CN103575918A - Device and method for detecting nitrogen trifluoride - Google Patents
Device and method for detecting nitrogen trifluoride Download PDFInfo
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- CN103575918A CN103575918A CN201310519856.5A CN201310519856A CN103575918A CN 103575918 A CN103575918 A CN 103575918A CN 201310519856 A CN201310519856 A CN 201310519856A CN 103575918 A CN103575918 A CN 103575918A
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Abstract
The invention relates to a device and method for detecting nitrogen trifluoride. The device for detecting nitrogen trifluoride comprises a high-temperature cracking furnace, a conversion pipe, a nitrogen dioxide sensor air chamber and an air extracting pump, wherein the high-temperature cracking furnace, a selective filter, the conversion pipe, a nitrogen dioxide sensor and the air extracting pump are sequentially connected through a pipe; a conversion agent is contained in the conversion pipe; and the nitrogen dioxide sensor is arranged in the nitrogen dioxide sensor air chamber. The method for detecting nitrogen trifluoride comprises the steps of (1) introducing air mixed with nitrogen trifluoride into the high-temperature cracking furnace, implementing cracking reaction, and cooling generated gas in a pipeline; (2) converting nitric oxide into nitrogen dioxide through the conversion agent in the conversion pipe; (3) detecting by the nitrogen dioxide sensor and outputting an electric signal; and (4) calculating concentration of the nitrogen trifluoride according to the detected electric signal and air inflow of the high-temperature cracking furnace in the step (1). The device is little in interference gas, does not use catalysts and is low in cost.
Description
Technical field
The invention belongs to Nitrogen trifluoride detection field, particularly a kind of apparatus and method that detect Nitrogen trifluoride.
Background technology
Nitrogen trifluoride is a kind of industrial special gas, mainly as propellant (rocket), fluorization agent, electron gas, plasma etching and for doping, laser, light transmitting fiber etc.Especially as a kind of good plasma etch gases, at current fast-developing microelectronic, be widely used.Nitrogen trifluoride is again a kind of toxicant simultaneously, has strong oxidizing property, with reductive agent, kickback can occur, and causes combustion explosion.Therefore, the leakage analyzing and testing of Nitrogen trifluoride is the needs of production safety, is also the needs of environmental protection.At present, catalytic pyrolysis+electrochemical process is a method of well analyzing Nitrogen trifluoride, the method utilizes the way that catalysis increases temperature to make Nitrogen trifluoride cracking, then with electrochemical sensor, detects the concentration of pyrolysis product, then calculates the concentration of Nitrogen trifluoride.Adopting the most outstanding advantage of analytical instrument of this thermal cracking+electrochemical process is to have superior long-time stability and environmental suitability.But, the external Nitrogen trifluoride analytical instrument (domestic without this quasi-instrument) of these principle research and development of application at present, in thermal cracking without exception all used catalyzer, although this method has realized Nitrogen trifluoride cracking at a lower temperature, because having used catalyzer, decomposition product is very complicated, the needed target detection gas of sensor---nitrogen dioxide content is less below, and interference gas is a lot, this just finally makes the overall performance of instrument good not, and testing result is undesirable.
Summary of the invention
For overcome that existing this quasi-instrument exists shortcoming, improve the performance of instrument, the invention provides a kind of apparatus and method that detect Nitrogen trifluoride, the detection object gas concentration of described generation is high, disturbs gas few, and does not need to use catalyzer, workable, analysis precision is high, and detectability is low, long service life.
A kind of device that detects Nitrogen trifluoride comprises high-temperature cracking furnace, conversion tube, nitrogen dioxide sensor air chamber, aspiration pump and special circuit.Described high-temperature cracking furnace, conversion tube, nitrogen dioxide sensor and aspiration pump are connected by pipeline successively; In described conversion tube, there is transforming agent, in described nitrogen dioxide sensor air chamber, have nitrogen dioxide sensor.
