阅读说明：本技术 一种嵌套式平衡坩埚及控制方法 (Nested balance crucible and control method ) 是由 彭学诚 郭汉杰 郭靖 王子涵 段生朝 苏耀 张明春 张礼涛 卢秀艳 于 2021-07-01 设计创作，主要内容包括：本发明涉及嵌套式平衡坩埚及控制方法,包括外置坩埚、内置坩埚和调节装置,其中,所述内置坩埚和外置坩埚为嵌套式设置,所述内置坩埚嵌套于所述外置坩埚的内部；所述外置坩埚包括外置坩埚盖和外置坩埚底座,所述外置坩埚盖和外置坩埚底座通过连接件进行连接；所述外置坩埚盖上设置有孔槽,所述孔槽用于放置调节装置；所述内置坩埚用于高温还原反应；所述外置坩埚用于外界隔绝空气进入所述嵌套式平衡坩埚；所述调节装置用于控制调节所述嵌套式平衡坩埚的气体进出。本发明的嵌套式平衡坩埚不但可与外界气体隔绝,而且还能与标准大气压保持一致,并在反应过程中保持还原性条件。(The invention relates to a nested balance crucible and a control method, wherein the nested balance crucible comprises an external crucible, an internal crucible and an adjusting device, wherein the internal crucible and the external crucible are arranged in a nested manner, and the internal crucible is nested in the external crucible; the external crucible comprises an external crucible cover and an external crucible base, and the external crucible cover and the external crucible base are connected through a connecting piece; the external crucible cover is provided with a hole groove, and the hole groove is used for placing an adjusting device; the built-in crucible is used for high-temperature reduction reaction; the external crucible is used for isolating air from the outside and entering the nested balance crucible; the adjusting device is used for controlling and adjusting the gas inlet and outlet of the nested balance crucible. The nested balance crucible can not only be isolated from the outside air, but also keep consistent with the standard atmospheric pressure, and keep the reducing condition in the reaction process.)

1. The nested balance crucible is characterized by comprising an external crucible, an internal crucible and an adjusting device, wherein the internal crucible and the external crucible are nested, and the internal crucible is nested inside the external crucible;

the external crucible comprises an external crucible cover and an external crucible base, and the external crucible cover and the external crucible base are connected through a connecting piece;

the external crucible cover is provided with a hole groove, and the hole groove is used for placing the adjusting device;

the adjusting device is used for controlling and adjusting the gas inlet and outlet of the nested balance crucible.

2. The nested balance crucible of claim 1, wherein the inner crucible and the outer crucible are made of different materials, and the outer crucible is made of graphite; the material of the built-in crucible is alumina.

3. The nested balance crucible of claim 1, wherein the adjusting means is made of high purity alumina.

4. The nested balance crucible of claim 1, wherein the outer crucible cover and the outer crucible base are connected by threads.

5. The nested balance crucible of claim 4, wherein the pitch of the threads is 0.05mm to 0.1 mm.

6. The nested balance crucible of claim 1, wherein the inner wall of the outer crucible is in close proximity to the outer wall of the inner crucible.

7. The nested balance crucible of claim 1, wherein the inner crucible comprises an inner crucible cover and an inner crucible base.

8. The nested balance crucible of claim 7, wherein the size of the orifice slot and the size of the adjustment device are the same.

9. The nested balance crucible of claim 7, wherein a gap is provided between the inner crucible cover and the inner crucible base.

10. A method of controlling a nested balance crucible according to any one of claims 1 to 9, comprising the steps of:

s1, adding a certain content of carbon into a reaction material, and fully stirring to form a sample;

s2, adding the sample into the built-in crucible, placing the built-in crucible into an external crucible, and placing the adjusting device at the hole groove;

s3, the nested balance crucible is integrally placed in a muffle furnace to be electrically heated, the sample is heated, gas is released to enable the gas pressure in the built-in crucible to be increased, the gas with the increased pressure enters the external crucible from the built-in crucible, and when the gas pressure in the external crucible is increased to jack up the adjusting device, the gas in the external crucible jacks up the adjusting device from the hole groove;

and S4, when the gas in the external crucible is released, the pressure in the external crucible is reduced, and the adjusting device falls back to the hole groove.

