CN117630094A - Fusing electrode device for falling-type high-temperature calorimeter and application method thereof - Google Patents

Fusing electrode device for falling-type high-temperature calorimeter and application method thereof Download PDF

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CN117630094A
CN117630094A CN202210980166.9A CN202210980166A CN117630094A CN 117630094 A CN117630094 A CN 117630094A CN 202210980166 A CN202210980166 A CN 202210980166A CN 117630094 A CN117630094 A CN 117630094A
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electrode
fusing
center
temperature
sample cell
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史全
吴冰
尹楠
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/20Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity

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Abstract

The invention relates to a high Wen Liang heat device in calorimetric field, in particular to a fusing electrode device for a falling-type high-temperature calorimeter and a use method thereof, wherein an electrode rod group penetrates through an electrode plug body and is of a sealing structure, a hook is arranged at the lower end of the electrode rod group, and an electrode joint is arranged at the upper end of the electrode rod group; the electrode plug body is provided with a penetrated electrode hole, the outside of the electrode plug is provided with a sealing ring, the electrode cap and the electrode plug are provided with six electrode holes, and the electrode connector and the electrode center column can pass through and are fixed with the electrode plug body; the electrode rod group comprises five electrode struts and an electrode center column, an electrode joint is arranged at the top end of each electrode strut, an electrode strut inner hook is arranged at the lower end of each electrode strut, a hollow cylinder is arranged below each electrode center column and provided with an electrode center column side hook, the hooks of the electrode rod group are used for hanging fusible links, the fusible links are used for hanging sample cells, and interference does not exist between any two sample cells. The invention has compact structure, novel design, flexible use, high temperature resistance and capability of effectively improving experimental efficiency by suspending a plurality of sample tanks.

Description

Fusing electrode device for falling-type high-temperature calorimeter and application method thereof
Technical Field
The invention relates to a high Wen Liang heat device in calorimetric field, in particular to a fusing electrode device for a falling type high temperature calorimeter and a use method thereof.
Background
The heat capacity is the sum of energy contributions of movement forms such as crystal lattice, electrons and the like in a substance system, and is one basic thermophysical parameter of a substance. Basic thermodynamic data such as enthalpy, entropy and Gibbs free energy of a substance can be obtained through accurate measurement of heat capacity, and the method for knowing the structure and phase change of the substance is also a method for obtaining lattice vibration and electron energy level transition of a microstructure of the substance and understanding superconducting phenomenon, magnetic action mechanism and structural distortion. Therefore, obtaining accurate data of the material height Wen Rerong has important significance for developing and designing new materials, optimizing the preparation process of the materials and promoting the understanding and development of material science.
Falling type calorimeter is one of the most accurate and reliable methods for measuring the heat capacity of a substance at high temperature, however, the defects of long test time, high temperature, troublesome sample changing, inconvenient sample falling, certain expertise required by operators and the like limit the development and use of the falling type calorimeter; therefore, the development and control are succinct, the sample change is convenient, the performance is stable, the working temperature area is high and wide, and the drop-in type heat measuring device with high accuracy is particularly important. One of the most critical links is that the sample cell falls into optimization of the method and structure, so that the sample cell has better stability, can realize quick sample falling and convenient replacement of the sample cell, and simultaneously ensures long-time repeated use of the fusing electrode in a high-temperature environment.
Currently, the high Wen Liang thermal systems that are internationally representative of the fall within the high Wen Liang thermal research area include an ice calorimeter, a water calorimeter, and a copper block calorimeter. However, the fusing electrode of the drop-in type high Wen Liang heat device can only hang one pool at a time, and the temperature is reduced and raised again after each experiment is finished; the method has the advantages of troublesome operation, low efficiency, poor repeatability and reliability at high temperature, unfavorable control of experiment time in a higher temperature environment, large heat leakage caused by long-term opening of the furnace cover, easy influence of quenching on the furnace hearth and reduced precision of the furnace. Meanwhile, the highest temperature of the fusing electrode of the three heat measuring devices does not exceed 1000K, and the application of the three heat measuring devices is seriously influenced.
Therefore, development of a fusing electrode which is compact in structure, excellent in performance, novel in design, efficient and resistant to high temperature is urgently needed to meet urgent needs of research on heat capacity properties of high-temperature substances.
