A SiC / g-C3N4 material anti-combustion composite fired crucible

Abstract

The present invention belongs to the field of materials and other instruments, and particularly relates to a combustion-proof composite firing crucible for SiC / g-C3N4 materials. The firing crucible consists of a storage crucible, a rotating lid, and a sealing plate. The storage crucible includes a crucible bottom, a crucible wall, a loop, a combustion wall, and a composite wall; the bottom of the storage crucible is the crucible bottom, a crucible wall is provided at the upper edge of the crucible bottom, and a loop is provided at the top of the crucible wall; a combustion wall is provided on the crucible bottom inside the crucible wall; a composite wall is provided inside the combustion wall; the height of the composite wall is lower than that of the combustion wall, and its interior is a composite cavity for the composite firing of materials; the space between the combustion wall and the composite wall is a combustion cavity, and a combustion hole is provided at the bottom of the combustion cavity; the space between the crucible wall and the combustion wall is a retention cavity. The rotating lid includes a lid top, a rotating wall, and a lid ring, and the rotating wall is provided outside the combustion wall. The sealing plate includes a plate support and a plate wall; the plate wall is hermetically sleeved outside the crucible wall. The present invention is used for the firing of SiC / g-C3N4 materials, can effectively prevent the combustion of melamine, and improve the yield of composite materials.

Description

Technical Field

[0001] The present invention belongs to the field of devices for photocatalytic materials, and particularly relates to a combustion-proof composite firing crucible made of SiC / g-C3N4 material. Background Art

[0002] SiC / g-C3N4 is a composite material that can be photocatalyzed by visible light, which is synthesized by calcining β-type cubic silicon carbide and melamine at a high temperature of 550 °C in a muffle furnace. At this temperature, although melamine alone will not burn, in this project, adding silicon carbide will cause about half of the melamine to be burned out, and sometimes all of the melamine will be burned out, ultimately resulting in the failure of the material composite. Currently, in response to this phenomenon, calcination is mainly carried out using inert gas protection, that is, using inert gases such as nitrogen, carbon dioxide, and argon to exclude oxygen inside the muffle furnace to prevent the material from being oxidized; and this requires connecting the muffle furnace to a high-pressure gas cylinder. For ordinary laboratories, this will undoubtedly increase the synthesis cost of SiC / g-C3N4 materials, and sometimes the use of high-pressure gas cylinders cannot be carried out due to safety production management; this has led to a very low synthesis rate of the materials. Summary of the Invention

[0003] In view of the technical problem of material combustion during the calcination of the above composite material, the present invention designs a combustion-proof composite firing crucible for SiC / g-C3N4 material, which is characterized in that the firing crucible is composed of a storage crucible 1, a transfer cover 2, and a sealing plate 3; the sealing plate 3 is hermetically sleeved on the lower part of the storage crucible 1, and the transfer cover 2 is inserted and covered on the upper part of the storage crucible 1.

[0004] The storage crucible 1 includes a crucible bottom 1.1, a crucible wall 1.2, a loop 1.3, a combustion wall 1.4, and a composite wall 1.5; the bottom of the storage crucible 1 is the crucible bottom 1.1, and a vertical crucible wall 1.2 is provided at the upper edge of the crucible bottom 1.1, and an inward horizontal loop 1.3 is provided at the top of the crucible wall 1.2; a vertical annular combustion wall 1.4 is provided on the crucible bottom 1.1 inside the crucible wall 1.2; a composite wall 1.5 is provided inside the combustion wall 1.4; the height of the composite wall 1.5 is lower than that of the combustion wall 1.4; the inside of the composite wall 1.5 is a composite cavity for the composite firing of SiC / g-C3N4 material; the inner bottom surface of the composite wall 1.5 is spherical, its outer side wall is vertically designed, and its inner side wall is an inverted cone-shaped cylinder; the space between the combustion wall 1.4 and the composite wall 1.5 is a combustion cavity, the bottom of which is a downwardly concave bottom surface, and a combustion hole 1.6 is provided at the bottom; the space between the crucible wall 1.2 and the combustion wall 1.4 is a retention cavity.

