CN211964205U - Device for preparing carbon tetrafluoride gas - Google Patents
Device for preparing carbon tetrafluoride gas Download PDFInfo
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- CN211964205U CN211964205U CN202020227838.5U CN202020227838U CN211964205U CN 211964205 U CN211964205 U CN 211964205U CN 202020227838 U CN202020227838 U CN 202020227838U CN 211964205 U CN211964205 U CN 211964205U
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Abstract
The utility model discloses a device of preparation carbon tetrafluoride gas, the novel nipple rectifier comprises a cylindrical shel, the barrel top is equipped with the carbon granule charge door, the lower part outside is equipped with the cooling water jacket in the barrel, barrel top side is equipped with the export of carbon tetrafluoride crude gas, the barrel lower extreme is violently managed the middle part with the barrel and is connected, the barrel is violently managed both ends upside and is connected fluorine import pipe respectively, the barrel is violently managed the bottom of one end and is equipped with and drags for the sediment mouth, the barrel is violently managed inside and is equipped with the sieve, the barrel is violently managed the outside and is equipped with the electric heating radiant panel, electric heating. The device admits air from the lower part of both ends through the fluorine import pipe, and it is big to let through fluorine gas volume, and reaction zone space is big, and gas-solid area of contact is big, and the reaction is more abundant, and it is more convenient to remove the gred slag, filters the fine sediment through the bottom sieve, and the product gas of top side goes out, prevents that the carbon sediment after fluorine gas and carbon granule react from blockking up, and fluorine gas conversion rate is higher than 98%, and the technology operation is stable.
Description
Technical Field
The utility model relates to a fluoride preparation technical field particularly, relates to a preparation carbon tetrafluoride gaseous device.
Background
Carbon tetrafluoride (CF)4) The plasma etching gas with the largest consumption in the microelectronic industry is widely used for etching thin film materials such as silicon, silicon dioxide, silicon nitride, phosphosilicate glass, tungsten and the like, and also has a large amount of applications in the aspects of cleaning the surfaces of electronic devices, producing solar batteries, laser technology, low-temperature refrigeration, gas insulation, leakage detection agents, controlling the attitudes of space rockets, detergents in printed circuit production, lubricants, brake fluids and the like. CF due to its extremely strong chemical stability4It can also be used in metal smelting and plastics industries.
The characteristics and development trend of electronic gas used by the current ultra-large scale integrated circuit are ultra-pure, ultra-clean, various and multi-scale, and in order to promote the development of the microelectronic industry of China, the China pays more and more attention to the development of the production technology of special electronic gas. At present, CF4Has a wide potential for development because of its long-term market for etching gases at a relatively low price. Carbon tetrafluoride is produced in a wide variety of ways, but essentially only elemental fluorine is reacted with solid carbon particles for industrial production. The prior art has various reaction devices for preparing carbon tetrafluoride, and most manufacturers adopt a typical vertical reaction device at present.
Chinese patent with granted publication No. CN 102863312B (application No. 201210355457.5) discloses a carbon tetrafluoride production apparatus, as shown in fig. 1, in the apparatus, an inlet is provided on the upper side of a first-stage reactor, a charging hole is provided on the top, a sieve plate is provided at the lower end inside the reactor, a gas outlet at the lower part of the reactor is directly connected with a second-stage reactor, and a cooling jacket is provided outside the reactor; the top of the second-stage reactor is communicated with the bottom of the first-stage reactor, the upper part of the second-stage reactor is provided with a solid carbon-containing raw material feeding port, the lower part of the second-stage reactor is provided with an outlet, the lower end in the reactor is provided with a sieve plate, the outside of the reactor is provided with a heating system, and the inside of the reactor is provided with a temperature measuring.
The reaction process for preparing carbon tetrafluoride by the equipment is as follows: solid carbon particles are added into a reactor through a top carbon raw material feeding port, the carbon particles are ignited by an ignition agent to react with fluorine gas during the reaction, the heat released by the reaction of the fluorine gas and the carbon particles is cooled through an upper cooling water cooling jacket 4 and is controlled by a thermometer, and the fluorine gas F2The fluorine gas enters the reactor through the fluorine gas inlet to react with carbon particles, carbon tetrafluoride generated in the first-stage reaction directly enters the second-stage reactor through the sieve plate, the second-stage reactor is provided with an electric heater to crack the first-stage product gas carbon tetrafluoride, the cracking is controlled by a thermometer to remove oxidizing substances in the mixed gas, and the generated carbon tetrafluoride gas enters the next process from the bottom product gas outlet.
Although the device has simple structure and convenient operation, the pressure fluctuation is large during the reaction, the carbon slag storage space after the reaction is too small, the carbon slag is easy to block the sieve plate, the full contact between carbon particles and fluorine gas is prevented, the reaction is quickly terminated, the fluorine gas capacity of the reactor is small, the reaction efficiency is relatively low, the reaction is incomplete, and the carbon slag at the bottom of the product gas outlet is easy to block.