Disclosure of Invention
The invention aims to provide a fusing electrode device for a falling-in type high-temperature calorimeter and a use method thereof, aiming at the defects of the fusing electrode of the existing high Wen Laru calorimeter. The fusing electrode device has strong high temperature resistance, can greatly improve experimental efficiency, realizes quick and convenient replacement of samples, and can work at 1500K at the highest temperature; meanwhile, the accuracy and precision of the drop-in calorimeter are not damaged, and the sample cell and the fusing electrode can be conveniently fixed at the central position of the vertical tube type high-temperature furnace body.
The aim of the invention is realized by the following technical scheme:
the fusing electrode device comprises an electrode plug body, an electrode rod group and a sample cell group, wherein the upper part of the electrode plug body is an electrode cap, the lower part of the electrode plug body is an electrode plug, the center of the electrode plug body is provided with a central electrode hole along the axial direction, the periphery of the central electrode hole is uniformly provided with a plurality of electrode holes along the circumferential direction, and the electrode plug is provided with a sealing ring; the electrode rod group comprises electrode center posts and electrode struts which are the same in number and in one-to-one correspondence with the electrode holes, the electrode center posts penetrate through the center electrode holes, the top ends of the electrode center posts are positioned outside the electrode plug body, the bottom ends of the electrode center posts are hollow cylinders, and a plurality of electrode center post side hooks are uniformly arranged at the bottoms of the hollow cylinders along the circumferential direction; each electrode pillar is respectively penetrated in the corresponding electrode hole, the top end of each electrode pillar is an electrode joint positioned outside the electrode plug body, the bottom end of each electrode pillar is provided with electrode pillar inner hooks, the number of the electrode center pillar side hooks is the same as that of the electrode pillar inner hooks and corresponds to that of the electrode pillar inner hooks one by one, and each electrode pillar inner hook is connected with the corresponding electrode center pillar side hook through a fuse wire; the sample cell group is provided with a plurality of sample cells, each fusible link is suspended with a sample cell, and the sample cells fall into the high-temperature calorimeter after the fusible links are electrified and fused.
Wherein: the electrode plug and the electrode cap are both cylinders, the diameter of the electrode cap is larger than that of the electrode plug, and the electrode hole and the central electrode hole are through holes penetrating through the electrode plug body.
The aperture of each electrode hole is equal and smaller than that of the central electrode hole.
The electrode plug is provided with a groove, and the sealing ring is accommodated in the groove; the sealing ring is an O-shaped ring, and the outer diameter of the sealing ring is larger than the diameter of the electrode plug.
The contact part of the electrode center column and the electrode plug body and the contact part of the electrode support column and the electrode plug body are wrapped and bonded by an insulating ceramic layer.
The electrode center column is a hollow cylinder with a closed top end, and the outer diameter of the hollow cylinder is larger than the outer diameter of other parts of the electrode center column.
The length of the electrode support is smaller than that of the electrode center column, when the fusing electrode device is vertically installed, hooks in the electrode support are arranged at equal heights and higher than the hooks on the electrode center column side, the sample Chi Xiang is hung on the fuse wire, the centers of the sample Chi Xiang are close, and each sample cell is arranged at the center of a high-temperature area of a hearth of the high-temperature furnace.
The two ends of the fuse wire are annular, the annular ring at one end is hung on the inner hook of the electrode pillar, and the other end is hung on the corresponding side hook of the electrode center pillar.
Each fusible link, the electrode joint connected with the fusible link and the electrode center post form a series direct current circuit, the fusing of the fusible links is controlled, so that a sample cell hung on the fusible links is controlled to fall into a high-temperature calorimeter, the fusing sequence of a plurality of fusible links is arranged, and the sample cell hung on each fusible link is controlled to fall down in sequence according to the fusing sequence.