[0005] The transfer and storage cover 2 includes a cover top 2.1, a transfer and storage wall 2.2, and a cover ring 2.3; the upper part of the transfer and storage cover 2 is the cover top 2.1, and a vertical transfer and storage wall 2.2 is provided at the lower edge of the cover top 2.1; a cover ring 2.3 is provided on the upper part of the cover top 2.1; the transfer and storage wall 2.2 is sleeved in the retention cavity outside the combustion wall 1.4.

[0006] The sealing plate 3 includes a plate support 3.1 and a plate wall 3.2; the bottom of the sealing plate 3 is the plate support 3.1, and a vertical plate wall 3.2 is provided at the upper edge of the plate support 3.1, and the plate wall 3.2 can be hermetically sleeved outside the crucible wall 1.2.

[0007] The volume of the retention cavity is twice the sum of the composite cavity and the combustion cavity. The transfer and storage wall 2.2 is inserted to the bottom of the retention cavity, there is a gap between the combustion wall 1.4 and the transfer and storage wall 2.2, and there is a gap between the top of the combustion wall 1.4 and the cover top 2.1. The SiC is β-type cubic silicon carbide with a particle size of 1 - 50 microns. The inner wall of the composite wall 1.5 is smooth. Charcoal is placed in the combustion hole 1.6, and after the charcoal burns, it is used to consume the oxygen inside the combustion cavity and the composite cavity.

[0008] The beneficial technical effects of the present invention are:

[0009] Now, the various inventive points of this application are further elaborated in combination with the technical features and technical effects: (1) The present invention is designed with a composite chamber and a combustion chamber. Charcoal is placed in the combustion hole at the bottom of the combustion chamber. After the charcoal burns, it will consume the oxygen inside the composite chamber and the combustion chamber, which can effectively prevent the combustion of melamine; charcoal can burn at about 300°C, and the space inside the composite chamber and the combustion chamber is small, and the oxygen will be consumed in a short time to form carbon dioxide; and under the barrier of the composite wall, melamine will not be ignited; the height of the composite wall is lower than the combustion wall, which can effectively ensure the consumption of oxygen inside the composite chamber and the combustion chamber. Since the same amount of oxygen will produce the same amount of carbon dioxide, and there is no substance that reacts with carbon dioxide in the firing crucible, it will not cause the internal pressure of the firing crucible to rise or fall rapidly, so the firing crucible is safe and reliable. The overall design of the present invention avoids the use of high-pressure gas cylinders, thereby reducing the firing cost of materials. (2) Place charcoal in the combustion chamber. After the muffle furnace cools down, open the lid and remove the sealing plate. Then, use an alcohol cotton swab to clean the charcoal and a small amount of charcoal ash on the combustion hole and the sealing plate. Scrape the composite material inside the composite chamber, cover the lid and turn the transfer cover and the storage crucible upside down. Then, the composite material can be smoothly transferred to the transfer cover. This is because the design of the combustion port can effectively balance the pressure inside the composite chamber and the combustion chamber, and can effectively prevent the powder from diffusing in the air inside the composite chamber and the combustion chamber, so as to prevent the powder dispersed inside from diffusing into the external air when the lid and the storage crucible are separated. (3) The volume of the storage chamber is about twice the sum of the composite chamber and the combustion chamber. The combustion temperature of charcoal is about 300℃, and the composite temperature of SiC / g-C3N4 composite material is 550℃. Therefore, according to the ideal gas state equation, the expansion of the air volume in the composite chamber and the combustion chamber caused by the temperature rise can be completely accommodated by the storage chamber. Therefore, in the previous stage of cooling from 550℃ to room temperature, the gas with reduced oxygen content in the storage chamber will flow back into the composite chamber and the combustion chamber, which can effectively prevent g-C3N4 from being burned. (4) The transfer wall penetrates into the bottom of the storage chamber, and the gas flowing out from the gap between the combustion wall and the transfer wall will exclude the gas in the storage chamber. Therefore, the gas with relatively high excess oxygen content will flow into the muffle furnace from the gap between the cover top and the return ring. BRIEF DESCRIPTION OF THE DRAWINGS

[0010] Figure 1 A combined perspective view of a SiC / g-C3N4 material combustion-proof composite sintering crucible;

[0011] Figure 2 It is a schematic diagram of the explosion of a SiC / g-C3N4 material anti-combustion composite sintered crucible;

[0012] Figure 3 It is an assembly cross-sectional view of a SiC / g-C3N4 material combustion-proof composite sintering crucible;

[0013] Figure 4 It is a schematic diagram of the inclined top view of the storage crucible;

[0014] Figure 5 It is a sectional view of the inclined top view of the storage crucible;

[0015] Figure 6 It is a schematic diagram of the inclined top view of the transfer cover;

[0016] Figure 7 It is a schematic diagram of the inclined top view of the sealing plate.

