CN108169321B - High-purity nitrogen detection method and device - Google Patents
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Abstract
The method is based on the ion mobility spectrometry principle, ionizes sample gas by adopting a negative corona ionization method to form ions, enables the formed ions to drift under the action of a drift electric field so as to separate impurity ions, and detects the separated impurity ions to obtain the impurity concentration in the sample gas. An apparatus for carrying out the method is further provided. The method improves the detection speed of the high-purity nitrogen, reduces the detection limit, and simplifies the structure of the device.
Description
Technical Field
The disclosure relates to the technical field of ion detection, in particular to a high-purity nitrogen detection method and device.
Background
High-purity gas plays an important role in modern industry, wherein high-purity nitrogen (N2) is one of the most widely used high-purity gases, and is mainly used in the industries of semiconductors, metallurgy, chemical industry, heat treatment, chemical fiber, food and the like. Protective gas N required in monocrystalline silicon preparation process in semiconductor industry2The purity of the N is more than 99.9999 percent, while the high-purity N produced in China at present2The purity is generally below 99.999%. The defect of the qualitative and quantitative detection method for the trace components in the high-purity gas is the bottleneck for further improving the purity of the high-purity gas in China. The impurity components in the high-purity nitrogen mainly comprise oxygen, water, carbon dioxide and the like, and the content of trace oxygen and water in the high-purity nitrogen has great influence on the process quality in the industries of semiconductors, chemical engineering and the like.
At present, the detection of trace impurities in high-purity gas is mainly carried out by a gas chromatography method. The method for detecting trace impurities in high-purity gas by using pulse discharge helium ionization chromatography is a new method which has just been developed in recent years, and has the advantages of high sensitivity and low detection limit. The pulse discharge helium ionization detector is a general-purpose detector with high sensitivity, and responds to both inorganic and organic compounds, so when analyzing trace impurities in a high-purity gas, it is necessary to perform separation by chromatography using a high-purity helium gas as a carrier gas. However, the following problems are mainly present when analyzing the impurity content in high-purity nitrogen gas: (1) after the large-component nitrogen enters the chromatograph, the photocurrent is extinguished, and the instrument is easily damaged; (2) the retention time of the large-component nitrogen in the chromatographic column is very long, so that the interval time of two analyses is very long, and the requirement of quick detection in industrial production cannot be met; (3) since PDHIDs are not selective, distinguishing between different impurities depends primarily on differences in their retention times in the column, resulting in an inability to detect the respective levels of certain impurities (e.g., oxygen and argon) in nitrogen.
In addition, the method can also be used for detecting the high-purity gas through atmospheric pressure ionization mass spectrometry, and because the impurities in the high-purity gas can be efficiently ionized under the atmospheric pressure condition, the method has extremely high sensitivity, becomes an extremely effective technical means in the analysis of trace impurities in the high-purity gas, and is particularly suitable for detecting 10-9mol/mol or even 10-12Gaseous impurities in the order of mol/mol concentration.
The atmospheric pressure ionization mass spectrum for detecting impurities in high-purity gas can be structurally divided into an ionization source, a mass analyzer, a gas sample introduction and correction system and the like. The ionization source is the most critical part of the mass spectrometer, and the ionization source commonly used for atmospheric pressure ionization mass spectrometry is a corona discharge ionization source63Both Ni radioactive ionization sources can work under atmospheric pressure and generate a large amount of reaction ions; the mass analyser is typically a quadrupole analyser, and a few mass spectra will fit into a triple quadrupole analyser; the gas sample introduction and correction system is different from a conventional mass spectrum structure in an atmospheric pressure ionization mass spectrum for pure gas analysis, and the whole system is required to be very clean and good in air tightness. However, the cost of the instrument is high and the sensitivity of the method is still to be improved in some gas analyses.
Disclosure of Invention
Technical problem to be solved
The present disclosure provides a high purity nitrogen detection method and apparatus to at least partially solve the above-identified technical problems.
(II) technical scheme
According to one aspect of the present disclosure, there is provided a high purity nitrogen detection method, including: ionizing the sample gas by a negative corona ionization method to form ions; the formed ions drift under the action of a drift electric field so as to separate impurity ions; and detecting the separated impurity ions to obtain the impurity concentration in the sample gas.
In some embodiments of the present disclosure, a second gas different from the sample gas is added as a drift gas in the ion drift region where the drift occurs, flowing against the ion drift direction; or adding a sample gas as a drift gas into the ion drift region where the drift occurs, so that the sample gas flow is ionized after passing through the ion drift region against the ion drift direction.
In some embodiments of the present disclosure, the ionization voltage of the sample gas is between-1.6 kv and-3.0 kv.