The invention relates to a method for using a fusing electrode device of a falling type high temperature calorimeter, which comprises the following steps of
Step one, cleaning each sample cell;
step two, drying and baking each sample cell, cooling to room temperature, weighing for multiple times, and taking an average value;
step three, filling a sample into each sample cell, weighing for multiple times, and taking an average value;
suspending the fusing electrode device on a lifting support frame of a furnace mouth of the high-temperature furnace, wherein the fusing electrode device is vertical to a horizontal plane, and the vertical distance between the hooks in the electrode support column and the hooks on the side of the electrode center column and the upper surface of the furnace body of the high-temperature furnace is larger than a set distance;
step five, respectively penetrating through the fusible links in hanging holes at the top end of each sample cell, and respectively hanging two ends of each fusible link on hooks in a corresponding group of electrode support posts and hooks at the side of an electrode center post, wherein the sample cells are hung in a vertical state due to traction of the two ends of the fusible links;
step six, vertically dropping the fusing electrode device with the suspended sample cells until the electrode plugs plug the furnace mouth of the high-temperature furnace, and sealing by the sealing rings, wherein the electrode caps and the parts above are exposed out of the high-temperature furnace, and each sample cell stays in a hot end temperature zone in a hearth of the high-temperature furnace;
step seven, respectively clamping a negative electrode connected with a direct current power supply on an electrode joint at the top end of each electrode support column, clamping a positive electrode at the top end of the electrode central column, forming a loop by the electrode central column connected with the positive electrode and the electrode support column connected with each negative electrode, wherein the positive electrode and the negative electrode can be mutually exchanged;
step eight, fixing the fusing electrode device and the lead of the connected electrode joint, and connecting a 48V direct current power supply and a switching relay at the other end of the electrode;
step nine, a high-temperature furnace is opened to start testing, when the temperature reaches a set value, a direct-current power switch is controlled to be closed, each fuse wire is fused in sequence, and each sample cell falls down in sequence according to the control of the switch;
step ten, after sample falling is finished, closing the high-temperature furnace, taking out the electrode clamp after the temperature in the furnace is reduced to be within a set temperature, and lifting the fusing electrode device;
and step eleven, after cooling the electrode support post, cleaning residual wires left on hooks in the electrode support post and hooks on the electrode center post side, and waiting for the next continuous use.
The invention has the advantages and positive effects that:
1. the invention has fine design and high temperature resistance, so that the electrode and the sample cell can be fused and sample-falling work under the high temperature environment of 1500K.
2. The invention can effectively block the furnace mouth of the tubular high-temperature furnace and prevent a large amount of heat leakage in the furnace through the matched use of the electrode plug and the electrode cap.
3. According to the invention, the contact part of the electrode rod group and the electrode plug body is wrapped with the insulating ceramic, and the sealing ring on the electrode plug can realize the sealing in the high-temperature furnace body and the insulation between the electrode plug body and the electrode rod group.
4. The suspension mode of the fusible link, the electrode rod group and the sample cells ensures that at most five sample cells can be placed in the furnace, the replacement is simpler and faster, the experimental efficiency can be effectively improved, and the operability is more flexible.
5. The electrode wire and the fusible link can normally work in a high-temperature environment, and the fusible link can be fused at any time, so that the sample cell can be dropped down in sequence due to no suspension.
6. The invention has simple combination and convenient installation and use, and the heating furnace area not only improves the effective heating efficiency in the middle of the furnace body, but also avoids the direct contact between the sample cell and other built-in parts in the high temperature furnace.
Drawings
FIG. 1 is a schematic view showing the overall structure of a fusing electrode device of the present disclosure;
FIG. 2 is a schematic view of the structure of an electrode plug body in the fusing electrode device of the present invention;
FIG. 3 is a schematic view of the structure of an electrode bar set in the fusing electrode device of the present disclosure;
FIG. 4 is a schematic view showing the arrangement of an electrode hook and a sample cell in the fusing electrode device of the present invention;
wherein: 1 is an electrode plug body, 101 is an electrode hole, 102 is a central electrode hole, 103 is a sealing ring, 104 is an electrode plug, 105 is an electrode cap, 2 is an electrode rod group, 201 is an electrode joint, 202 is an electrode central column, 203 is an electrode pillar, 204 is a hollow cylinder, 3 is a sample cell group, 301 is an electrode inner hook, 302 is a side hook, 303 is a fuse, and 304 is a sample cell.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings.