[0017] In the figure, 1 - storage crucible, 2 - transfer cover, 3 - sealing plate; 1.1 - crucible bottom, 1.2 - crucible wall, 1.3 - loop, 1.4 - combustion wall, 1.5 - composite wall, 1.6 - combustion hole; 2.1 - cover top, 2.2 - transfer wall, 2.3 - cover ring; 3.1 - plate support, 3.2 - plate wall. Specific embodiments

[0018] The following further describes the specific structure of the present invention in conjunction with the attached Figure 1-7 drawings and embodiments:

[0019] A SiC / g-C3N4 material anti-combustion composite firing crucible, characterized in that the firing crucible is composed of a storage crucible 1, a transfer cover 2, and a sealing plate 3; the sealing plate 3 is hermetically sleeved on the lower part of the storage crucible 1, and the transfer cover 2 is inserted and covered on the upper part of the storage crucible 1.

[0020] The storage crucible 1 includes a crucible bottom 1.1, a crucible wall 1.2, a loop 1.3, a combustion wall 1.4, and a composite wall 1.5; the bottom of the storage crucible 1 is the crucible bottom 1.1, a vertical crucible wall 1.2 is provided at the upper edge of the crucible bottom 1.1, and an inward horizontal loop 1.3 is provided at the top of the crucible wall 1.2; a vertical annular combustion wall 1.4 is provided on the crucible bottom 1.1 inside the crucible wall 1.2; a composite wall 1.5 is provided inside the combustion wall 1.4; the height of the composite wall 1.5 is lower than that of the combustion wall 1.4; the inside of the composite wall 1.5 is a composite cavity for the composite firing of SiC / g-C3N4 materials; the inner bottom of the composite wall 1.5 is spherical, its outer wall is vertically designed, and its inner wall is an inverted conical cylinder; the space between the combustion wall 1.4 and the composite wall 1.5 is a combustion cavity, the bottom of which is a downwardly concave bottom surface, and a combustion hole 1.6 is provided at the bottom; the space between the crucible wall 1.2 and the combustion wall 1.4 is a retention cavity.

[0021] The transfer cover 2 includes a cover top 2.1, a transfer wall 2.2, and a cover ring 2.3; the upper part of the transfer cover 2 is the cover top 2.1, a vertical transfer wall 2.2 is provided at the lower edge of the cover top 2.1; a cover ring 2.3 is provided on the upper part of the cover top 2.1; the transfer wall 2.2 is sleeved in the retention cavity outside the combustion wall 1.4.

[0022] The sealing plate 3 includes a tray 3.1 and a tray wall 3.2; the bottom of the sealing plate 3 is the tray 3.1, and a vertical tray wall 3.2 is provided at the upper edge of the tray 3.1, and the tray wall 3.2 can be hermetically sleeved outside the crucible wall 1.2.

[0023] The volume of the retention cavity is twice the sum of the composite cavity and the combustion cavity. The rotating holding wall 2.2 is inserted into the bottom of the retention cavity, there is a gap between the combustion wall 1.4 and the rotating holding wall 2.2, and there is a gap between the top of the combustion wall 1.4 and the lid top 2.1. The SiC is β-type cubic silicon carbide with a particle size of 1 - 50 microns. The inner wall of the composite wall 1.5 is smooth. Charcoal is placed in the combustion hole 1.6, and after the charcoal burns, it is used to consume the oxygen inside the combustion cavity and the composite cavity.

