JP5963204B2 - Pre-calibrated micro leak filter for gas leak - Google Patents
Pre-calibrated micro leak filter for gas leak Download PDFInfo
- Publication number
- JP5963204B2 JP5963204B2 JP2013097052A JP2013097052A JP5963204B2 JP 5963204 B2 JP5963204 B2 JP 5963204B2 JP 2013097052 A JP2013097052 A JP 2013097052A JP 2013097052 A JP2013097052 A JP 2013097052A JP 5963204 B2 JP5963204 B2 JP 5963204B2
- Authority
- JP
- Japan
- Prior art keywords
- vacuum
- pressure
- gas
- pipe
- molecular flow
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Description
本発明は、標準混合ガスを真空容器に導入する際に用いる微小孔フィルターの校正方法及び校正装置に関し、特に、微粒子の焼結体で構成された微小孔フィルターであって、微小孔フィルターの校正方法により予め校正された圧力領域の範囲内の圧力において分子流を実現する微小孔フィルターに関する。 The present invention related standard mixed gas calibration method and calibration device of microporous filter used in introducing into the vacuum container, in particular, a microporous filter constituted by a sintered body of fine particles, microporous filter The present invention relates to a microporous filter that realizes a molecular flow at a pressure within a range of a pressure region calibrated in advance by the calibration method .
従来、標準混合ガスを、リークバルブ又はマスフローコントローラーを介して真空装置に導入する際には、気体の流れが途中で中間流になってしまうため、混合ガスの流量比が元の標準混合ガスの組成比と異なってしまい、予測できなくなるという問題があった。また、バルブの開度や元圧によっても、混合ガスの流量比が変化するため再現性がないという問題があった。
一方、本発明者は、非特許文献１において、純ガスを用いた分圧真空計の校正方法であって、焼結フィルターを用いて校正室に流れ込む気体が分子流となるようにしたものを提案している。しかしながら、非特許文献１の方法では、混合ガスを用いた校正を行うことができない。なぜなら、焼結フィルターの上流に、キャピラリーと副排気系を設けてあるため、これらの影響により、導入される混合ガスの流量比が、元の標準混合ガスの組成比と異なってしまうためである。さらに、提案した焼結フィルターは、微粒子の焼結体で構成されており、焼結条件などにより一つ一つの焼結フィルターでばらつきがあり、焼結フィルターを一個一個校正するための、校正方法及び校正装置の開発が必要であった。
Conventionally, when a standard mixed gas is introduced into a vacuum apparatus via a leak valve or a mass flow controller, the gas flow becomes an intermediate flow in the middle, so the flow rate ratio of the mixed gas is that of the original standard mixed gas. There is a problem that it is different from the composition ratio and cannot be predicted. Further, there is a problem in that there is no reproducibility because the flow rate ratio of the mixed gas changes depending on the opening degree and the original pressure of the valve.
On the other hand, the present inventor is a method for calibrating a partial pressure vacuum gauge using pure gas in Non-Patent Document 1, wherein the gas flowing into the calibration chamber using a sintered filter is a molecular flow. is suggesting. However, the method of Non-Patent Document 1 cannot perform calibration using a mixed gas. This is because the flow rate ratio of the introduced mixed gas differs from the composition ratio of the original standard mixed gas due to these effects because the capillary and the auxiliary exhaust system are provided upstream of the sintered filter. . Furthermore, the proposed sintered filter is composed of a sintered body of fine particles, and there are variations in each sintered filter depending on the sintering conditions, etc., and a calibration method for calibrating each sintered filter one by one And the development of calibration equipment was necessary.
本発明が解決しようとする問題点は、微粒子の焼結体で構成された微小孔フィルターであって、微小孔フィルターを流れる流体が分子流となるようにした標準混合ガスリーク用微小孔フィルターを一個一個校正するための、校正方法及び校正装置を提供することにある。分子流を実現すると、気体同士の相互作用が無くなるため、混合ガスを構成するそれぞれのガス種を独立に扱うことができる。 The problem to be solved by the present invention is a microporous filter composed of a sintered body of fine particles, and one microporous filter for standard mixed gas leak in which the fluid flowing through the microporous filter becomes a molecular flow. An object is to provide a calibration method and a calibration apparatus for calibrating one piece. When the molecular flow is realized, there is no interaction between gases, so that each gas type constituting the mixed gas can be handled independently.
