CN211872100U - Device for preparing tungsten hexafluoride gas - Google Patents
Device for preparing tungsten hexafluoride gas Download PDFInfo
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- CN211872100U CN211872100U CN201922467283.1U CN201922467283U CN211872100U CN 211872100 U CN211872100 U CN 211872100U CN 201922467283 U CN201922467283 U CN 201922467283U CN 211872100 U CN211872100 U CN 211872100U
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- kettle
- electrolytic cell
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- tungsten hexafluoride
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Abstract
The utility model relates to a preparation tungsten hexafluoride gas's device belongs to fine chemistry industry technical field. The device comprises an electrolytic cell, a collection kettle, a charging steel cylinder, a vacuum and temperature control unit, wherein the electrolytic cell is used for electrolyzing to prepare fluorine, the anode of the electrolytic cell is a tungsten bar, the cathode of the electrolytic cell is a nickel copper plate, and the collection kettle is provided with a feed inlet, a discharge outlet and a vacuum pump connecting port; an anode gas outlet of the electrolytic cell is connected with a feed inlet of the collecting kettle through a pipeline, a filling steel cylinder is connected with a discharge outlet of the collecting kettle through a pipeline, and a vacuum pump is connected with a vacuum pump connecting port of the collecting kettle through a pipeline; the collection kettle is used for purifying the collected gas, and valves are arranged on the pipelines. Fluorine gas generated by electrolysis reacts with tungsten bars to generate a crude tungsten hexafluoride product, impurities are removed in a collection kettle, and the crude tungsten hexafluoride product is filled into a steel cylinder to obtain high-purity tungsten hexafluoride. The residence time of the fluorine gas in the equipment and the pipeline is reduced, the device has a simple structure, and the risk of the synthesis process is reduced.
Description
Technical Field
The utility model relates to a preparation tungsten hexafluoride gas's device belongs to fine chemistry industry technical field.
Background
Among the fluorides of tungsten, tungsten hexafluoride is the only species that is stable and industrially produced. Its main application is as raw material of tungsten Chemical Vapor Deposition (CVD) process in electronic industry, especially WSi made of it2Can be used as a wiring material in a large scale integrated circuit (LSI). With the development of semiconductor 3D-NAND technology, the demand for tungsten hexafluoride is rapidly increasing.
The traditional method for preparing tungsten hexafluoride gas is to react fluorine gas or nitrogen trifluoride with tungsten powder in a reaction vessel, and the fluorine gas needs to stay in the reactor for a certain time. The fluorine gas is strongly corrosive, and the reaction is exothermic, so that the process is relatively risky.
SUMMERY OF THE UTILITY MODEL
In view of this, the present invention provides an apparatus for preparing tungsten hexafluoride gas.
In order to achieve the above purpose, the technical scheme of the utility model is as follows:
an apparatus for producing tungsten hexafluoride gas, comprising: the device comprises an electrolytic cell, a collection kettle, a filling steel cylinder and a vacuum and temperature control unit, wherein the electrolytic cell is used for electrolyzing to prepare fluorine, the anode of the electrolytic cell is a tungsten bar, the cathode of the electrolytic cell is a nickel copper plate, and the purity of the tungsten bar is more than 99%; the mass fraction of carbon in the nickel copper plate is less than or equal to 0.5 percent; a feed inlet, a discharge outlet and a vacuum pump connector are arranged on the collection kettle; an anode gas outlet of the electrolytic cell is connected with a feed inlet of the collecting kettle through a pipeline, a filling steel cylinder is connected with a discharge outlet of the collecting kettle through a pipeline, and a vacuum pump is connected with a vacuum pump connecting port of the collecting kettle through a pipeline; the temperature control unit is used for controlling the temperature in the electrolytic bath and the collection kettle; the collecting kettle is used for purifying the collected gas, and the vacuum pump is used for vacuumizing the device; and valves are arranged on the pipelines.
Preferably, the device also comprises an absorption tower, and the absorption tower is connected with a cathode gas outlet of the electrolytic cell through a pipeline.