The device of described detection Nitrogen trifluoride also comprises selective filter, and selective filter is fixed between high-temperature cracking furnace and conversion tube.Dew, dust and chaff interference that selective filter is exported high-temperature cracking furnace in gas are removed, for good condition is created in the detection of nitrogen dioxide sensor.In the good situation of environmental baseline, also can save filtrator.
A kind of method that detects Nitrogen trifluoride, comprise the following steps: (1), the air that is mixed with Nitrogen trifluoride is passed in high-temperature cracking furnace, carry out cracking reaction, the gas producing outputs to the pipeline between high-temperature cracking furnace and selective filter cooling from the gas outlet of high-temperature cracking furnace, enter selective filter; (2), the transforming agent in conversion tube is converted into nitrogen dioxide by nitrogen monoxide, the concentration of nitrogen dioxide in raising secondary product; (3), nitrogen dioxide sensor detects the nitrogen dioxide composition in the gas of exporting in transforming agent, output electrical signals, the gas having detected is taken away by aspiration pump; (4), according to the air inflow of measured electric signal and gas circuit, can calculate the concentration of Nitrogen trifluoride.
1), detectability is low the present invention has following advantages:, the detectability of Nitrogen trifluoride can reach 0.05ppm; 2. precision is high, can reach 5%:3. long service life, owing to having saved catalyzer, does not exist other instruments to affect the life-span because of the existence of catalysis, and sensor is also more simple and reliable because noiseless device exists; 4. workable, can, by regulating the temperature of pyrolysis furnace, realize the detection of the different ranges of Nitrogen trifluoride, and external same quasi-instrument cannot be realized this function.(object gas that sensor below detects) 2), interference product reduced, the intersection of target is disturbed and is reduced.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
(Fig. 1 is schematic diagram of the present invention.）
Embodiment
As shown in Figure 1, a kind of device that detects Nitrogen trifluoride, comprise high-temperature cracking furnace, selective filter, conversion tube, nitrogen dioxide sensor air chamber and aspiration pump, described high-temperature cracking furnace, selective filter, conversion tube, nitrogen dioxide sensor and aspiration pump are connected by pipeline successively; In described conversion tube, there is transforming agent, in described nitrogen dioxide sensor air chamber, have nitrogen dioxide sensor.
The principal ingredient of described transforming agent can be MnO2, FeCl3 and KMnO4 etc. oxygenant.
In described high-temperature cracking furnace, there is temperature sensor.
The working temperature of described high-temperature cracking furnace is 600～1100 ℃.
The working gas flow of described high-temperature cracking furnace is 5mL/min～500mL/min.
The range of described nitrogen dioxide sensor is 1ppm～200ppm.
Or the range of nitrogen dioxide sensor is 0.1～20ppm.
The device of described detection Nitrogen trifluoride also comprises:
Signal processing circuit: the input end of signal processing circuit is electrically connected to the nitrogen dioxide sensor of nitrogen dioxide sensor air chamber, and output terminal is electrically connected to governor circuit;
Governor circuit: governor circuit one tunnel is electrically connected to ，Er road and is electrically connected to ，San road with temperature sensor in high-temperature cracking furnace and is electrically connected to liquid crystal display touch screen is two-way with pyrolysis furnace heating control circuit;
Pyrolysis furnace heating control circuit: pyrolysis furnace heating control circuit is electrically connected to the heater circuit of high-temperature cracking furnace;
And liquid crystal display touch screen: the function of LCDs finishing man-machine interaction, makes user be shielded and instrument to be completed to the related settings such as demarcation by touch LCD.