As shown in fig. 1 to 4, the fusing electrode device of the invention comprises an electrode plug body 1, an electrode rod group 2 and a sample cell group 3, wherein the upper part of the electrode plug body 1 is provided with an electrode cap 105, the lower part is provided with an electrode plug 104, the center of the electrode plug body 1 is provided with a central electrode hole 102 along the axial direction, the periphery of the central electrode hole 102 is uniformly provided with a plurality of electrode holes 101 along the circumferential direction, and the electrode plug 104 is provided with a sealing ring 103, so that the electrode plug 104 and the furnace mouth of a high-temperature furnace can be tightly sealed; the electrode rod group 2 comprises electrode center posts 202 and electrode support posts 203 which are the same as the electrode holes 101 in number and correspond to each other one by one, the electrode center posts 202 penetrate through the center electrode holes 102, the top ends of the electrode center posts 202 are positioned outside the electrode plug body 1, the bottom ends of the electrode center posts 202 are hollow cylinders 204, and a plurality of electrode center post side hooks 302 are uniformly arranged at the bottoms of the hollow cylinders 204 along the circumferential direction; each electrode pillar 203 is respectively penetrated in the corresponding electrode hole 102, the top end of the electrode pillar 203 is an electrode joint 201 positioned outside the electrode plug body 1, the bottom end of the electrode pillar 203 is provided with electrode pillar inner hooks 301, the number of electrode center pillar side hooks 302 is the same as that of the electrode pillar inner hooks 301 and corresponds to that of the electrode pillar inner hooks 301 one by one, and each electrode pillar inner hook 301 is connected with the corresponding electrode center pillar side hook 302 through a fuse wire 303; the sample cell group 3 has a plurality of sample cells 304, and each fuse 303 is suspended with a sample cell 304, and the sample cell 304 falls into the pyrometer after the fuse 303 is electrically fused.
The number of the electrode holes 101 in the embodiment is five, and the five electrode holes 101 are arranged in a regular pentagon shape; correspondingly, the electrode support 203 of the present embodiment is that the bottom ends of the five hollow cylinders 204 are uniformly provided with five electrode center post side hooks 302 in the circumferential direction, and the five electrode center post side hooks 302 are regular pentagons.
The electrode plug 104 and the electrode cap 105 of the embodiment are both cylinders, the diameter of the electrode cap 105 is larger than that of the electrode plug 104, and the electrode cap 105 is used for clamping a furnace mouth of a high-temperature furnace; the electrode hole 101 and the central electrode hole 102 are through holes penetrating the electrode plug body 1, and the aperture of each electrode hole 101 is equal and smaller than the aperture of the central electrode hole 102.
The electrode plug body 1 of the embodiment is made of nickel-based alloy material, the diameter of the electrode cap 105 is 30-80 mm, and the height is 10-30 mm; the diameter of the electrode plug 104 is 20-50 mm, and the height is 20-60 mm. A groove is formed in the outer surface of the upper part of the electrode plug 104, a sealing ring 103 is arranged in the groove, the sealing ring 103 is an O-shaped ring, the material is silicon rubber, and the wire diameter is 1-5 mm; the outer diameter of the sealing ring 103 is larger than the diameter of the electrode plug 104. The aperture of the central electrode hole 102 is 2-10 mm, five identical electrode holes 101 are arranged around the central electrode hole, and the aperture of the electrode holes 101 is 1-5 mm.
The electrode rod group 2 of this embodiment is made of tungsten metal, and the electrode rod group 2 is divided into five electrode struts 203 and one electrode central strut 202 with the same size, and the contact portion between the electrode central strut 202 and the electrode plug body 1 and the contact portion between the electrode struts 203 and the electrode plug body 1 are wrapped and bonded by an insulating ceramic layer. The electrode center pillar 202 of this embodiment is a cylindrical structure made of tungsten, the electrode center pillar 202 is a hollow cylinder with a closed top, and the outer diameter of the hollow cylinder 204 is larger than the outer diameter of other parts of the electrode center pillar 202. The electrode support 203 is a solid columnar body made of tungsten metal. The diameter of the electrode support 203 of the embodiment is 1-5 mm, and the length is 150-400 mm; the tip of the electrode pillar 203 is an electrode tab 201 formed by turning, the length of the electrode tab 201 is 2-4 mm, the width is 1-3 mm, and the height is 100-500 mm. The diameter of the electrode center column is 2-15 mm, and the length is 160-410 mm.
The length of the electrode support 203 is smaller than that of the electrode center post 202, and when the fusing electrode device is vertically installed, hooks 301 in the electrode support are arranged at equal height and higher than hooks 302 on the electrode center post side; five sample cells 304 suspended on the fuse wire 303 are suspended in a regular pentagon arrangement, the center of gravity of the five sample cells is close to the center of the five sample cells, and each sample cell 304 is positioned at the center of a high-temperature area of a hearth of the high-temperature furnace, so that the heating degree of each sample cell 304 is kept consistent.