SUMMERY OF THE UTILITY MODEL
To the above-mentioned technical problem in the prior art, the utility model provides a preparation carbon tetrafluoride gaseous device can overcome prior art's the above-mentioned not enough.
In order to achieve the technical purpose, the technical scheme of the utility model is realized as follows:
the utility model provides a device for preparing carbon tetrafluoride gas, includes the barrel, the barrel top is equipped with the carbon granule charge door, the lower part outside is equipped with the cooling water jacket in the barrel, barrel top side is equipped with the thick gas outlet of carbon tetrafluoride, the barrel lower extreme is violently managed the middle part with the barrel and is connected, fluorine gas import pipe is connected respectively to barrel violently pipe both ends upside, the barrel is violently managed the bottom of one end and is equipped with and drags for the sediment mouth, the barrel is violently managed inside and is equipped with the sieve, the barrel is violently managed the outside and is equipped with the electric heating radiant panel, electric heating radiant panel.
Furthermore, a cooling water outlet is formed in the upper end of the cooling water jacket, a cooling water inlet is formed in the right lower end of the cooling water jacket, the cooling water inlet and the cooling water outlet are communicated with the cooling water jacket, and a first thermometer is arranged at the middle lower part of the cooling water jacket.
Furthermore, a lifting lug is arranged on the outer side of the upper part of the cylinder body.
Furthermore, the outlet end of the fluorine gas inlet pipe extends into the middle part of the transverse pipe of the cylinder body, and a spray head is arranged at the outlet end of the fluorine gas inlet pipe.
The utility model has the advantages that: the device is of a horizontal structure, has a simple structure compared with an old-fashioned vertical reactor, is fed with gas from the lower part of the device through a fluorine inlet pipe, has large fluorine flow, large reaction zone space, large gas-solid contact area, more sufficient reaction and more convenient slag removal, filters fine slag through a bottom sieve plate, discharges products on the side surface of the top, prevents carbon slag blockage after the reaction of the fluorine gas and carbon particles, has a fluorine conversion rate higher than 98 percent, and is stable in process operation.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic view of a prior art apparatus for preparing carbon tetrafluoride;
FIG. 2 is a schematic view of an apparatus for producing carbon tetrafluoride according to the present invention;
FIG. 3 is a side view of an apparatus for manufacturing carbon tetrafluoride according to the present invention;
FIG. 4 is a top view of the apparatus for manufacturing carbon tetrafluoride according to the present invention;
in the figure: 1. carbon particle feed inlet, 2, lug, 3, cooling water outlet, 4, cooling water jacket, 5, thermometer I, 6, thermometer II, 7, fluorine gas inlet pipe, 8, barrel horizontal pipe, 9, electric heating radiant panel, 10, slag fishing port, 11, sieve plate, 12, cooling water inlet, 13, barrel, 14, carbon tetrafluoride crude gas outlet.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art all belong to the protection scope of the present invention.
As shown in fig. 2-4, according to the embodiment of the utility model, the device for preparing carbon tetrafluoride gas, including barrel 13, barrel 13 top is equipped with carbon granule charge door 1, the lower part outside is equipped with cooling water jacket 4 in barrel 13, barrel top side is equipped with carbon tetrafluoride crude gas export 14, barrel 13 lower extreme and barrel are violently managed 8 middle parts and are connected, fluorine import pipe 7 is connected respectively to 8 both ends upsides are violently managed to the barrel, the bottom that 8 one end was violently managed to the barrel is equipped with drags for sediment mouth 10, the barrel is violently managed 8 inside and is equipped with sieve 11, the barrel is violently managed 8 outsides and is equipped with electric heating radiant panel 9, electric heating radiant panel 9 upper portion is equipped with thermometer two 6.
The upper end of the cooling water jacket is provided with a cooling water outlet 3, the right lower end of the cooling water jacket is provided with a cooling water inlet 12, the cooling water inlet 12 and the cooling water outlet 3 are both communicated with the cooling water jacket 4, and the middle lower part of the cooling water jacket 4 is provided with a first thermometer 5. The outer side of the upper part of the cylinder body 13 is provided with a lifting lug 2. The outlet end of the fluorine inlet pipe 7 extends into the middle part of the transverse cylinder pipe 8, and a spray head is arranged at the outlet end of the fluorine inlet pipe 7.
The inside of the cylinder 13 is a gas phase area, a reaction area (A) is arranged above the sieve plate 11, a slag storage area (B) is arranged below the sieve plate 11, the reaction area and the slag storage area separate carbon particles of raw materials from fine carbon slag after reaction through the sieve plate 11, the reaction area can simultaneously use two fluorine gas inlet pipes to add fluorine gas to the device, and the fluorine gas is communicated with product gas.
The gas phase zone and the reaction zone both adopt 16 manganese steel.
For the convenience of understanding the above technical solutions of the present invention, the above technical solutions of the present invention are explained in detail through specific use modes below.
