse wire can be fused at any time by controlling the power supply of the electrode column and the electrode rod, and the sample cell can fall under the action of gravity, so that the replacement of each sample cell in the high-temperature furnace is more simple and fast, the experimental efficiency is effectively improved, and the control flexibility is more flexible.

[0019] 2、The electrode column and the electrode rod are used in cooperation, the furnace mouth of the tubular high-temperature furnace can be effectively blocked, a large amount of heat leakage in the furnace is avoided, and each component is made of high-temperature resistant material, so that the electrode column and the electrode rod are wrapped with the insulating ceramic layer to realize effective insulation, the lower end of the electrode column and the upper end of the corresponding electrode rod are screw-connected, the replacement of the electrode rod is facilitated, and the sample pool is directly contacted with other components in the high-temperature furnace.

[0020] 3、The electrode column and the electrode rod are wrapped with the insulating ceramic layer to realize effective insulation, and the lower end of the electrode column and the upper end of the corresponding electrode rod are screw-connected, facilitating replacement of the electrode rod.

[0021] 4、The combination is simple and convenient to disassemble, and direct contact of the sample pool with other components in the high-temperature furnace is avoided. BRIEF DESCRIPTION OF DRAWINGS

[0022] Figure 1 is a schematic view of the overall structure of the present application,

[0023] Figure 2 is a schematic view of the electrode plug structure in the present application, Figure 1

[0024] is a schematic view of the electrode rod and the sample pool structure in the present application. Figure 3 Figure 1

[0025] Among them, 1 is an electrode plug, 101 is an electrode column, 1011 is an electrode connector, 1012 is a first connecting end, 102 is an electrode cap, 1021 is a clamping groove, 103 is an electrode sleeve, 2 is an electrode rod, 201 is a first electrode rod group, 202 is a second electrode rod group, 203 is a third electrode rod group, 204 is a second connecting end, 205 is a hook, 3 is a sample pool, and 301 is a fuse. DETAILED DESCRIPTION

[0026] The present application will be further described in detail below with reference to the drawings.

[0027] As shown in the drawings, the present application comprises an electrode plug 1, an electrode rod assembly and a sample pool 3, wherein the electrode plug 1 comprises an electrode column 101, an electrode cap 102 and an electrode sleeve 103, each electrode column 101 is arranged in the electrode sleeve 103, the electrode cap 102 is arranged at the upper end of the electrode sleeve 103, and the part of the electrode column 101 exposed after penetrating through the electrode sleeve 103 forms an electrode connector 1011, the electrode rod assembly comprises a plurality of electrode rods 2, the lower end of the electrode column 101 is connected with the corresponding electrode rod 2, the electrode rods 2 with the same length form a group of electrode rod groups, and the sample pool 3 is hung at the lower end of the corresponding electrode rod group through a fuse 301. Figures 1 to 3

[0028] ​​​In this embodiment, the electrode column 101 is made of high-temperature-resistant metal rod, the electrode sleeve 103 and the electrode cap 102 are both provided with a through hole for the electrode column 101 to pass through, the outer side of the electrode column 101 is wrapped with an insulating ceramic layer in contact with the electrode sleeve 103 and the electrode cap 102, and the top of the electrode column 101 is bare metal to form an electrode joint 1011.

[0029] As shown in Figures 1 to 3 the lower end of the electrode column 101 forms a first connecting end 1012, the upper end of the electrode rod 2 forms a second connecting end 204, and the first connecting end 1012 is threadedly connected with the corresponding second connecting end 204, in this embodiment, the first connecting end 1012 is an internally threaded end with an internally threaded hole, and the second connecting end 204 is an externally threaded column end.

[0030] As shown in Figure 2 the two sides of the electrode cap 102 are provided with clamping grooves 1021 for fixing the electrode plug 1, the electrode sleeve 103 is a metal tubular structure, and the upper end is sealingly welded with the electrode cap 102 to protect the electrode column 101 and can be docked with the furnace mouth of a high-temperature furnace to achieve dynamic sealing.