Preferably, the purity of the tungsten bar is 99.9% -99.9999%.
Preferably, the mass fraction of carbon in the nickel copper plate is less than or equal to 0.3 percent.
Preferably, in the method, the collection kettle and the connecting pipeline are both made of nickel-copper alloy.
Advantageous effects
The method uses the tungsten bar as the anode, electrolyzes the mixture of HF and KF, and the generated fluorine gas reacts with the tungsten bar in the electrolytic bath to generate tungsten hexafluoride, thereby reducing the residence time of the fluorine gas in the equipment and the pipeline, and the device has simple structure and reduces the risk of the synthesis process.
Drawings
FIG. 1 is a schematic structural view of the device of the present invention;
wherein, the method comprises the steps of 1-electrolytic bath, 2-collection kettle, 3-filling steel cylinder, 4-vacuum pump and 5-absorption tower.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
As shown in fig. 1, an apparatus for producing tungsten hexafluoride gas is characterized in that: the device comprises an electrolytic cell 1, a collecting kettle 2, a charging steel cylinder 3, a vacuum pump 4 and a temperature control unit, wherein the electrolytic cell 1 is used for electrolyzing to prepare fluorine, the anode of the electrolytic cell 1 is a tungsten bar, the cathode of the electrolytic cell 1 is a nickel copper plate, and the purity of the tungsten bar is more than 99%; the mass fraction of carbon in the nickel copper plate is less than or equal to 0.5 percent; a feed inlet, a discharge outlet and a vacuum pump connector are arranged on the collection kettle 2; an anode gas outlet of the electrolytic cell 1 is connected with a feed inlet of the collecting kettle 2 through a pipeline, a filling steel cylinder 3 is connected with a discharge outlet of the collecting kettle 2 through a pipeline, and a vacuum pump 4 is connected with a vacuum pump connecting port of the collecting kettle 2 through a pipeline; the temperature control unit is used for controlling the temperature in the electrolytic bath 1 and the collection kettle 2; the collection kettle 2 is used for purifying the collected gas, and the vacuum pump 4 is used for vacuumizing the device; and valves are arranged on the pipelines.
The device also comprises an absorption tower 5, and the absorption tower 5 is connected with the cathode gas outlet of the electrolytic cell 1 through a pipeline.
In the method, the collecting kettle and the connecting pipeline are both made of nickel-copper alloy materials.
Example 1
HF and KF are added into the electrolytic cell in a mass ratio of 1:1, a 99.9% purity tungsten bar is used as an anode, and a nickel-copper plate with a carbon content of 0.2% is used as a cathode. Opening all valves, vacuumizing to-0.099 MPa, heating the liquid in the electrolytic cell to 50 ℃, setting the electrolytic voltage to 10V and the current to 200A, starting electrolysis, reacting fluorine gas generated by electrolysis with tungsten strips to generate tungsten hexafluoride, absorbing cathode collecting gas by an absorption tower 5, then emptying, and collecting anode gas into a collection kettle 2. When the tungsten hexafluoride content in the collection kettle 2 reaches 160Kg, the electrolysis is stopped, only the valve on the connecting pipeline between the collection kettle 2 and the vacuum pump 4 is opened, the pressure in the collection kettle 2 is controlled to be-0.1 MPa, the temperature is controlled to be-160 ℃, and low-boiling-point impurities in the collection kettle 2 are discharged. And opening a valve on a connecting pipeline between the collection kettle 2 and the filling steel cylinder 3, heating the collection kettle 2 to 20 ℃, pressing gas in the collection kettle 2 into the filling steel cylinder 3 under 0.1MPa, and discharging residual heavy components in the collection kettle 2 through vacuum after heating.
And detecting the gas in the filling steel cylinder 3, wherein the gas is tungsten hexafluoride and the purity is 99.99 percent.