In some embodiments of the present disclosure, the drift electric field is a constant uniform electric field or an asymmetric alternating electric field.
In some embodiments of the present disclosure, the electric field strength of the constant uniform electric field is from 10V/cm to 500V/cm; the electric field intensity of the asymmetric alternating electric field is 10000V/cm-60000V/cm.
According to another aspect of the present disclosure, there is provided a high purity nitrogen gas detection apparatus including: an ionization unit for ionizing the sample gas from molecules into ions; an ion separation unit for separating impurity ions by drifting ions generated in the ionization unit; the ion detection unit is arranged at the tail end of the ion separation unit and is used for converting an ion signal into an electric signal; and
and the signal processing unit is electrically connected to the ion detection unit and used for receiving the electric signal of the ion detection unit, processing and calculating the electric signal to obtain the impurity concentration in the sample gas.
In some embodiments of the present disclosure, the ionization unit comprises a corona discharge ionization source selected from a corona discharge ionization source of a single needle structure, a needle-cylinder structure, a needle-mesh structure, or a double needle structure; the ion separation unit comprises a drift tube, and ions generated by the sample gas are drifted in the drift tube to realize the separation of impurity ions.
In some embodiments of the present disclosure, the drift tube comprises: an ionization region for collecting therein ions formed from the sample gas; a separation region for separating the formed impurity ions; and an ion gate disposed between the ionization region and the separation region for controlling ions drifting from the ionization region to the separation region.
In some embodiments of the present disclosure, the detection device further comprises: the sample introduction unit comprises a sample gas inlet, and the sample gas enters the detection device through the sample gas inlet; and a temperature control unit for performing temperature control on the ionization unit, the ion separation unit and the ion detection unit.
In some embodiments of the present disclosure, a sample gas inlet is provided at an end of the ion separation unit and a gas outlet is provided at the ionization unit, such that the sample gas flows within the ion separation unit against the ion drift direction and reaches the ionization unit to be ionized.
(III) advantageous effects
According to the technical scheme, the high-purity nitrogen detection method and the high-purity nitrogen detection device have at least one of the following beneficial effects:
(1) based on the principle of ion mobility spectrometry, high-purity nitrogen is ionized, ion separation detection is carried out by utilizing the difference of ion mobility speed, gas chromatography separation is not needed, and the rapid detection of trace impurities in high-purity gas can be realized.
(2) Detection by ion mobility spectrometry is advantageous for distinguishing certain impurities in high purity gases, such as oxygen and argon.
(3) The ion separation is carried out under certain air pressure (generally normal pressure), and compared with the atmospheric pressure ion mass spectrum, the ion separation device has the advantages of simple structure, low cost and convenient operation.
(4) High-purity nitrogen is used as drift gas, a sample gas inlet and a drift gas inlet are combined into a whole, the structure of the device is simplified, the detection limit is reduced, and the air tightness is improved.
Drawings
FIG. 1 is a schematic flow chart of a high purity nitrogen detection method according to a first embodiment of the disclosure.
Fig. 2 is a block diagram of a high purity nitrogen gas detection apparatus according to a first embodiment of the present disclosure.
Fig. 3 is a schematic structural diagram of a high-purity nitrogen gas detection device according to a first embodiment of the disclosure.
Fig. 4 is a schematic structural diagram of an ionization unit according to a first embodiment of the disclosure.
Fig. 5(a) is a signal spectrum obtained by detecting high purity nitrogen gas according to the first embodiment of the present disclosure.
FIG. 5(b) is a signal spectrum of a high purity nitrogen gas containing trace oxygen according to the first embodiment of the present disclosure.
FIG. 6 is a schematic structural diagram of a high-purity nitrogen gas detection device according to a second embodiment of the present disclosure.
Fig. 7 is a schematic structural diagram of a high-purity nitrogen gas detection device according to a third embodiment of the present disclosure.
Detailed Description
The invention discloses a high-purity nitrogen detection method and a device thereof, and the inventive conception is as follows: based on the principle of ion mobility spectrometry, a sample gas is ionized to form ions by adopting a corona ionization method, impurity ion separation is realized in a drift tube based on the difference of the drift velocity of different gas-phase ions in an electric field, and the separated impurity ions are detected by an ion detection unit. Drift velocity V of ionsdProportional to the drift electric field strength E: vdK · E; where K is the mobility coefficient/mobility of the ion, and is usually converted to reduced mobility K at 273K and 1.013X 105Pa0：K0K (273/T) (p/1.013 × 105), where T is the drift region temperature (unit: K) and p is the drift region gas pressure (unit: Pa). The ion separation detection can be realized at a certain air pressure (generally one atmospheric pressure or slightly lower than one atmospheric pressure), the detection speed is high, the detection limit is low, and the cost is low.