本発明で利用した微小孔フィルター校正装置は、微小孔フィルターの上流に、標準混合ガス及び純ガスのガス導入系、容積輸送式真空ポンプ、上流圧力Ｐu測定用隔膜真空計を配置する。容積輸送式真空ポンプと隔膜真空計を用いる理由は、これらの特性にガス種依存性が無いためである。容積輸送式真空ポンプと隔膜真空計の動作圧力範囲から、微小孔フィルターの上流の圧力は１０2Ｐａ〜１０5Ｐａ程度が想定される。分子流を実現するためには、微小孔フィルターの孔径を、圧力の関数である気体の平均自由行程より小さくする必要がある。よって、１０2Ｐａ〜１０5Ｐａで分子流を実現するためには、微小孔フィルターの孔径を数十μm以下にする必要があり、実用的には１μm以下にすることが望まれる。また、微小孔フィルターの下流には、真空容器を配置し、前記真空容器には排気用高真空ポンプ、下流圧力Ｐd測定用全圧真空計、下流圧力Ｐd測定用分圧真空計を接続した微小孔フィルター校正装置において、微小孔フィルターを介して、真空容器に気体を導入した際、真空容器内部の圧力が、全圧真空計、分圧真空計の動作圧力範囲内にあるように、高真空ポンプの排気速度を選択して微小孔フィルターで分子流が実現されているかどうかを校正することを特徴とする。排気速度を調整するため、排気用高真空ポンプの前にオリフィスを設置する場合もある。
本発明は、微粒子の焼結体からなる微小孔フィルターと、前記微小孔フィルターの上流側に接続された真空用クロス配管と、該真空用クロス配管内の圧力を測定するために真空用クロス配管に接続された隔膜真空計からなる分子流を実現するためのガスリーク用微小孔フィルター装置であって、分子流を実現するための前記真空用クロス配管内の圧力領域について、予め、前記真空用クロス配管に接続されたガス導入系から純ガスを導入し、前記微小孔フィルターの下流に接続された真空容器を高真空ポンプで排気速度ＣPで排気し、前記真空用クロス配管内の圧力Ｐuを前記隔膜真空計で、前記真空容器内の圧力Ｐdを全圧真空計で測定し、式ＣF＝ＣPＰd／Ｐuを使って、前記真空用クロス配管内の圧力Ｐuを変えながらＣFを求め、ＣFが一定となる真空用クロス配管内の圧力Ｐ u の圧力領域を、分子流が実現している領域として校正しかつ値付けされていることを特徴とする。
また、本発明は、微粒子の焼結体からなる微小孔フィルターと、前記微小孔フィルターの上流側に接続された真空用クロス配管と、該真空用クロス配管内の圧力を測定するために真空用クロス配管に接続された隔膜真空計からなる分子流を実現するためのガスリーク用微小孔フィルター装置であって、分子流を実現するための前記真空用クロス配管内の圧力領域について、予め、前記真空用クロス配管に接続されたガス導入系から標準混合ガスを導入し、前記微小孔フィルターの下流に接続された真空容器を高真空ポンプでガス種ｉの排気速度ＣPiで排気したとき、前記真空用クロス配管内の全圧Ｐuを前記隔膜真空計で測定し、前記真空用クロス配管内の全圧Ｐuを変えながら前記真空容器のガス種ｉの分圧Ｐdiを分圧真空計で測定し、Ｐdi／Ｐu比が一定となる前記真空用クロス配管内の全圧Ｐ u の圧力領域を、分子流が実現している領域として校正し、さらに、ＣPi・Ｐdiの値と、ＣFi・Ｐu・ｍiの値と、ここで、ＣFiはガス種ｉの前記微小孔フィルターのコンダクタンス、ｍiは標準混合ガスにおけるガス種ｉの濃度である、を比較して両者が等しくなっている前記真空用クロス配管内の全圧Ｐ u の圧力範囲を、分子流が実現している圧力範囲として校正しかつ値付けされていることを特徴とする。
また、本発明は、微粒子の焼結体からなる微小孔フィルターと、前記微小孔フィルターの上流側に接続された真空用クロス配管と、該真空用クロス配管内の圧力を測定するために真空用クロス配管に接続された隔膜真空計からなる分子流を実現するためのガスリーク用微小孔フィルター装置であって、分子流を実現するための前記真空用クロス配管内の圧力領域について、予め、前記真空用クロス配管に接続されたガス導入系から標準混合ガスを導入し、前記微小孔フィルターの下流に接続された真空容器を高真空ポンプで排気速度ＣPiで排気し、前記真空用クロス配管内の全圧Ｐuを前記隔膜真空計で測定し、前記真空用クロス配管内の全圧Ｐuを変えながら前記真空容器の全圧Ｐdを全圧真空計で測定し、ＣFi・Ｐu・ｍiの値、ここで、ＣFiはガス種ｉの前記微小孔フィルターのコンダクタンス、ｍiは標準混合ガスにおけるガス種ｉの濃度である、を求め、この求めた値をさらにＣPiで除した値を全てのガス種ｉについて求めて総和し、この総和した値が、前記全圧真空計で測定した前記真空容器の全圧Ｐdと等しくなっている前記真空用クロス配管内の全圧Ｐ u の圧力範囲を分子流が実現している圧力範囲として校正しかつ値付けされていることを特徴とする。
In the micropore filter calibration apparatus used in the present invention, a standard mixed gas and pure gas introduction system, a positive displacement pump, and an upstream pressure Pu measurement diaphragm vacuum gauge are arranged upstream of the micropore filter. The reason for using a positive displacement vacuum pump and a diaphragm vacuum gauge is that these characteristics do not depend on the gas species. From the