[0031] As shown in Figure 3 In this embodiment, the electrode rod assembly includes six electrode rods 2, the two shortest electrode rods 2 form a first electrode rod group 201, the two electrode rods 2 of intermediate length form a second electrode rod group 202, and the two longest electrode rods 2 form a third electrode rod group 203, this embodiment includes three sample pools 3 arranged from top to bottom, and the uppermost sample pool 3 is hung at the lower end of the first electrode rod group 201, the middle sample pool 3 is hung at the lower end of the second electrode rod group 202, and the lowermost sample pool 3 is hung at the lower end of the third electrode rod group 203.

[0032] As shown in Figure 3 In this embodiment, the lower end of the electrode rod 2 is provided with a hook 205, the two ends of the fuse 301 are respectively hung on the hooks 205 at the lower ends of different electrode rods in the corresponding electrode rod group, and the upper end of the sample pool 3 is provided with a hanging ring hung on the fuse 301.

[0033] When viewed along the axial direction of the electrode column 101, each electrode column 101 is uniformly distributed along the circumferential direction, and the two electrode rods 2 belonging to the same electrode rod group are symmetrically arranged, and the six electrode rods 2 in this embodiment are uniformly distributed along the circumferential direction to form a regular hexagon.

[0034] The number of electrode rods 2 can be set according to actual needs.

[0035] In the embodiment, the electrode cap 102 is made of nickel-based alloy material, with a diameter of 30-80mm and a height of 20-50mm, and six holes with a diameter of 1-5mm are arranged through the electrode cap 102, and a clamping groove 1021 is arranged on each side of the electrode cap 102.

[0036] In the embodiment, the electrode column 101 is a tungsten wire wrapped by insulating ceramic, with an outer diameter of 1-5mm, and a first connecting end 1012 on the lower side of the electrode column 101 has an inner threaded hole with an inner diameter of 0.8-4.8mm and a length of 100-500mm.

[0037] In the embodiment, the electrode column 101 is a tubular structure made of nickel-based alloy material, with an inner diameter of 20-70mm, an outer diameter of 25-75mm, and a height of 90-400mm.

[0038] In the embodiment, the electrode rod 2 is a tungsten wire structure wrapped by ceramic, with an outer diameter of 0.8-4.8mm, wherein the first electrode rod group 201 with the shortest length is 100-200mm long, the second electrode rod group 202 with the middle length is 150-250mm long, and the third electrode rod group 203 with the longest length is 250-300mm long, and the second connecting end 204 on the upper side of the electrode rod 2 has an outer threaded diameter of 0.8-4.8mm.

[0039] In the embodiment, the fuse wire 301 is made of nickel wire with a purity of 99.9%, with a wire diameter of 0.1-0.5mm and a length of 50-150mm, and the two ends of the fuse wire 301 are bent into a circular shape to form a fuse wire hanger ring which is hung on the corresponding hook 205 at the lower end of the electrode rod 2.

[0040] In the embodiment, the sample cell 3 is a hollow bottle body made of nickel-based alloy material, with an inner diameter of 10-15mm, an outer diameter of 15-20mm, and a height of 40-60mm, and the sample cell 3 is arranged in the center of the fuse electrode in an upward, middle, and downward order, and the vertical direction spacing between the sample cells 3 is 5-10mm.

[0041] The working principle of the present application is as follows:

[0042] The falling-type calorimeter heats the sample cell 3 in the high-temperature furnace, and when the set temperature is reached, the electrode column 101 and the electrode rod 2 are connected to 24V direct current, causing the fuse wire 301 to be sequentially fused from bottom to top, and the sample cell 3 is sequentially lowered from bottom to top into the calorimeter under the action of gravity, and then data collection and high-temperature specific heat measurement are performed, so the present application is one of the important components in the design of the falling-type calorimeter.

[0043] The present application specifically adopts the following steps to measure the temperature of the sample cell 3:

[0044] (1) The second connecting end 204 at the top of the electrode rod 2 is threaded to the first connecting end 1012 at the bottom of the electrode post 101. In this embodiment, each electrode rod 2 constituting the first electrode rod group 201, the second electrode rod group 202 and the third electrode rod group 203 is evenly distributed in a regular hexagonal pattern along the circumferential direction when viewed from the axial direction, and the two electrode rods 2 in the same electrode rod group are arranged diagonally.

[0045] (2) Fix the electrode slot 1021 to the lifting frame of the high temperature furnace so that the whole invention is perpendicular to the horizontal plane.

[0046] (3) Clean the inside and outside of sample cell 3 three times with anhydrous ethanol, and then wash it three times with deionized water.