For the purpose of promoting a better understanding of the objects, aspects and advantages of the present disclosure, reference is made to the following detailed description taken in conjunction with the accompanying drawings.
The first embodiment:
as a first exemplary embodiment, a high purity nitrogen detection method and apparatus are provided. FIG. 1 is a schematic flow chart of a high purity nitrogen detection method according to a first embodiment of the disclosure. As shown in fig. 1, a method for detecting high purity nitrogen gas includes:
step A: and (4) sample introduction, namely sending the sample gas of the high-purity nitrogen into a high-purity nitrogen detection device.
And B: in the high-purity nitrogen gas detection device, the sample gas is ionized into ions by a negative corona ionization method, for example, if the sample gas contains a trace amount of oxygen, the ions are ionized into ions
And NO-(H2O)nPlasma impurity ions; if the sample gas contains trace amount of CO2Will ionize to form
And plasma impurity ions.
The corona discharge ionization method has the advantages of relatively simple structure, high ionization efficiency, no radiation damage and the like; the ionization voltage of the sample gas is-1.6 kv to-3.0 kv;
and C: the formed ions drift under the action of a drift electric field, and impurity ions are separated.
In the step, a constant uniform electric field in the traditional ion mobility spectrometry is used as a drift electric field, and the intensity of the drift electric field is 10V/cm-500V/cm, so that ions of different types can be separated according to the drift speed of the ions.
Of course, an asymmetric alternating electric field in a high-field asymmetric wave ion mobility spectrometry can be used as a drift electric field, so that ions of different types can be separated according to different change rules of the drift speed along with the electric field intensity, wherein the high field intensity of the asymmetric alternating electric field is 10000V/cm-60000V/cm;
in this embodiment, the high-purity nitrogen gas is also a drift gas while being used as a sample gas, and the sample gas is added into the ion drift region and flows against the ion drift direction, so that the cleaning of the detection device is facilitated on one hand, and the detection limit can be reduced on the other hand.
Step D: and carrying out ion detection on the separated ion current, and converting an ion signal into a current signal.
Step E: and processing and calculating the current signal to obtain the concentration of the trace impurities in the high-purity gas.
So far, the method for detecting high purity nitrogen gas of the present embodiment has been described. It should be noted that the high purity nitrogen gas detection method is implemented in a high purity nitrogen gas detection apparatus, and the structure of the high purity nitrogen gas detection apparatus of the present embodiment is as follows:
FIG. 2 is a block diagram of a high purity nitrogen detection device according to a first embodiment of the disclosure; fig. 3 is a schematic structural diagram of a high-purity nitrogen gas detection device according to a first embodiment of the disclosure. As shown in fig. 2 and 3, a high purity nitrogen gas detection apparatus includes: the sample introduction unit comprises a sample gas inlet, and the sample gas enters the detection device through the sample gas inlet; an ionization unit for ionizing the sample gas from molecules into ions; the ion separation unit is used for drifting the ions generated in the ionization unit so as to separate the impurity ions; the ion detection unit is arranged at the tail end of the ion separation unit and is used for converting an ion signal into an electric signal; the signal processing unit is connected with the ion detection unit and used for receiving the electric signal of the ion detection unit, processing and calculating the electric signal to obtain the impurity concentration in the sample gas; and a temperature control unit for performing temperature control on the ionization unit, the ion separation unit and the ion detection unit. The following further describes each constituent unit of the high purity nitrogen gas detection apparatus.
The sample gas inlet in the sample introduction unit is arranged at the tail end of the ion separation unit, the gas outlet is arranged at the ionization unit, so that the sample gas flows in the ion separation unit against the drift direction of ions and reaches the ionization unit to be ionized, and the cleanness of the interior of the device can be maintained. At the moment, the ocean gas inlet and the drift gas inlet are one, the measured sample gas is also drift gas, and compared with the traditional detection instrument based on the ion mobility spectrometry technology, the device has the advantages that the structure of the device is simplified, the detection limit is reduced, the air tightness of the device is improved, and the environmental interference is reduced.
The ionization unit adopts single-needle corona discharge to realize the ionization process of trace impurities in the sample gas, the structure of the ionization unit is shown in figure 4, the ionization unit comprises a corona discharge ionization source with a corona discharge needle, the structure is simplified, the maintenance is simple, and the discharge parameter optimization process can be omitted.