operating pressure range of the volumetric transport vacuum pump and diaphragm vacuum gauge, the pressure upstream of the microporous filter is assumed to be about 10 2 Pa to 10 5 Pa. In order to realize the molecular flow, it is necessary to make the pore diameter of the micropore filter smaller than the mean free path of gas as a function of pressure. Therefore, in order to realize the molecular flow at 10 2 Pa to 10 5 Pa, the pore diameter of the microporous filter needs to be several tens of μm or less, and is practically desired to be 1 μm or less. Further, in the downstream of the micropore filter, a vacuum vessel is arranged, the vacuum in the chamber high vacuum pump for evacuation, downstream pressure P d for measuring the total pressure vacuum gauge, connected downstream pressure P d for measuring partial pressure vacuum gauge In the micropore filter calibration apparatus, when gas is introduced into the vacuum vessel through the micropore filter, the pressure inside the vacuum vessel is within the operating pressure range of the total pressure vacuum gauge and the partial pressure vacuum gauge. The pumping speed of the high vacuum pump is selected to calibrate whether the molecular flow is realized by the micropore filter. In order to adjust the exhaust speed, an orifice may be installed in front of the high vacuum pump for exhaust.
The present invention relates to a micropore filter made of a sintered body of fine particles, a vacuum cross pipe connected to the upstream side of the micropore filter, and a vacuum cross pipe for measuring the pressure in the vacuum cross pipe A gas leak micropore filter device for realizing a molecular flow consisting of a diaphragm vacuum gauge connected to the vacuum cross-section for the pressure region in the vacuum cross pipe for realizing the molecular flow in advance. introducing a pure gas from a gas introduction system connected to the pipe, the micro vacuum container connected downstream of the hole filter was evacuated by the exhaust rate C P at the high vacuum pump, the pressure P u of the vacuum cross the pipe in the diaphragm gauge, said pressure P d of the vacuum container measured by the total pressure vacuum gauge, using the equation C F = C P P d / P u, the pressure P u in a cross-pipe the vacuum I asked the C F while changing, C F The pressure area of the pressure P u in the vacuum cloth in the pipe becomes constant, wherein the molecular flow is calibrated vital pricing as a region is realized.