The electrode pillar inner hook 301 of the embodiment is of five hook structures which are made by turning and have the same size and the same shape, the width of the hook is 0.2-0.8 mm, and the length of the hook is 2-5 mm; the whole length of the electrode pillar inner hook 301 is 2-4 mm, the width is 1-3 mm, and the height is 5-400 mm.
The electrode center post side hook 302 of the embodiment is of five hook structures which are made by cutting and turning the edge side of the bottom of the hollow cylinder 204 and have the same size and the same shape, the width of the electrode center post side hook 302 is 0.2-0.8 mm, and the length of the hook is 2-5 mm; the overall length of the electrode center post side hook 302 is 2 to 4mm, the width is 1 to 3mm, and the height is 5 to 20m.
The material of the fuse wire 303 in this embodiment is made of tungsten wire with purity of 99.9%, the wire diameter of the fuse wire 303 is 0.1-0.5 mm, the length is 50-150 mm, the two ends of the fuse wire 304 are circular rings formed by bending the material, and the diameter of each circular ring is 2-8 m. The circular ring at one end of the fuse link 304 is suspended from the electrode pillar inner hook 301, and the other end is suspended from the corresponding electrode center pillar side hook 302.
The sample cell 304 in this embodiment is a hollow bottle made of nickel-based alloy material, and a suspension hole for suspending the fuse 303 is provided at the top. The inner diameter of the sample cell 304 in this embodiment is 10-15 mm, the outer diameter is 15-20 mm, the height is 40-60 mm, the center of the sample cell 304 is the center of the sample cell group 3 by taking the center of the fusing electrode device, the Cheng Zheng pentagons are sequentially arranged, and the transverse interval between the sample cells 304 is 1-5 mm. Each fusible link 303, the electrode joint 201 and the electrode center column 202 which are connected form a series direct current circuit, the fusing of the fusible links 303 is controlled, so that the sample cells 304 hung on the fusible links 303 are controlled to fall into a high-temperature calorimeter, the fusing sequence of the fusible links 303 is set, and the sample cells 304 hung on each fusible link 303 are controlled to fall down in sequence according to the fusing sequence.
The using method of the fusing electrode device comprises the following steps:
the drop-in calorimeter heats the sample cell 304 in the hearth at high temperature through a high temperature furnace, when the set temperature is reached, the fusing electrode is introduced with 48V direct current, so that the fuse wire 303 is fused in sequence, the sample cell 304 is enabled to drop into the calorimeter from top to bottom in sequence due to the influence of gravity, and then the calorimeter is used for data acquisition and high-temperature specific heat measurement, so that the fusing electrode device is one of the indispensable important constituent devices in the design of the drop-in calorimeter. The method specifically comprises the following steps:
step one, washing the inside and outside of each sample cell 304 three times by using absolute ethyl alcohol, and washing the sample cells three times by using deionized water;
step two, drying and baking each sample cell 304, cooling to room temperature, weighing for multiple times (three times in the embodiment), and taking an average value;
step three, filling each sample cell 304 with a sample, weighing for a plurality of times (three times in the embodiment), and taking an average value;
suspending the fusing electrode device on a lifting support frame of a furnace mouth of the high-temperature furnace, wherein the fusing electrode device is vertical to a horizontal plane, and the vertical distance between the hooks 301 in the electrode support column and the hooks 302 on the side of the electrode center column and the upper surface of the furnace body of the high-temperature furnace is larger than a set distance (100 mm in the embodiment);
step five, respectively penetrating through the fusible links 303 in hanging holes at the top end of each sample cell 304, respectively hanging two ends of each fusible link 303 on a corresponding group of electrode pillar inner hooks 301 and electrode center pillar side hooks 302, hanging the sample cells 304 in a vertical state due to traction of the two ends of the fusible links 303, and adjusting the positions of the sample cells 304 to enable the five sample cells 304 to be in a regular pentagon arrangement;
step six, the fusing electrode device hung with the sample pool 304 is vertically dropped until the electrode plug 104 plugs the furnace mouth of the high-temperature furnace, and is sealed by the sealing ring 103, at the moment, the electrode cap 105 and the above parts are exposed out of the high-temperature furnace, and each sample pool 304 stays in a hot end temperature zone in the hearth of the high-temperature furnace;
step seven, the electrode joint 201 at the top end of each electrode pillar 203 is respectively clamped with a negative electrode connected with a direct current power supply, the positive electrode is clamped at the top end of the electrode center pillar 202, the electrode center pillar 202 connected with the positive electrode and the electrode pillar 203 connected with each negative electrode form a loop, and the positive electrode and the negative electrode can be mutually exchanged;
step eight, fixing the fusing electrode device and the lead of the connected electrode joint, and connecting a 48V direct current power supply and a switching relay at the other end of the electrode;
step nine, a high-temperature furnace is opened to start testing, when the temperature reaches a set value, a direct-current power switch is controlled to be closed, each fuse wire 303 is fused in sequence, and each sample pool 304 falls down in sequence according to the switch control;
step ten, after sample falling is finished, closing the high-temperature furnace, taking out the electrode clamp after the temperature in the furnace is reduced to be within a set temperature (200 ℃ in the embodiment), and lifting the fusing electrode device;
step eleven, after cooling the room temperature, cleaning the residual wires remained on the hooks 301 and 302 in the electrode support column and waiting for the next continuous use.