Example 2
HF and KF with the mass ratio of 1:1.5 are added into the electrolytic cell, a 99.999 percent purity tungsten bar is used as an anode, and a nickel-copper plate with the carbon content of 0.1 percent is used as a cathode. Opening all valves, vacuumizing to-0.05 MPa, heating the liquid in the electrolytic bath to 70 ℃, setting the electrolytic voltage to 7V and the current to 1000A, starting electrolysis, absorbing cathode collected gas by an absorption tower 5, then emptying, and collecting anode gas into a collection kettle 2. When the collection amount of tungsten hexafluoride in the collection kettle 2 reaches 120Kg, the electrolysis is stopped, only a valve on a connecting pipeline between the collection kettle 2 and the vacuum pump 4 is opened, the pressure in the collection kettle 2 is controlled to be-0.05 MPa, the temperature is controlled to be-50 ℃, and low-boiling-point impurities in the collection kettle 2 are discharged. And opening a valve on a connecting pipeline between the collection kettle 2 and the filling steel cylinder 3, heating the collection kettle 2 to 30 ℃, pressing gas in the collection kettle 2 into the filling steel cylinder 3 under 0.07MPa, and discharging residual heavy components in the collection kettle 2 through vacuum after heating.
And detecting the gas in the filling steel cylinder 3, wherein the gas is tungsten hexafluoride and the purity is 99.999 percent.
Example 3
HF and KF with the mass ratio of 1:0.5 are added into the electrolytic cell, a 99% purity tungsten bar is used as an anode, and a nickel-copper plate with the carbon content of 0.5% is used as a cathode. And opening all valves to pump the whole system to-0.099 MPa, heating the liquid in the electrolytic cell to 20 ℃, setting the electrolytic voltage to 7V and the current to 20A to start electrolysis, discharging the cathode collected gas after the cathode collected gas is absorbed by the absorption tower, and collecting the anode gas into the collection kettle. When the tungsten hexafluoride content in the collection kettle reaches 100Kg, the electrolysis is stopped, only the valve on the connecting pipeline between the collection kettle 2 and the vacuum pump 4 is opened, the pressure in the collection kettle 2 is controlled to be-0.1 MPa, the temperature is controlled to be 0 ℃, and low-boiling-point impurities in the collection kettle 2 are discharged. And opening a valve on a connecting pipeline between the collection kettle 2 and the filling steel cylinder 3, heating the collection kettle 2 to 70 ℃, pressing gas in the collection kettle 2 into the filling steel cylinder 3 under 0.05MPa, and discharging residual heavy components in the collection kettle 2 through vacuum after heating.
The gas in the steel cylinder 3 is detected to be tungsten hexafluoride, and the purity of the gas is 99.995%.
Example 4
HF and KF are added into the electrolytic cell in a mass ratio of 1:5, a 99.99% purity tungsten bar is used as an anode, and a nickel-copper plate with a carbon content of 0.3% is used as a cathode. Opening all valves to pump the whole system to-0.099 MPa, heating the liquid in the electrolytic cell to 200 ℃, setting the electrolytic voltage to 100V and the current to 2000A to start electrolysis, discharging the cathode collected gas after the cathode collected gas is absorbed by the absorption tower 5, and collecting the anode gas into the collection kettle 2. When the tungsten hexafluoride content in the collection kettle 2 reaches 200Kg, the electrolysis is stopped, only the valve on the connecting pipeline between the collection kettle 2 and the vacuum pump 4 is opened, the pressure in the collection kettle 2 is controlled to be-0.1 MPa, the temperature is controlled to be 0 ℃, and low-boiling-point impurities in the collection kettle 2 are discharged. And opening a valve on a connecting pipeline between the collection kettle 2 and the filling steel cylinder 3, heating the collection kettle 2 to 50 ℃, pressing gas in the collection kettle 2 into the filling steel cylinder 3 under 0.09MPa, and discharging residual heavy components in the collection kettle 2 through vacuum after heating.
And detecting the gas in the filling steel cylinder 3, wherein the gas is tungsten hexafluoride and the purity is 99.993%.