The present invention also provides a microporous filter made of a sintered body of fine particles, a vacuum cross pipe connected to the upstream side of the microporous filter, and a vacuum for measuring the pressure in the vacuum cross pipe. A gas leak micropore filter device for realizing a molecular flow comprising a diaphragm vacuum gauge connected to a cross pipe, wherein the vacuum is previously applied to the pressure region in the vacuum cross pipe for realizing a molecular flow. When a standard mixed gas is introduced from a gas introduction system connected to a cross pipe for use, and a vacuum vessel connected downstream of the micropore filter is exhausted at a gas type i exhaust speed C Pi with a high vacuum pump, the vacuum the total pressure P u in use the cross in the pipe was measured by the diaphragm gauge, the partial pressure P di gas species i of the vacuum vessel while changing the total pressure P u of the vacuum cross the pipe in minutes pressure vacuum gauge Measure and P di / P u ratio pressure area of the total pressure P u of the vacuum cloth in the pipe becomes constant, calibrated as a region molecular flow is realized, further, the value of C Pi · P di, C Fi · the value of P u · m i, where, C Fi is the conductance of the microporous filter of the gas species i, m i is the concentration of a gas species i in the standard gas mixture, is equal both to compare the pressure range of the total pressure P u of the vacuum cloth in piping are characterized by molecular flow is calibrated vital pricing as pressure range is realized.
The present invention also provides a microporous filter made of a sintered body of fine particles, a vacuum cross pipe connected to the upstream side of the microporous filter, and a vacuum for measuring the pressure in the vacuum cross pipe. A gas leak micropore filter device for realizing a molecular flow comprising a diaphragm vacuum gauge connected to a cross pipe, wherein the vacuum is previously applied to the pressure region in the vacuum cross pipe for realizing a molecular flow. introducing a standard gas mixture from the gas introduction system connected to use the cross pipe, the micro vacuum container connected downstream of the hole filter was evacuated by the exhaust rate C Pi at the high vacuum pump, in cross piping the vacuum the total pressure P u measured by the diaphragm gauge, the total pressure P d of the vacuum container while changing the total pressure P u in a cross-pipe the vacuum measured in all pressure vacuum gauge, · C Fi · P u the value of m i, where, C Fi is the microporous filter of the conductance of the gas species i, m i is the concentration of a gas species i in the standard gas mixture, the calculated for all the value obtained by dividing this calculated value further C Pi of the gas species i calculated by summation, the total sum value is, the molecular flow pressure range of the total pressure P u of the total pressure vacuum gauge the vacuum chamber a total pressure P d equally turned by the vacuum cloth inside of the pipe and the measured by the It is characterized by being calibrated and priced as an actual pressure range.
本発明の校正方法及び校正装置を用いることにより、標準混合ガスリーク用微小孔フィルターを一個一個校正するための、校正方法及び校正装置が実現できた。 By using the calibration method and calibration apparatus of the present invention, a calibration method and calibration apparatus for calibrating each standard mixed gas leak micropore filter one by one could be realized.
混合ガスを、微小孔フィルターを介して真空容器に導入する。フィルター上流の圧力がある閾値以下(例えば１０ｋＰａ)になると、混合ガスが分子流を保ったまま真空容器に導入される。分子流では、気体同士の相互作用を無くなり、流量が気体の質量数の１／２乗に比例する。従って、元の混合ガスの組成比や圧力から、真空容器に導入される混合気体の流量や流量比を求めることができる。そこで、混合ガスが微小孔フィルターを介して分子流を保ったまま真空容器に導入されることを、標準混合ガスリークということにする。
微小孔フィルターの一例を、図３に示す。図３に示した例では、混合ガスがフィルター面に接する前に、中間流の影響を受けないように、フィルター面が前に突き出た形状になっている。
微小孔フィルターの校正とは、以下の２点を測定することである。
（１）分子流が実現される微小孔フィルター上流の圧力範囲
（２）微小孔フィルターの分子流コンダクタンス
コンダクタンスは、ユーザーの装置への適合性を判断する指標となり、また、微小孔フィルター上流圧力と温度を測定することにより、流量の絶対値を求めることができるようになる。
The mixed gas is introduced into the vacuum vessel through a microporous filter. When the pressure upstream of the filter falls below a certain threshold (for example, 10 kPa), the mixed gas is introduced into the vacuum vessel while maintaining the molecular flow. In the molecular flow, there is no interaction between gases, and the flow rate is proportional to the 1/2 power of the mass number of the gas. Therefore, the flow rate and flow rate ratio of the mixed gas introduced into the vacuum vessel can be obtained from the composition ratio and pressure of the original mixed gas. Therefore, the introduction of the mixed gas into the vacuum vessel through the microporous filter while maintaining the molecular flow is referred to as a standard mixed gas leak.