The invention can meet the requirements of the falling type high temperature calorimeter such as good temperature, accuracy and repeatability, can realize the high-efficiency experiment of one-time temperature rise and multiple measurement of the furnace body, avoids a great amount of time consumed in the repeated temperature reduction and temperature rise processes of the furnace body, and still has perfect functionality at a high temperature of 1500K.

Claims (10)

1. A fusing electrode device for falling into formula high temperature calorimeter, its characterized in that: the electrode plug comprises an electrode plug body (1), an electrode rod group (2) and a sample cell group (3), wherein an electrode cap (105) is arranged at the upper part of the electrode plug body (1), an electrode plug (104) is arranged at the lower part of the electrode plug body, a central electrode hole (102) is formed in the center of the electrode plug body (1) along the axial direction, a plurality of electrode holes (101) are uniformly formed in the periphery of the central electrode hole (102) along the circumferential direction, and a sealing ring (103) is arranged on the electrode plug (104); the electrode rod group (2) comprises electrode center columns (202) and electrode support columns (203) which are the same as the electrode holes (101) in number and correspond to each other one by one, the electrode center columns (202) are arranged in the center electrode holes (102) in a penetrating mode, the top ends of the electrode center columns (202) are located outside the electrode plug body (1), the bottom ends of the electrode center columns (202) are hollow cylinders (204), and a plurality of electrode center column side hooks (302) are uniformly arranged at the bottoms of the hollow cylinders (204) along the circumferential direction; each electrode pillar (203) is respectively penetrated in the corresponding electrode hole (102), the top end of each electrode pillar (203) is an electrode joint (201) positioned outside the electrode plug body (1), the bottom end of each electrode pillar (203) is provided with electrode pillar inner hooks (301), the number of the electrode center pillar side hooks (302) is the same as that of the electrode pillar inner hooks (301) and corresponds to that of the electrode pillar inner hooks (301) one by one, and each electrode pillar inner hook (301) is connected with the corresponding electrode center pillar side hooks (302) through a fuse wire (303); the sample cell group (3) is provided with a plurality of sample cells (304), each fuse wire (303) is suspended with the sample cell (304), and the sample cell (304) falls into the high-temperature calorimeter after the fuse wire (303) is electrified and fused.
2. The fusing electrode assembly for a drop-in pyrometer of claim 1, wherein: the electrode plug (104) and the electrode cap (105) are both cylinders, the diameter of the electrode cap (105) is larger than that of the electrode plug (104), and the electrode hole (101) and the central electrode hole (102) are through holes penetrating through the electrode plug body (1).
3. The fusing electrode assembly for a drop-in pyrometer of claim 1, wherein: the aperture of each electrode hole (101) is equal and smaller than the aperture of the central electrode hole (102).
4. The fusing electrode assembly for a drop-in pyrometer of claim 1, wherein: the electrode plug (104) is provided with a groove, and the sealing ring (103) is accommodated in the groove; the sealing ring (103) is an O-shaped ring, and the outer diameter of the sealing ring (103) is larger than the diameter of the electrode plug (104).