The ion separation unit comprises a drift tube, the drift tube comprises an ionization region and a separation region, an ion gate is arranged between the ionization region and the separation region, and when sample gas molecules are converted into ions in the ionization region through the ionization unit, part of the ions enter the separation region and drift towards the ion detection unit under the action of an electric field under the control of the ion gate.
The ion detection unit comprises a Faraday disc and is used for converting an ion signal into a current signal, and different ions reach the ion detection device at different times due to different ion drift speeds, so that the ion current signal changing along with the time is obtained in the ion detection device.
The specific structure of the signal processing unit and the temperature control unit is conventional in the art and is not related to the inventive step of the present disclosure, so that the detailed description thereof is omitted.
So far, the introduction of the high-purity nitrogen detection device of the embodiment is completed.
The high purity nitrogen gas and the high purity nitrogen gas containing a trace amount of oxygen were detected by the detection apparatus and method of this example, and signal spectra as shown in fig. 5(a) and 5(b) were obtained. As shown in fig. 5(a), electrons generated by ionization have a very large drift velocity in the electric field, and thus an electron peak is formed at a position near the drift time of 0 ms. As shown in FIG. 5(b), O is formed in the negative corona discharge in addition to electrons due to the presence of a small amount of oxygen2 -(H2O)nAnd NO-(H2O)nThe plasma has a small drift velocity in the electric field, and negative ion peaks are formed at positions near the drift time of 9.7ms and 11.1ms respectively, so that the composition and content information of trace impurities in high-purity nitrogen can be obtained according to the positions and heights of the ion peaks.
In the detection of high purity nitrogen, the content of "active" gases such as oxygen, carbon dioxide, etc. is of greater concern relative to the inert gas argon. In the method, the inert gas argon does not form negative ions under the ionization of the negative corona, so that the influence of trace argon in the high-purity nitrogen on the content detection of oxygen, carbon dioxide and the like is avoided.
Thus, the method and apparatus for detecting high purity nitrogen gas of the first embodiment have been described.
Second embodiment:
in a second exemplary embodiment of the present disclosure, a high purity nitrogen detection apparatus is provided. Fig. 6 is a schematic structural diagram of a high purity nitrogen gas detection apparatus according to a second embodiment of the present disclosure, as shown in fig. 6, compared with the high purity nitrogen gas detection apparatus of the first embodiment, the difference is that: the ionization source structure of the ionization unit comprises a corona discharge needle and a counter electrode plate with holes, the voltage of the discharge needle relative to the counter electrode plate with holes is between-1.6 kv and-3.0 kv, and the diameter of the counter electrode plate is about 1mm to 7 mm.
It is to be understood that the ionization source structure is not limited to the structures mentioned in the present embodiment and the first embodiment, and may be a corona discharge ionization source of a needle-cylinder structure, a needle-net structure, or a double-needle structure.
So far, the introduction of the high-purity nitrogen detection device of the second embodiment of the disclosure is completed.
The third embodiment:
in a third exemplary embodiment of the present disclosure, a high purity nitrogen detection apparatus is provided. Fig. 7 is a schematic structural diagram of a high purity nitrogen gas detection apparatus according to a third embodiment of the present disclosure, as shown in fig. 7, which is different from the high purity nitrogen gas detection apparatus according to the first embodiment in that: the sample gas inlet of the sample introduction unit is provided near the ionization source, and the drift gas inlet is provided separately, in this case, the drift gas does not need to be limited to the sample gas, and may be clean air or high-purity nitrogen gas other than the sample gas, but obviously, the apparatus structure is more complicated than that of the first embodiment.
So far, the introduction of the high-purity nitrogen detection device of the third embodiment of the disclosure is completed.
In conclusion, the high-purity nitrogen detection method and the high-purity nitrogen detection device provided by the disclosure are based on the principle of ionization mobility spectrometry, so that the detection speed is increased, the detection limit is reduced, further, the high-purity nitrogen is used as drift gas, a sample gas inlet and a drift gas inlet are combined into a whole, and the structure of the device is simplified.
It should also be noted that directional terms, such as "upper", "lower", "front", "rear", "left", "right", and the like, used in the embodiments are only directions referring to the drawings, and are not intended to limit the scope of the present disclosure. Throughout the drawings, like elements are represented by like or similar reference numerals. Conventional structures or constructions will be omitted when they may obscure the understanding of the present disclosure.
And the shapes and sizes of the respective components in the drawings do not reflect actual sizes and proportions, but merely illustrate the contents of the embodiments of the present disclosure. Furthermore, in the claims, any reference signs placed between parentheses shall not be construed as limiting the claim.