An example of the micropore filter is shown in FIG. In the example shown in FIG. 3, before the mixed gas contacts the filter surface, the filter surface protrudes forward so as not to be affected by the intermediate flow.
The calibration of the micropore filter is to measure the following two points.
(1) Pressure range upstream of the microporous filter where molecular flow is realized (2) Molecular flow conductance of the microporous filter Conductance is an index for determining suitability to the user's device, By measuring the temperature, the absolute value of the flow rate can be obtained.
本発明の校正は、図１に一実施例として示したような本発明の校正装置を用いて行う。図に示すように、微小孔フィルターの上流にガス導入系、容積輸送式真空ポンプ、隔膜真空計を配置する。容積輸送式真空ポンプと隔膜真空計は、原理的にガス種依存性が無いので、混合ガスの組成を変化せず、混合ガスの測定に問題もない。また、微小孔フィルターの下流に、真空容器、ターボ分子ポンプなどの高真空ポンプ、校正された全圧真空計(電離真空計、スピニングローター真空計など)と分圧真空計(質量分析計)を配置する。微小孔フィルターを介して、真空容器に気体を導入した際、真空容器内部の圧力が、全圧真空計、分圧真空計の動作圧力範囲内にあるように、高真空ポンプの排気速度を選択する。排気速度を調整するため、排気用高真空ポンプの前にオリフィスを設置する場合もある。 The calibration according to the present invention is performed using the calibration apparatus according to the present invention as shown in FIG. As shown in the figure, a gas introduction system, a volume transport vacuum pump, and a diaphragm vacuum gauge are arranged upstream of the micropore filter. Since the volumetric transport vacuum pump and the diaphragm vacuum gauge are not dependent on the gas species in principle, the composition of the mixed gas does not change, and there is no problem in the measurement of the mixed gas. Also, downstream of the micropore filter is a vacuum vessel, a high vacuum pump such as a turbo molecular pump, a calibrated total pressure vacuum gauge (ionization vacuum gauge, spinning rotor vacuum gauge, etc.) and a partial pressure vacuum gauge (mass spectrometer). Deploy. Select the pumping speed of the high vacuum pump so that the pressure inside the vacuum vessel is within the operating pressure range of the total pressure partial pressure gauge and the partial pressure vacuum gauge when the gas is introduced into the vacuum container through the micropore filter. To do. In order to adjust the exhaust speed, an orifice may be installed in front of the high vacuum pump for exhaust.
微小孔フィルターの上流圧力をＰu、下流圧力をＰd(真空容器内の圧力)、微小孔フィルターのコンダクタンスをＣF、高真空ポンプの排気速度をＣPとした時、流量が保存されることから、微小孔フィルターを通って真空容器内に導入される気体流量は高真空ポンプで排気される気体流量に等しいので以下の関係が成り立つ。
ＣF(Ｐu−Ｐd)＝ＣPＰd
ここで、Ｐu＞＞Ｐdであるから、ＣFＰu＝ＣPＰdとみなすことができ、よって、
ＣF＝ＣPＰd／Ｐu ・・・(１)
と表すことができる。
分子流が成立していると、ＣFは圧力に依存せずに一定となる。高真空ポンプの排気速度ＣPは予め見積もっておく。例えば、ターボ分子ポンプを使用すれば、ＣPは１０-2Ｐａ以下の圧力に対して一定値となるので便利である。
The flow rate is preserved when the upstream pressure of the micropore filter is P u , the downstream pressure is P d (pressure in the vacuum vessel), the conductance of the micropore filter is C F , and the exhaust speed of the high vacuum pump is C P. Therefore, since the gas flow rate introduced into the vacuum vessel through the micropore filter is equal to the gas flow rate exhausted by the high vacuum pump, the following relationship is established.
C F (P u −P d ) = C P P d
Here, since P u >> P d , it can be considered that C F P u = C P P d .
C F = C P P d / P u (1)
It can be expressed as.
If molecular flow is established, C F becomes constant without depending on pressure. Exhaust rate C P of the high vacuum pump is kept estimated beforehand. For example, if a turbo molecular pump is used, C P is convenient because it has a constant value for a pressure of 10 −2 Pa or less.