A kind of method that detects Nitrogen trifluoride, comprise the following steps: (1), the air that is mixed with Nitrogen trifluoride is passed in high-temperature cracking furnace, carry out cracking reaction, the gas producing outputs to the pipeline between high-temperature cracking furnace and selective filter cooling from the gas outlet of high-temperature cracking furnace, enter selective filter pyrolysis product is carried out to selective filter; (2), the transforming agent in conversion tube is converted into nitrogen dioxide by nitrogen monoxide, the concentration of nitrogen dioxide in raising secondary product; (3), nitrogen dioxide sensor detects the nitrogen dioxide composition in the gas of exporting in transforming agent, output electrical signals, the gas having detected is taken away by aspiration pump; (4), according to the air inflow of measured electric signal and gas circuit, can calculate the concentration of Nitrogen trifluoride.The scaling method of Nitrogen trifluoride concentration is: the Nitrogen trifluoride that first passes into three kinds of variable concentrations is demarcated instrument, every kind of Standard Gases all can a corresponding electric signal, so just formed three points, these three points connect into a broken line, each broken line relational expression is y=ax+b, and wherein y is concentration, the slope that a is this section of broken line, x is the magnitude of voltage of sensor output, the concentration at zero point that b is this broken line.When carrying out input, the electric signal that nitrogen dioxide sensor is produced is directly brought this relational expression into and just can be drawn corresponding concentration value.
First the gas that enters into device from air intake opening will carry out Pintsch process through high-temperature cracking furnace, pyrolysis gas is removed dust, chaff interference etc. through selective filter may cause the material of interference to electrochemical sensor, gas after selective filter transforms by transforming agent again, and the nitrogen monoxide in gas is converted into nitrogen dioxide.Gas after conversion continues by nitrogen dioxide sensor again, and nitrogen dioxide sensor output current signal is sampled, become the voltage signal that governor circuit can be sampled after the processing such as filtering through signal processing circuit.Governor circuit is carried the signal detecting to show in LCDs.LCDs is gone back the function of finishing man-machine interaction simultaneously, makes user be shielded and instrument to be completed to the related settings such as demarcation by touch LCD.
The functions such as the collection of the main settling signal of main control circuit, storage, man-machine interaction.If the concentration detecting surpasses alarming value, the relevant alarm of control is carried out to output alarm, when surpassing secondary alarm limit, in order to protect nitrogen dioxide sensor, aspiration pump will quit work.At this moment need instrument to be positioned in clean air, by operating manually, instrument is purged.
When the excess Temperature of pyrolysis furnace, instrument can cut off pyrolysis furnace heater circuit in time, plays the effect of protection pyrolysis furnace.After device start, first carry out initialization, from storer, read related setting value, the heating progress that shows pyrolysis furnace with the form of progress bar, reaches after design temperature when pyrolysis furnace being detected, by the gas concentration that automatically switches to the real-time demonstration of observation interface and monitor at present.If monitoring detectable concentration surpasses alarm limit by output alarm signal, and automatically stops aspiration pump, protect sensor to avoid the pollution of high concentrations of gas.By touching liquid-crystal display screen, can allow easily user and instrument carry out alternately, the function such as the demarcation, alarm limit that completes instrument set, alarm history record is checked.
Signal processing circuit mainly completes that sensor signal is stablized, the effect of filtering, amplification.Because electrochemical sensor output signal is microampere order signal, must signal process and just can give governor circuit and detect, otherwise owing to being subject to the impact of single-chip microcomputer sampling precision, do not collect sensor signal.The filtering of signal is necessary, otherwise cannot export a stable signal.
Claims (10)
1. a device that detects Nitrogen trifluoride, it is characterized in that: a kind of device that detects Nitrogen trifluoride, comprise high-temperature cracking furnace, conversion tube, nitrogen dioxide sensor air chamber and aspiration pump, described high-temperature cracking furnace, selective filter, conversion tube, nitrogen dioxide sensor and aspiration pump are connected by pipeline successively; In described conversion tube, there is transforming agent, in described nitrogen dioxide sensor air chamber, have nitrogen dioxide sensor.
2. detection Nitrogen trifluoride device according to claim 1, is characterized in that: also comprise that selective filter, selective filter are fixed between high-temperature cracking furnace and conversion tube.