Technical Field

The invention relates to the technical field of crucible equipment, in particular to a nested balance crucible and a control method.

Background

The crucible has the advantages of high temperature resistance, high thermal stability, strong heat conductivity and the like in the high-temperature reduction experiment process. However, in the practical process, due to the characteristic of poor air tightness of the crucible, when the oxygen content in the reaction crucible is too high, carbon in the carbon reaction used as the reducing agent will firstly complete the oxidation process to form carbon dioxide, which causes the phenomenon of reduction failure. In addition, a fully-enclosed crucible is often adopted in a common enclosed crucible, and during a high-temperature reaction process, the change of gas-phase components inside the crucible can cause the change of the reaction balance inside the crucible, thereby influencing the high-temperature reduction reaction. In order to solve the above problems, the high temperature reduction reaction process is usually protected by inert gas at a high flow rate to realize the carbon reduction process and the normal pressure equilibrium reaction, but the high precision gas supply device often limits the high temperature reduction reaction and causes a dynamic non-equilibrium state in the high temperature reduction process. In order to realize the high-temperature static reduction process of carbon reduction and reduce the operation difficulty of a high-temperature reduction experiment, the reaction device is designed, absolute isolated air can be provided, and the static high-temperature reduction reaction is realized so as to solve the related problems generated in the practical application process of the crucible.

Disclosure of Invention

The invention aims to solve the defects in the prior art, and provides a nested balance crucible and a control method, which are used for solving the problems in the prior art.

The above technical object of the present invention will be achieved by the following technical solutions.

A nested balance crucible comprises an external crucible, an internal crucible and an adjusting device, wherein the internal crucible and the external crucible are arranged in a nested manner, and the internal crucible is nested in the external crucible;

the external crucible comprises an external crucible cover and an external crucible base, and the external crucible cover and the external crucible base are connected through a connecting piece;

the external crucible cover is provided with a hole groove, and the hole groove is used for placing the adjusting device;

the adjusting device is used for controlling the gas inlet and outlet of the nested balance crucible.

In the aspect and any possible implementation manner described above, there is further provided an implementation manner, in which the material of the inner crucible is different from that of the outer crucible, and the material of the outer crucible is graphite; the material of the built-in crucible is alumina.

The above aspect and any possible implementation manner further provide an implementation manner, wherein the material of the adjusting device is high-purity alumina.

The above aspects and any possible implementations further provide an implementation in which the external crucible cover and the external crucible base are connected by a screw thread.

There is further provided in accordance with the above-described aspect and any one of the possible implementations, an implementation in which the pitch of the threads is 0.05mm to 0.1 mm.

The above aspects and any possible implementations further provide an implementation in which the inner wall of the outer crucible is in close contact with the outer wall of the inner crucible.

The above aspects and any possible implementations further provide an implementation in which the inner crucible includes an inner crucible cover and an inner crucible base.

The above aspect and any possible implementation further provide an implementation in which the size of the hole slot is the same as the size of the adjustment device.

The above aspects and any possible implementations further provide an implementation in which a gap is provided between the inner crucible cover and the inner crucible base.

The above aspects and any possible implementation manners further provide an implementation manner, wherein the hole groove is arranged at the middle position of the external crucible cover, and the internal crucible is used for high-temperature reduction reaction; the external crucible is used for isolating air from the outside and entering the nested balance crucible.

The invention also provides a control method of the nested balance crucible, which comprises the following steps:

s1, adding a certain amount of carbon into a reaction material, fully stirring to form a sample,

s2, adding the sample into the built-in crucible, placing the built-in crucible into an external crucible, and placing the adjusting device at the hole groove;

s3, the nested balance crucible is integrally placed in a muffle furnace to be electrically heated, the sample is heated, gas is released to enable the gas pressure in the built-in crucible to be increased, the gas with the increased pressure enters the external crucible from the built-in crucible, and when the gas pressure in the external crucible is increased to jack up the adjusting device, the gas in the external crucible jacks up the adjusting device from the hole groove;

and S4, when the gas in the external crucible is released, the pressure in the external crucible is reduced, and the adjusting device falls back to the hole groove.