（１）純ガスを使った校正方法
図４のように、微小孔フィルター上流に純ガスを導入し、上流圧力Ｐuを隔膜真空計で、下流圧力Ｐdを全圧真空計で測定する。(１)式を使ってＣFを求める。さらに、図４のように上流圧力Ｐuを変えながらＣＦを求め、ＣFが一定となる圧力領域で分子流が実現しているので、その圧力範囲を求める。また、ガス種を変えてＣFを測定し、その比が気体の質量数の１／２乗になっていることからも、分子流が成立していることを示すことが出来る。
(1) As in the calibration method Figure 4 using pure gas, introducing a pure gas into the microporous filter upstream, the upstream pressure P u in diaphragm gauge to measure the downstream pressure P d at full pressure vacuum gauge. Find C F using equation (1). Further, as shown in FIG. 4, C F is obtained while changing the upstream pressure P u , and the molecular flow is realized in the pressure region where C F is constant, so the pressure range is obtained. In addition, the C F is measured by changing the gas type, and the ratio is the 1/2 power of the mass number of the gas, so it can be shown that the molecular flow is established.
（２）標準混合ガスを使った校正方法
図５のように、微小孔フィルター上流に標準混合ガスを導入し、上流圧力Ｐuを隔膜真空計で、下流圧力Ｐdを分圧真空計、または全圧真空計で測定する。
この時、標準混合ガス中のガス種ｉの流量Ｑiは、Ｐuiを上流のガス種ｉの分圧、ｍiを標準混合ガスにおけるガス種ｉの濃度、Ｐdiを下流のガス種ｉの分圧、ＣPiを高真空ポンプのガス種ｉの排気速度とすると、以下の式で表される。
＜微小孔フィルターの上流から真空容器＞
Ｑi＝ＣFiＰui＝ＣFi・Ｐu・ｍi (∵Ｐu＞＞Ｐd)・・・(２)
＜真空容器から排気＞
Ｑi＝ＣPi・Ｐdi ・・・(３)
（ｉ）分圧真空計を使った校正
図５のように上流の全圧Ｐｕを変化させながら、分圧真空計で真空容器内の分圧Ｐdiを測定し、Ｐdi／Ｐu比が一定となる圧力領域で、分子流が実現しているので、その圧力範囲を求める。さらに、(３)式を使ってＱｉを求め、この値と、ＣFiが質量数の１／２乗に比例しているとして(２)式を使って求めた値を比較し、両者が等しくなることからも、分子流が実現していることを示すことが出来る。
（ｉｉ）全圧真空計を使った校正
真空容器内の圧力Ｐdは、各ガス種の分圧の和になる。
At this time, the flow rate Q i of the gas type i in the standard mixed gas is such that P ui is the partial pressure of the upstream gas type i, m i is the concentration of the gas type i in the standard mixed gas, and P di is the downstream gas type i. Is expressed by the following equation, where C Pi is the exhaust speed of the gas type i of the high vacuum pump.
<Vacuum container from upstream of micropore filter>
Q i = C Fi P ui = C Fi · P u · m i (∵P u >> P d ) (2)
<Exhaust from vacuum vessel>
Q i = C Pi · P di (3)
(I) min while changing the total pressure P u in the upstream as calibration Figure 5 using pressure vacuum gauge to measure the partial pressure P di in the vacuum chamber at a partial pressure vacuum gauge, P di / P u ratio Since the molecular flow is realized in the pressure region where is constant, the pressure range is obtained. Furthermore, Q i is obtained using equation (3), and this value is compared with the value obtained using equation (2) assuming that C Fi is proportional to the 1/2 power of the mass number. It can be shown that the molecular flow is realized also from equality.
(Ii) Calibration using a total pressure vacuum gauge The pressure P d in the vacuum vessel is the sum of the partial pressures of each gas type.