3. detection Nitrogen trifluoride device according to claim 1, is characterized in that: also comprise:
Signal processing circuit: the input end of signal processing circuit is electrically connected to the nitrogen dioxide sensor of nitrogen dioxide sensor air chamber, and output terminal is electrically connected to governor circuit;
Governor circuit: governor circuit one tunnel is electrically connected to ，Er road and is electrically connected to ，San road with temperature sensor in high-temperature cracking furnace and is electrically connected to liquid crystal display touch screen is two-way with pyrolysis furnace heating control circuit;
Pyrolysis furnace heating control circuit: pyrolysis furnace heating control circuit is electrically connected to the heater circuit of high-temperature cracking furnace;
And liquid crystal display touch screen: the function of LCDs finishing man-machine interaction, makes user be shielded and instrument to be completed to the related settings such as demarcation by touch LCD.
4. detection Nitrogen trifluoride device according to claim 1, is characterized in that: the principal ingredient of described transforming agent can be MnO2, FeCl3 and KMnO4.
5. detection Nitrogen trifluoride device according to claim 1, is characterized in that: in described high-temperature cracking furnace, have temperature sensor.
6. detection Nitrogen trifluoride device according to claim 1, is characterized in that: the working temperature of described high-temperature cracking furnace is 600～1100 ℃.
7. detection Nitrogen trifluoride device according to claim 1, is characterized in that: the working gas flow of described high-temperature cracking furnace is 5～500mL/min.
8. detection Nitrogen trifluoride device according to claim 7, is characterized in that: the range of described nitrogen dioxide sensor is 1ppm～200ppm.
9. detection Nitrogen trifluoride device according to claim 1, is characterized in that: the range of described nitrogen dioxide sensor is 0.5～20ppm.
10. a method that detects Nitrogen trifluoride, it is characterized in that: comprise the following steps: (1), the air that is mixed with Nitrogen trifluoride is passed in high-temperature cracking furnace, carry out cracking reaction, the gas producing outputs to the pipeline between high-temperature cracking furnace and selective filter cooling from the gas outlet of high-temperature cracking furnace, enter selective filter; (2), the transforming agent in conversion tube is converted into nitrogen dioxide by nitrogen monoxide, the concentration of nitrogen dioxide in raising secondary product; (3), nitrogen dioxide sensor detects the nitrogen dioxide composition in the gas of exporting in transforming agent, output electrical signals, the gas having detected is taken away by aspiration pump; (4), according to the air inflow of measured electric signal and step (1) high-temperature cracking furnace, can calculate the concentration of Nitrogen trifluoride.
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| CN201310519856.5A CN103575918A (en) | 2013-10-28 | 2013-10-28 | Device and method for detecting nitrogen trifluoride |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108351323A (en) * | 2015-11-13 | 2018-07-31 | 新宇宙电机株式会社 | Catalyzed conversion formula sensor |
| CN110031510A (en) * | 2019-03-12 | 2019-07-19 | 北京时安科创仪器有限公司 | Catalytic combustion type methane concentration measuring system |
| CN113247870A (en) * | 2021-04-03 | 2021-08-13 | 中船重工（邯郸）派瑞特种气体有限公司 | Method and device for preparing high-purity nitrogen trifluoride gas |
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| US20040151630A1 (en) * | 2002-08-26 | 2004-08-05 | Hernandez Herbert A. | Total nitrogen and sulphur analysis using a catalytic combustion gas converter system |
| CN1450202A (en) * | 2003-04-30 | 2003-10-22 | 中国船舶重工集团公司第七一八研究所 | Technological method and equipment for preparing nitrogen trifluoride gas |
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Cited By (3)
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|---|---|---|---|---|
| CN108351323A (en) * | 2015-11-13 | 2018-07-31 | 新宇宙电机株式会社 | Catalyzed conversion formula sensor |
| CN110031510A (en) * | 2019-03-12 | 2019-07-19 | 北京时安科创仪器有限公司 | Catalytic combustion type methane concentration measuring system |
| CN113247870A (en) * | 2021-04-03 | 2021-08-13 | 中船重工（邯郸）派瑞特种气体有限公司 | Method and device for preparing high-purity nitrogen trifluoride gas |
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