The invention has the beneficial technical effects

The nested balance crucible provided by the embodiment of the invention comprises an external crucible, an internal crucible and an adjusting device, wherein the internal crucible and the external crucible are nested, and the internal crucible is nested in the external crucible; the external crucible comprises an external crucible cover and an external crucible base, and the external crucible cover and the external crucible base are connected through a connecting piece; the external crucible cover is provided with a hole groove, and the hole groove is used for placing the adjusting device; the built-in crucible is used for high-temperature reduction reaction; the external crucible is used for isolating air from the outside and entering the nested balance crucible; the adjusting device is used for controlling and adjusting the gas inlet and outlet of the nested balance crucible. The nested balance crucible can not only be isolated from the outside air, but also keep consistent with the standard atmospheric pressure, and keep the reducing condition in the reaction process. The nested balance crucible can be applied to the relevant reduction reaction of the reaction with carbon in a common muffle furnace, has simple reaction conditions, and is suitable for the relevant high-temperature reduction process in a laboratory.

Drawings

Embodiments of the invention are described in detail below with reference to the attached drawing figures, wherein:

FIG. 1 is a schematic cross-sectional elevation view of a nested balance crucible in an embodiment of the invention;

FIG. 2 is a schematic cross-sectional front view of an external crucible of a nested balance crucible in an embodiment of the present invention;

FIG. 3 is a schematic front cross-sectional view of an inner crucible of a nested balance crucible in an embodiment of the present invention;

FIG. 4 is a schematic cross-sectional front view of gas control spheres of a nested equilibrium crucible in an embodiment of the invention.

In the figure: 1-a hole groove; 2-clearance; 3-arranging a crucible cover; 4-external crucible cover; 5-thread; 6-arranging a crucible base inside; 7-external crucible base; 8-gas control ball.

Detailed Description

In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description is made with reference to the accompanying drawings and specific examples, but the embodiments of the present invention are not limited thereto.

As shown in FIG. 1, the nested balance crucible comprises an external crucible, an internal crucible and an adjusting device, wherein the adjusting device is a gas control ball 8, the internal crucible and the external crucible are nested, and the internal crucible is nested inside the external crucible; the external crucible comprises an external crucible cover 4 and an external crucible base 7, and the external crucible cover 4 and the external crucible base 7 are connected through a connecting piece; the external crucible cover 4 is provided with a hole groove 1, and the hole groove 1 is used for placing the gas control ball 8; the built-in crucible is used for high-temperature reduction reaction; the external crucible is used for isolating air from the outside and entering the nested balance crucible; the gas control ball 8 is used for controlling the gas inlet and outlet of the nested balance crucible.

The nested balance crucible is used by nesting two crucibles which are made of different materials, namely an inner crucible and an outer crucible, the outer crucible is made of graphite, silicon carbide, silica, refractory clay, asphalt and tar which are used as main components, and the material has the excellent characteristics of heat conductivity coefficient of 151w/(m.k), high temperature resistance, corrosion resistance and high fusion rate; the gas control ball 8 is made of light alumina corundum balls and controls gas to enter and exit, so that the gas pressure inside the nested balance crucible is kept consistent with the standard atmospheric pressure.

Preferably, the external crucible is divided into an upper part and a lower part, and comprises an external crucible cover 4 and an external crucible base 7, wherein the external crucible cover 4 and the external crucible base 7 are connected through a connecting piece, specifically, the external crucible cover 4 and the external crucible base 7 are connected through threads, and the thread pitch of the threads is 0.05mm-0.1 mm.