5. The fusing electrode assembly for a drop-in pyrometer of claim 1, wherein: the contact part of the electrode center column (202) and the electrode plug body (1) and the contact part of the electrode support column (203) and the electrode plug body (1) are wrapped and bonded by an insulating ceramic layer.
6. The fusing electrode assembly for a drop-in pyrometer of claim 1, wherein: the electrode center column (202) is a hollow cylinder with a closed top end, and the outer diameter of the hollow cylinder (204) is larger than the outer diameter of other parts of the electrode center column (202).
7. The fusing electrode assembly for a drop-in pyrometer of claim 1, wherein: the length of the electrode support column (203) is smaller than that of the electrode center column (202), when the fusing electrode device is vertically installed, hooks (301) in the electrode support columns are arranged at equal height and higher than electrode center column side hooks (302), the sample cells (304) are hung on the fuse wire (303) to be close to the center, and each sample cell (304) is located at the center of a high-temperature area of a hearth of the high-temperature furnace.
8. The fusing electrode assembly for a drop-in pyrometer of claim 1, wherein: both ends of the fuse wire (303) are annular, the annular ring at one end is hung on the electrode pillar inner hook (301), and the other end is hung on the corresponding electrode center pillar side hook (302).
9. The fusing electrode assembly for a drop-in pyrometer of claim 1, wherein: each fusible link (303), the electrode joint (201) and the electrode center column (202) which are connected form a series direct current circuit, the fusing of the fusible links (303) is controlled, so that a sample cell (304) hung on the fusible links (303) is controlled to fall into a high-temperature calorimeter, the fusing sequence of a plurality of fusible links (303) is set, and the sample cell (304) hung on each fusible link (303) is controlled to sequentially fall down according to the fusing sequence.
10. A method of using the fused electrode assembly for a drop-in pyrometer of any of claims 1 to 9, wherein: comprises the following steps
Step one, cleaning each sample cell (304);
step two, drying and baking each sample cell (304), cooling to room temperature, weighing for multiple times, and taking an average value;
step three, filling a sample into each sample cell (304), weighing again for multiple times, and taking an average value;
suspending the fusing electrode device on a lifting support frame of a furnace mouth of the high-temperature furnace, wherein the fusing electrode device is vertical to a horizontal plane, and the vertical distance between an electrode pillar inner hook (301) and an electrode center pillar side hook (302) and the upper surface of the furnace body of the high-temperature furnace is larger than a set distance;
step five, respectively penetrating through the fusible links (303) at hanging holes at the top end of each sample cell (304), and respectively hanging two ends of each fusible link (303) on hooks (301) in a corresponding group of electrode support posts and hooks (302) at the side of an electrode center post, wherein the sample cells (304) are hung in a vertical state due to traction at the two ends of the fusible links (303);
step six, the fusing electrode device hung with the sample cells (304) is vertically dropped until the electrode plugs (104) plug the furnace mouth of the high-temperature furnace, the sealing rings (103) are used for sealing, at the moment, the electrode caps (105) and the parts above are exposed out of the high-temperature furnace, and each sample cell (304) stays in a hot end temperature zone in the hearth of the high-temperature furnace;
step seven, respectively clamping negative electrodes connected with a direct current power supply on electrode joints (201) at the top ends of the electrode support posts (203), wherein positive electrodes are clamped at the top ends of the electrode center posts (202), the electrode center posts (202) connected with the positive electrodes and the electrode support posts (203) connected with the negative electrodes form a loop, and the positive electrodes and the negative electrodes can be mutually exchanged;
step eight, fixing the fusing electrode device and the lead of the connected electrode joint, and connecting a 48V direct current power supply and a switching relay at the other end of the electrode;
step nine, a high-temperature furnace is opened to start testing, when the temperature reaches a set value, a direct-current power switch is controlled to be closed, each fuse wire (303) is fused in sequence, and each sample cell (304) falls down in sequence according to the control of the switch;
step ten, after sample falling is finished, closing the high-temperature furnace, taking out the electrode clamp after the temperature in the furnace is reduced to be within a set temperature, and lifting the fusing electrode device;
and step eleven, cleaning residual wires left on the hooks (301) in the electrode support column and the hooks (302) on the electrode center column side after cooling the electrode support column to room temperature, and waiting for the next continuous use.
CN202210980166.9A 2022-08-16 2022-08-16 Fusing electrode device for falling-type high-temperature calorimeter and application method thereof Pending CN117630094A (en)

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