Unless otherwise indicated, the numerical parameters set forth in the specification and attached claims are approximations that can vary depending upon the desired properties sought to be obtained by the present disclosure. In particular, all numbers expressing magnitudes of voltages, magnitudes of electric field strengths, and so forth, used in the specification and claims are to be understood as being modified in all instances by the term [ about ]. Generally, the expression is meant to encompass variations of ± 10% in some embodiments, 5% in some embodiments, 1% in some embodiments, 0.5% in some embodiments by the specified amount.
Furthermore, the words "comprising" and "comprises" do not exclude the presence of elements or steps other than those listed in a claim.
In addition, unless steps are specifically described or must occur in sequence, the order of the steps is not limited to that listed above and may be changed or rearranged as desired by the desired design. The embodiments described above may be mixed and matched with each other or with other embodiments based on design and reliability considerations, i.e., technical features in different embodiments may be freely combined to form further embodiments.
The above-mentioned embodiments are intended to illustrate the objects, aspects and advantages of the present disclosure in further detail, and it should be understood that the above-mentioned embodiments are only illustrative of the present disclosure and are not intended to limit the present disclosure, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present disclosure should be included in the scope of the present disclosure.
Claims (8)
1. A high-purity nitrogen detection method comprises the following steps:
ionizing the sample gas by a negative corona ionization method to form negative ions or electrons;
the formed negative ions or electrons drift under the action of a drift electric field so as to separate impurity negative ions, wherein sample gas is added into an ion drift region where drift occurs to serve as drift gas, so that the sample gas flow is ionized after passing through the ion drift region against the ion drift direction; and
and detecting the separated impurity negative ions to obtain the impurity concentration in the sample gas.
2. The method for monitoring high purity nitrogen gas according to claim 1, wherein the ionization voltage of the sample gas is-1.6 kv to-3.0 kv.
3. The high purity nitrogen monitoring method of claim 1, wherein the drift electric field is a constant uniform electric field or an asymmetric alternating electric field.
4. The high purity nitrogen detection method of claim 3, wherein:
the electric field intensity of the constant uniform electric field is 10V/cm-500V/cm;
the electric field intensity of the asymmetric alternating electric field is 10000V/cm-60000V/cm.
5. A high-purity nitrogen gas detection device comprises:
an ionization unit for ionizing the sample gas from molecules into negative ions or electrons by a negative corona ionization method;
an ion separation unit for separating negative ions or electrons generated in the ionization unit from impurities by drift;
the sample introduction unit comprises a sample gas inlet, the sample gas enters the detection device through the sample gas inlet, the sample gas inlet is arranged at the tail end of the ion separation unit, and a gas outlet is arranged at the ionization unit, so that the sample gas flows in the ion separation unit against the drift direction of ions and reaches the ionization unit to be ionized;
the ion detection unit is arranged at the tail end of the ion separation unit and is used for converting negative ion signals into electric signals; and
and the signal processing unit is electrically connected with the ion detection unit and used for receiving the electric signal of the ion detection unit, processing and calculating to obtain the impurity concentration in the sample gas.
6. The high purity nitrogen detection apparatus of claim 5, wherein:
the ionization unit comprises a corona discharge ionization source, and the corona discharge ionization source is selected from a corona discharge ionization source with a single-needle structure, a needle-cylinder structure, a needle-net structure or a double-needle structure;
the ion separation unit comprises a drift tube, and is used for drifting negative ions or electrons generated by the sample gas in the drift tube so as to realize separation of impurity negative ions.
7. The high purity nitrogen detection apparatus of claim 6, wherein the drift tube comprises:
an ionization region for collecting therein negative ions or electrons formed from the sample gas;
a separation zone for separating the formed impurity negative ions; and
and the ion gate is arranged between the ionization region and the separation region and is used for controlling the negative ions or electrons to drift from the ionization region to the separation region.
8. The high purity nitrogen detection apparatus of claim 5, further comprising:
and the temperature control unit is used for controlling the temperature of the ionization unit, the ion separation unit and the ion detection unit.
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| CN2898824Y (en) * | 2006-06-08 | 2007-05-09 | 汪献忠 | Quantitative SF gas leakage detector |
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| CN1476534A (en) * | 2000-12-22 | 2004-02-18 | Method for measuring concentration of impurities in hitrgen, hydrogen and oxygen by means of ion mobility spetrometry | |
| CN1503907A (en) * | 2001-06-06 | 2004-06-09 | Method for measuring concentration of water in argon, hydrogen, nitrogen and helium by means of ionization mobility spectrometry | |
| CN1869648A (en) * | 2006-06-12 | 2006-11-29 | 中国科学院合肥物质科学研究院 | System for investigating harmful nano-particle in air |
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