Preferably, the built-in crucible is made of high-purity alumina, the built-in crucible is used in a high-temperature reduction reaction generation area, the built-in crucible comprises a built-in crucible cover 3 and a built-in crucible base 6, the built-in dry crucible cover 3 is used for preventing reaction from splashing and eroding an external crucible in the high-temperature reaction process, the built-in crucible base 6 is mainly used as a high-temperature reaction area, compared with a traditional integrated crucible, the internal crucible has higher protection performance and can be replaced at any time, a gap 2 is arranged between the built-in crucible cover 3 and the built-in crucible base 6 for carrying out the gas transmission process in the high-temperature reduction reaction process, reducing atmosphere is produced by carbon powder in the built-in crucible, the upper part of the built-in crucible is made of high-purity alumina with the content of 99% Al2O3, the material has high heat conductivity, corrosion resistance and high-quality performance crucible cover 3 with high thermal deformation temperature for protection, so as to prevent a molten sample from splashing in the built-in crucible base 6 due to severe high-temperature reaction, causing loss of the external crucible.

Preferably, the external crucible cover 4 is provided with a hole groove 1, the hole groove 1 is used for placing the gas control ball 8, the hole groove 1 is realized in the form of a gas hole, specifically, the middle position of the external crucible cover 4 is provided with a gas hole, the gas hole is circular and has the size consistent with that of the gas control ball 8, the gas control ball 8 is placed on the gas hole, the gas control ball 8 is made of a light alumina material with 99% Al2O3 content, when the material receives the pressure of the internal gas, the material releases the pressure of the internal gas because the low-density gas control ball 8 is easy to jack up, and the gas control ball 8 does not melt and deform when the temperature of the reaction furnace is lower than 2050 ℃.

The size of the light high-purity alumina gas control ball 8 is consistent with that of the circular air hole at the top of the external crucible cover 4, so that the light high-purity alumina gas control ball and the circular air hole are tightly attached to each other when being connected, and no gas is leaked from the boundary of the joint of the light high-purity alumina gas control ball and the circular air hole. The working principle of the gas control ball 8 is as follows: when the gas pressure inside the built-in crucible is reduced due to the release, the light alumina balls 8 fall back to the gas holes again, and therefore the external gas is prevented from entering the built-in crucible from the gap 2 through the light alumina gas control balls 8. When the high-temperature reduction reaction in the built-in crucible further proceeds, the gas pressure inside the built-in crucible will rise again, and the light alumina gas control ball 8 will be ejected again by the rising gas pressure, so that the reaction gas pressure inside the built-in crucible is released again. The gas in the built-in crucible is heated to expand at high temperature and is released out of the built-in crucible, and meanwhile, the external gas cannot enter the built-in crucible due to the obstruction of the gas control ball 8.

Preferably, a certain gap is left between the outer crucible cover 4 and the inner crucible cover 3 in the present invention, so that the gas flowing out of the inner crucible cover 3 in the inner crucible is discharged to the external atmosphere through the gas hole.

Preferably, the inner wall of the outer crucible and the outer wall of the inner crucible in the present invention are closely attached, the content of air existing between the inner wall of the outer crucible and the inner crucible is small, and the outer crucible is made of a high purity graphite crucible, even if a small amount of air exists, the air will be rapidly consumed by carbon, so that no oxidizing atmosphere exists in the whole apparatus. When the sample in the inner crucible and the carbon generate high-temperature reduction reaction to generate gas, the gas in the inner crucible flows according to the structure shown in figure 1, and the generated gas overflows from the gap 2 between the inner crucible cover 3 and the inner crucible base 6 and enters the outer crucible due to the expansion of the gas caused by heating and the high concentration of the gas. Then, the gas is further gathered and the pressure is increased, so that the gas control ball 8 made of light alumina is jacked up to release the gas in the inner crucible. When the pressure inside is not sufficient to support the gas control ball 8, the gas control ball 8 falls back to the gas hole, thereby blocking the external gas from entering the built-in crucible. Therefore, the pressure of the built-in crucible is kept consistent with the standard atmospheric pressure, and meanwhile, the damage of reducing conditions caused by the fact that external gas enters the built-in crucible is avoided.