上記した３種類の校正方法の長所と短所を、以下にまとめた。ユーザーの要求精度に応じて、これらの校正を組み合わせる。
＜Ｉの校正方法＞
使用ガス：純ガス
計測器：全圧真空計
長所：測定の再現性が良く、不確かさが小さい。コンダクタンスを精度良く測定できる。
短所：混合ガスの挙動を測定していない。
＜ＩＩの校正方法＞
使用ガス：標準混合ガス
計測器：分圧真空計
長所：混合ガスそれぞれの気体の挙動を直接測定できる。
短所：測定のバラツキが大きく、再現性が悪い。不確かさが大きい。
＜ＩＩＩの校正方法＞
使用ガス：標準混合ガス
計測器：全圧真空計
長所：測定の再現性が良く、不確かさが小さい。
短所：混合ガスの挙動を間接的に測定しているものの、気体それぞれの挙動まではわからない。
The advantages and disadvantages of the above three calibration methods are summarized below. These calibrations are combined according to the accuracy required by the user.
<I calibration method>
Gas used: Pure gas Measuring instrument: Total pressure vacuum gauge Advantage: Good reproducibility of measurement and small uncertainty. Conductance can be measured with high accuracy.
Cons: The behavior of the mixed gas is not measured.
<II calibration method>
Gas used: standard mixed gas Measuring instrument: partial pressure vacuum gauge Advantage: The gas behavior of each mixed gas can be measured directly.
Disadvantages: Large measurement variations and poor reproducibility. Uncertainty is great.
<III Calibration method>
Gas used: Standard gas mixture Measuring instrument: Total pressure vacuum gauge Advantage: Good reproducibility of measurement and small uncertainty.
Cons: Although the behavior of the mixed gas is indirectly measured, the behavior of each gas is not known.
なお、校正は、具体的には例えば図２に示すように、微小孔フィルターに真空用クロス配管を接続し、隔膜真空計を付属した状態で校正し、校正証明書を付属して頒布する。 Specifically, for example, as shown in FIG. 2, the calibration is performed by connecting a vacuum cross pipe to a micropore filter, with a diaphragm vacuum gauge attached, and distributing with a calibration certificate.
また、本発明の校正方法及び校正装置により校正された微小孔フィルターの使用例として、四重極質量分析計の標準混合ガスによる校正に使用する場合について説明する。
四重極質量分析計の構成手順
（１）ユーザーが保有する真空装置の排気速度や希望する圧力範囲といった条件から、微小孔フィルターを選択し、装置に接続する。
（２）任意の標準混合ガスを、微小孔フィルター上流に導入し、微小孔フィルター上流の圧力を、分子流が実現する圧力範囲内に設定する。
（３）＜ａ：流量比、または分圧比に対して校正する場合＞
ガス種Ａの流量、標準混合ガスの濃度、質量数をＱA、ｍA、ＭA、ガス種Ｂの流量、標準混合ガスの濃度、質量数をＱB、ｍB、ＭBとすると、ガス種ＡとＢの流量比は
In addition, as an example of use of the micropore filter calibrated by the calibration method and calibration apparatus of the present invention, a case where it is used for calibration with a standard mixed gas of a quadrupole mass spectrometer will be described.
Configuration Procedure of Quadrupole Mass Spectrometer (1) A micropore filter is selected and connected to the apparatus based on conditions such as the pumping speed of the vacuum apparatus owned by the user and the desired pressure range.
(2) An arbitrary standard mixed gas is introduced upstream of the microporous filter, and the pressure upstream of the microporous filter is set within a pressure range that realizes the molecular flow.
(3) <a: When calibrating against flow rate ratio or partial pressure ratio>
The flow rate of the gas type A, the concentration of the standard gas mixture, the mass number Q A, m A, M A, the gas type B flow rate, concentration of the standard gas mixture, the mass number Q B, m B, When M B, The flow ratio of gas types A and B is
と表される。
このとき、四重極質量分析計でガス種Ａとガス種Ｂの信号強度の比ＩA／ＩBを測定し、数式１の値と比較して四重極質量分析計の信号強度の比を流量比に対して校正する。また、ガス種ＡとＢの排気速度の比ＳA／ＳBが既知であれば、
It is expressed.
At this time, the signal intensity ratio I A / IB of the gas type A and the gas type B is measured with a quadrupole mass spectrometer, and the ratio of the signal intensity of the quadrupole mass spectrometer is compared with the value of Equation 1. Is calibrated against the flow ratio. Also, if the ratio S A / S B of the exhaust speeds of the gas types A and B is known,
ガス種ＡとＢの分圧の比ＰA／ＰBは、数式２で表される。このとき、四重極質量分析計でガス種Ａとガス種Ｂの信号強度の比ＩA／ＩBを測定し、数式２の値と比較することで、信号強度の比を分圧比に対して校正する。 The ratio P A / P B of the partial pressures of the gas species A and B is expressed by Equation 2. At this time, the signal intensity ratio I A / IB of the gas type A and the gas type B is measured with a quadrupole mass spectrometer, and the ratio of the signal intensity is compared with the partial pressure ratio by comparing with the value of Equation 2. And calibrate.