[0047] (4) Dry and bake each component of sample cell 3, cool it to room temperature, weigh it three times and take the average value;

[0048] (5) Place the sample into sample cell 3 and weigh it three times, taking the average value;

[0049] (6) Pass the fuse 301 through the hanging ring at the top of the sample cell 3;

[0050] (7) Hang the two ends of the fuse 301 on the hooks 205 at the lower end of the corresponding electrode rod 2 to complete the suspension of the sample cell 3. The sample cell 3 is suspended in order from top to bottom.

[0051] (8) The present invention with the sample cell 3 suspended is slowly placed into the tubular high-temperature furnace of the drop-in high-temperature calorimeter by the lifting frame, wherein the electrode sleeve 103 is inserted into the furnace mouth, and the electrode cap 102 and the electrode connector 1011 above are exposed.

[0052] (9) Clamp the electrode clips connected to the DC power supply onto the corresponding electrode connectors 101 respectively, so that the two electrode connectors 101 of each electrode group are energized, and the energization is not distinguished by positive and negative poles.

[0053] (10) Turn on the tubular high temperature furnace to start the test. When the temperature reaches the set point, control the closed DC power switch to melt the fuse 301 in sequence, so that the sample cell 3 falls from bottom to top in sequence.

[0054] (11) After the sample is dropped, close the tubular high-temperature furnace, wait for the temperature inside the furnace to drop to below 200 degrees, remove the six electrode clamps, and raise the present invention.

[0055] (12) After cooling to room temperature, clean the remaining threads on hook 205 before using it again.

[0056] The application can meet the requirements of temperature, accuracy and good repeatability of the falling-in high temperature calorimeter, realize efficient experiment of three measurements of the furnace body in one-time heating, avoid repeated heating and cooling process of the furnace body, and still has perfect functionality at 1800K high temperature.

Claims

1. A fusible electrode device for suspending multiple sample cells and resistant to high temperatures, characterized in that: The device includes an electrode plug (1), an electrode rod assembly, and a sample cell (3). The electrode plug (1) includes an electrode post (101), an electrode cap (102), and an electrode sleeve (103). Each electrode post (101) is located in the electrode sleeve (103). The electrode cap (102) is located at the upper end of the electrode sleeve (103). The part of the upper end of the electrode post (101) that is exposed after passing through the electrode sleeve (103) forms an electrode connector (1011). The electrode rod assembly includes multiple electrode rods (2). The lower end of the electrode post (101) is connected to the corresponding electrode rod (2). Electrode rods (2) of the same length form a group of electrode rods. The sample cell (3) is suspended from the lower end of the corresponding electrode rod group by a fuse (301). The lower end of the electrode post (101) forms a first connection end (1012), and the upper end of the electrode rod (2) forms a second connection end (204), and the first connection end (1012) is threadedly connected to the corresponding second connection end (204); Looking along the axial direction of the electrode post (101), each electrode post (101) is evenly distributed along the circumferential direction, and two electrode rods (2) belonging to the same electrode rod group are symmetrically arranged. The lower end of the electrode rod (2) is provided with a hook (205), and the two ends of the fuse (301) are respectively hung on the hooks (205) at the lower end of different electrode rods in the corresponding electrode rod group. The upper end of the sample cell (3) is provided with a hanging ring that is hung on the fuse (301). Each sample cell (3) is set up sequentially along the vertical direction.

2. The fusible electrode device for suspending multiple sample cells and with high temperature resistance according to claim 1, characterized in that: Both the electrode sleeve (103) and the electrode cap (102) are provided with through holes for the electrode post (101) to pass through, and the electrode post (101) is wrapped with an insulating ceramic layer on the outside.

3. The fusible electrode device for suspending multiple sample cells and with high temperature resistance according to claim 1, characterized in that: The exposed metal at the top of the electrode post (101) forms an electrode connector (1011).

4. The fusible electrode device for suspending multiple sample cells and with high temperature resistance according to claim 1, characterized in that: The first connecting end (1012) is an internally threaded end with an internally threaded hole, and the second connecting end (204) is an externally threaded column end.

5. The fusible electrode device for suspending multiple sample cells and with high temperature resistance according to claim 1, characterized in that: The electrode cap (102) has slots (1021) on both sides.

Images