[0024] Specific usage method: Sleeve the sealing plate 3 on the bottom of the storage and combustion crucible 1, take a small amount of charcoal and place it into the combustion hole 1.6, and place the mixed melamine and silicon carbide into the composite cavity; cover the rotating holding lid 2 and place it into a muffle furnace, and heat it to 550 °C for calcination according to a certain procedure; then cool it down to the temperature at which the muffle furnace can be opened according to the procedure. Uncover the rotating holding lid 2, remove the sealing plate, and use a cotton swab dipped in anhydrous ethanol to remove the charcoal and carbon ash on the combustion hole and the bottom plate. The alcohol will evaporate quickly without polluting the composite material; then scrape the composite material in the combustion cavity from the inner wall and the bottom of the composite cavity. Cover the rotating holding lid 2 on the storage and combustion crucible, then invert the rotating holding lid 2 and the storage and combustion crucible 1, transfer the composite material into the rotating holding lid 2, and then transfer the composite material into a centrifuge tube for storage.

[0025] As mentioned above, it is only a preferred specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. For example, the connection method can adopt a method other than the connecting column, etc. Any change or replacement that can be easily thought of by any person skilled in the technical field within the technical scope disclosed by the present invention should be covered within the protection scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.

Claims

1. A SiC / g-C3N4 material anti-combustion composite fired crucible, characterized in that, The firing crucible is composed of a storage crucible (1), a transfer cover (2), and a sealing plate (3); the sealing plate (3) is hermetically sleeved on the lower part of the storage crucible (1), and the transfer cover (2) is inserted and covered on the upper part of the storage crucible (1); The storage crucible (1) includes a crucible bottom (1.1), a crucible wall (1.2), a loop (1.3), a combustion wall (1.4), and a composite wall (1.5); the bottom of the storage crucible (1) is the crucible bottom (1.1), and a vertical crucible wall (1.2) is provided at the upper edge of the crucible bottom (1.1), and an inward horizontal loop (1.3) is provided at the top of the crucible wall (1.2); a vertical annular combustion wall (1.4) is provided on the crucible bottom (1.1) inside the crucible wall (1.2); a composite wall (1.5) is provided inside the combustion wall (1.4); the height of the composite wall (1.5) is lower than that of the combustion wall (1.4); the inside of the composite wall (1.5) is a composite cavity for the composite firing of SiC / g-C3N4 materials. The inner bottom of the composite wall (1.5) is spherical, its outer wall is vertical, and its inner wall is an inverted conical cylinder; the space between the combustion wall (1.4) and the composite wall (1.5) is a combustion cavity, the bottom of which is a downward concave bottom surface, and a combustion hole (1.6) is provided at the bottom; the space between the crucible wall (1.2) and the combustion wall (1.4) is a retention cavity; The transfer cover (2) includes a cover top (2.1), a transfer wall (2.2), and a cover ring (2.3); the upper part of the transfer cover (2) is the cover top (2.1), and a vertical transfer wall (2.2) is provided at the lower edge of the cover top (2.1); a cover ring (2.3) is provided on the upper part of the cover top (2.1); the transfer wall (2.2) is sleeved in the retention cavity outside the combustion wall (1.4); The sealing plate (3) includes a plate support (3.1) and a plate wall (3.2); the bottom of the sealing plate (3) is the plate support (3.1), and a vertical plate wall (3.2) is provided at the upper edge of the plate support (3.1), and the plate wall (3.2) can be hermetically sleeved on the outside of the crucible wall (1.2).

2. A SiC / g-C3N4 material anti-combustion composite fired crucible according to claim 1, characterized in that, The volume of the retention cavity is twice the sum of the volumes of the composite cavity and the combustion cavity.

3. A SiC / g-C3N4 material anti-combustion composite fired crucible according to claim 1, characterized in that, The transfer wall (2.2) extends to the bottom of the retention cavity, there is a gap between the combustion wall (1.4) and the transfer wall (2.2), and there is a gap between the top of the combustion wall (1.4) and the cover top (2.1).

4. A SiC / g-C3N4 material anti-combustion composite fired crucible according to claim 1, characterized in that, The SiC is β-type cubic silicon carbide with a particle size of 1-50 microns.

5. A SiC / g-C3N4 material anti-combustion composite fired crucible according to claim 1, characterized in that, The inner wall of the composite wall (1.5) is smooth.

6. The anti-combustion composite fired crucible made of SiC / g-C3N4 material according to claim 1, characterized in that, Charcoal is placed in the combustion hole (1.6), and after the charcoal burns, it is used to consume the oxygen inside the combustion cavity and the composite cavity.

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