In the using process, the built-in crucible is placed into the inner base of the external crucible, and after the built-in crucible is stably placed, the external crucible cover 4 is tightly connected with the external crucible base 7 through the threads by rotating. After the gas control ball 8 is put into the circular hole on the external crucible cover 4, no gap exists between the circular hole and the gas control ball, and at the moment, the nested balance crucible forms a closed space system.

The invention also provides a control method of the nested balance crucible, which comprises the following steps:

step 1, adding a certain amount of carbon into a reaction material, fully stirring to form a sample,

step 2, adding the sample into the built-in crucible, placing the built-in crucible into an external crucible, and placing the adjusting device at the hole groove;

step 3, the nested balance crucible is integrally placed in a muffle furnace to be electrically heated, the sample is heated, gas is released to enable the gas pressure in the built-in crucible to be increased, the gas with the increased pressure enters the external crucible from the built-in crucible, and when the gas pressure in the external crucible is increased to jack up the adjusting device, the gas in the external crucible jacks up the adjusting device from the hole groove;

and 4, when the gas in the external crucible is released, the pressure in the external crucible is reduced, and the adjusting device falls back to the hole groove.

The specific process is as follows:

according to the proportion of reaction materials set by experiments, carbon with a certain content is added as a high-temperature reduction reactant, the prepared reaction materials are fully stirred to form a uniform sample, the sample is added into an internal crucible base 6 and an internal crucible cover 3 is added, an internal crucible is placed in an external crucible base 7 and is connected with the external crucible base 7 and the external crucible cover 4 through threads, a gas control ball 8 is placed at a gas hole to allow air to enter and exit with the air, the whole reaction device is stably placed in a muffle furnace for electric heating, when heat is conducted to the reaction sample through the external crucible and the internal crucible, the reactant is heated at the moment, the reactivity of the sample is increased, when the temperature of the sample reaches the reaction temperature, the high-temperature reduction reaction starts, a gas-phase reduction product is released, the continuously increased gas product and the gas are heated to expand, so that the pressure of the gas in the internal crucible is increased, high-pressure gas overflows from the gap 2 and enters the external crucible, and when the gas pressure in the external crucible is increased to be enough to jack the gas control ball 8, the gas can enable the gas control ball 8 to be ejected out of the gas hole, so that the gas in the external crucible is released; after the gas in the external crucible is released, the pressure in the external crucible is reduced, namely when the pressure in the external crucible is not enough to support the gas control ball 8, the gas control ball 8 falls back to the air hole, so that the external gas is prevented from entering the internal crucible, the pressure of the internal crucible is kept consistent with the standard atmospheric pressure, and meanwhile, the external gas is prevented from entering the internal crucible to cause the damage of the reducing condition.

The nested balance crucible is nested by adopting crucibles of different materials inside and outside, and the gas control ball 8 is arranged at the top end of the external crucible cover 4, so that a sample prepared into a carbon reducing agent with uniform components in a certain proportion is arranged in the internal crucible, the internal crucible is arranged in the external crucible, the gas control ball 8 is used for controlling the inlet and the outlet of reaction gas, the device is stably arranged in a muffle furnace to realize high-temperature reduction reaction, and the pressure in a reaction system in the reaction of the reaction device is kept consistent with the standard atmospheric pressure due to the air tightness difference inside the muffle furnace. The invention can realize balanced type high temperature reduction reaction, not only can ensure that a certain carbon content is proportioned in the built-in crucible, but also can realize that the reaction sample is heated by heat conduction from the external crucible cover 4 and the external crucible base 7 to the internal crucible by utilizing the electric heating of the muffle furnace, thereby realizing the high temperature reduction reaction process in the muffle furnace, and simultaneously, the invention utilizes the mechanism that the gas control ball 8 moves up and down by receiving the strength of the gas pressure in the external crucible, and controls the system pressure and the external atmospheric pressure to keep consistent excellent performance in the reaction process.

While the foregoing description shows and describes several preferred embodiments of the invention, it is to be understood, as noted above, that the invention is not limited to the forms disclosed herein, but is not intended to be exhaustive or to exclude other embodiments and may be used in various other combinations, modifications, and environments and is capable of changes within the scope of the invention as expressed herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.