The utility model discloses a device of preparation carbon tetrafluoride prepares carbon tetrafluoride's reaction process is: solid carbon granules enter the reaction zone A through a raw material carbon granule feeding port 1. Electrifying the reaction area A and the slag storage area B through an electric heating radiation plate, heating carbon particles on the sieve plate 11, and controlling the temperature to be 200-350 ℃; the valves of fluorine gas inlets 7 at the left and right sides of the upper end of the bottom of the device (reactor) are opened to introduce fluorine, superheated carbon particles and fluorine gas react immediately, and generated carbon tetrafluoride CF4 enters the next stage of process from a product gas outlet 14 at the side of the top of the reactor, and the reaction equation is as follows:
6C+9F2＝CF4+C2F6+C3F8
simultaneously produces a plurality of by-product impurities SF6、SO2F2、C2F6、CO2、C3F8And the like. The reaction is violent, a lot of heat is generated at the same time, the reactor is cooled by cooling water passing through a cooling water jacket 4 and cooling water inlets 12 and outlets 3 of the reaction zone, the water temperature is controlled to be 50-80 ℃, and the pressure of the reactor is controlled to be +/-200 Pa. The reaction efficiency is more than 98 percent. During the reaction production, when the height of the carbon granules in the reaction area A is lower than the diameter of the transverse pipe of the cylinder body of the reactor, the valve of the fluorine gas inlet 7 is closed, the reactor is withdrawn, a standby reactor is put into use, and the reactor is blown with nitrogen, replaced completely, subjected to slag removal treatment and refilled with the carbon granules for standby.
Carbon tetrafluoride (CF) prepared by the utility model4) Wherein the contents of the components are shown in Table 1
TABLE 1 reactor outlet carbon tetrafluoride and other component contents
To sum up, with the help of the above-mentioned technical scheme of the utility model, admit air by the device low part through the fluorine import pipe, it is big to lead to fluorine gas volume, and the reaction zone space is big, and gas-solid area of contact is big, and the reaction is more abundant, and it is more convenient to remove the sediment, filters thin sediment through the bottom sieve, and top side product is gas-out, prevents that the carbon sediment after fluorine and carbon particle reaction from blockking up, and fluorine gas conversion rate is higher than 98%, and the technology operation is stable.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The utility model provides a device of preparation carbon tetrafluoride gas, includes barrel (13), barrel (13) top is equipped with carbon granule charge door (1), the lower part outside is equipped with cooling water jacket (4) in barrel (13), its characterized in that, barrel (13) top side is equipped with carbon tetrafluoride crude gas export (14), barrel (13) lower extreme and barrel are violently managed (8) middle part and are connected, fluorine import pipe (7) are connected respectively to barrel violently pipe (8) both ends upside, the bottom of barrel violently managing (8) one end is equipped with drags for cinder notch (10), barrel violently is managed (8) inside and is equipped with sieve (11), barrel violently manages (8) the outside and is equipped with electric heating radiant panel (9), electric heating radiant panel (9) upper portion is equipped with thermometer two (6).
2. The apparatus for manufacturing carbon tetrafluoride gas according to claim 1, wherein a cooling water outlet (3) is provided at an upper end of the cooling water jacket (4), a cooling water inlet (12) is provided at a lower right end of the cooling water jacket (4), the cooling water inlet (12) and the cooling water outlet (3) are both communicated with the cooling water jacket (4), and a first thermometer (5) is provided at a lower middle portion of the cooling water jacket (4).
3. The apparatus for manufacturing carbon tetrafluoride gas according to claim 1, wherein a lifting lug (2) is provided on an outer side of an upper portion of the cylinder (13).
4. The apparatus for producing carbon tetrafluoride gas according to claim 1, wherein the outlet end of the fluorine gas inlet pipe (7) extends to the middle of the cross tube (8) of the cylinder, and the outlet end of the fluorine gas inlet pipe (7) is provided with a shower head.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020227838.5U CN211964205U (en) | 2020-02-28 | 2020-02-28 | Device for preparing carbon tetrafluoride gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020227838.5U CN211964205U (en) | 2020-02-28 | 2020-02-28 | Device for preparing carbon tetrafluoride gas |
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| Publication Number | Publication Date |
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| CN211964205U true CN211964205U (en) | 2020-11-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202020227838.5U Active CN211964205U (en) | 2020-02-28 | 2020-02-28 | Device for preparing carbon tetrafluoride gas |
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| CN (1) | CN211964205U (en) |
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2020
- 2020-02-28 CN CN202020227838.5U patent/CN211964205U/en active Active
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Address after: No. 6, Gongye Road, Jiaoyang industrial concentration zone, Jiaoyang Town, Shanghang County, Longyan City, Fujian Province, 364204 Patentee after: Fujian del Technology Co.,Ltd. Address before: No. 6, Gongye Road, Jiaoyang industrial concentration zone, Jiaoyang Town, Shanghang County, Longyan City, Fujian Province, 364204 Patentee before: FUJIAN DEER TECHNOLOGY CO.,LTD. |
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