In summary, the present invention includes but is not limited to the above embodiments, and any equivalent substitutions or partial modifications made under the spirit and principle of the present invention are considered to be within the protection scope of the present invention.
Claims (5)
1. An apparatus for producing tungsten hexafluoride gas, comprising: the device comprises an electrolytic cell (1), a collecting kettle (2), a filling steel cylinder (3), a vacuum pump (4) and a temperature control unit, wherein the electrolytic cell (1) is used for preparing fluorine by electrolysis, the anode of the electrolytic cell (1) is a tungsten bar, the cathode of the electrolytic cell (1) is a nickel copper plate, and the purity of the tungsten bar is more than 99%; the mass fraction of carbon in the nickel copper plate is less than or equal to 0.5 percent; a feed inlet, a discharge outlet and a vacuum pump connector are arranged on the collection kettle (2); an anode gas outlet of the electrolytic cell (1) is connected with a feed inlet of the collecting kettle (2) through a pipeline, a filling steel cylinder (3) is connected with a discharge outlet of the collecting kettle (2) through a pipeline, and a vacuum pump (4) is connected with a vacuum pump connecting port of the collecting kettle (2) through a pipeline; the temperature control unit is used for controlling the temperature in the electrolytic bath (1) and the collection kettle (2); the collection kettle (2) is used for purifying the collected gas, and the vacuum pump (4) is used for vacuumizing the device; and valves are arranged on the pipelines.
2. The apparatus for producing a tungsten hexafluoride gas as recited in claim 1, wherein: the device also comprises an absorption tower (5), wherein the absorption tower (5) is connected with a cathode gas outlet of the electrolytic cell (1) through a pipeline.
3. The apparatus for producing a tungsten hexafluoride gas as recited in claim 1, wherein: the purity of the tungsten bar is 99.9% -99.9999%.
4. The apparatus for producing a tungsten hexafluoride gas as recited in claim 1, wherein: the mass fraction of carbon in the nickel copper plate is less than or equal to 0.3 percent.
5. The apparatus for producing a tungsten hexafluoride gas as recited in claim 1, wherein: the collection kettle (2) and the connecting pipeline are both made of nickel-copper alloy materials.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922467283.1U CN211872100U (en) | 2019-12-31 | 2019-12-31 | Device for preparing tungsten hexafluoride gas |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922467283.1U CN211872100U (en) | 2019-12-31 | 2019-12-31 | Device for preparing tungsten hexafluoride gas |
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| Publication Number | Publication Date |
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| CN211872100U true CN211872100U (en) | 2020-11-06 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201922467283.1U Withdrawn - After Issue CN211872100U (en) | 2019-12-31 | 2019-12-31 | Device for preparing tungsten hexafluoride gas |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111020619A (en) * | 2019-12-31 | 2020-04-17 | 中船重工（邯郸）派瑞特种气体有限公司 | Device and method for preparing tungsten hexafluoride gas |
-
2019
- 2019-12-31 CN CN201922467283.1U patent/CN211872100U/en not_active Withdrawn - After Issue
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111020619A (en) * | 2019-12-31 | 2020-04-17 | 中船重工（邯郸）派瑞特种气体有限公司 | Device and method for preparing tungsten hexafluoride gas |
| CN111020619B (en) * | 2019-12-31 | 2023-10-17 | 中船(邯郸)派瑞特种气体股份有限公司 | Device and method for preparing tungsten hexafluoride gas |
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Address after: 057550 No. five Weir Road, chemical industry gathering area, Feixiang District, Handan, Hebei, 1 Patentee after: China shipbuilding (Handan) Perry Special Gas Co.,Ltd. Address before: No.1 Weiwu Road, chemical industry gathering area, Feixiang County, Handan City, Hebei Province Patentee before: PERIC SPECIAL GASES Co.,Ltd. |
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Granted publication date: 20201106 Effective date of abandoning: 20231017 |
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| AV01 | Patent right actively abandoned |
Granted publication date: 20201106 Effective date of abandoning: 20231017 |