＜ｂ：流量、または分圧(絶対値)を校正する場合＞
微小孔フィルターの校正証明書に窒素(Ｍ＝２８)のコンダクタンスＣN2が記載されている場合、校正時の温度をＴCとすると、任意の気体ｉのコンダクタンスＣiは、
<B: When calibrating the flow rate or partial pressure (absolute value)>
When the conductance C N2 of nitrogen (M = 28) is described in the calibration certificate of the micropore filter, if the temperature at the time of calibration is T C , the conductance C i of any gas i is
となる。ここで、Ｍiは任意の気体ｉの質量数、Ｔはユーザーが使用する時の温度である。
任意の気体ｉの流量Ｑiは、微小孔フィルター上流圧力ＰUを測定することにより、任意の気体ｉの濃度ｍiとコンダクタンスＣiから、以下のように求められる。
It becomes. Here, M i is the mass number of an arbitrary gas i, and T is the temperature when the user uses it.
The flow rate Q i of an arbitrary gas i is obtained from the concentration mi of the arbitrary gas i and the conductance C i by measuring the micropore filter upstream pressure P U as follows.
数式４で得られたＱiと、四重極質量分析計の信号Ｉiを比較して、四重極質量分析計を流量に対して校正する。また、任意の気体iの排気速度Ｓiが既知であれば、 The quadrupole mass spectrometer is calibrated with respect to the flow rate by comparing Q i obtained by Equation 4 and the signal I i of the quadrupole mass spectrometer. If the exhaust speed S i of any gas i is known,
任意の気体ｉの分圧Ｐiは、数式５で表されるから、このときの、四重極質量分析計の信号強度のＰiを測定し、数式５の値と比較して四重極質量分析計を分圧に対して校正する。 Since the partial pressure P i of an arbitrary gas i is expressed by Equation 5, the signal intensity P i of the quadrupole mass spectrometer at this time is measured, and compared with the value of Equation 5, the quadrupole Calibrate the mass spectrometer for partial pressure.
校正対象として微小孔フィルターについて説明したが、分子流を生じさせるものであれば、本発明の校正方法及び校正装置が適用できる。 Although the micropore filter has been described as a calibration target, the calibration method and calibration apparatus of the present invention can be applied as long as they generate a molecular flow.
Claims (3)
分子流を実現するための前記真空用クロス配管内の圧力領域について、予め、前記真空用クロス配管に接続されたガス導入系から純ガスを導入し、前記微小孔フィルターの下流に接続された真空容器を高真空ポンプで排気速度ＣPで排気し、前記真空用クロス配管内の圧力Ｐuを前記隔膜真空計で、前記真空容器内の圧力Ｐdを全圧真空計で測定し、式ＣF＝ＣPＰd／Ｐuを使って、前記真空用クロス配管内の圧力Ｐuを変えながらＣFを求め、ＣFが一定となる真空用クロス配管内の圧力Ｐ u の圧力領域を、分子流が実現している領域として校正しかつ値付けされていることを特徴とする分子流を実現するためのガスリーク用微小孔フィルター装置。 A micropore filter made of a sintered compact of fine particles, a vacuum cross pipe connected to the upstream side of the micropore filter, and a vacuum cross pipe connected to measure the pressure in the vacuum cross pipe A gas leak micropore filter device for realizing a molecular flow consisting of a diaphragm vacuum gauge ,
For a pressure region in the vacuum cross pipe for realizing a molecular flow, a pure gas is introduced in advance from a gas introduction system connected to the vacuum cross pipe, and a vacuum connected downstream of the micropore filter. the vessel was evacuated by the exhaust rate C P at the high vacuum pump to measure the pressure P u of the vacuum cross the pipe in the diaphragm gauge, the pressure P d of the vacuum container in all pressure vacuum gauge, formula C using F = C P P d / P u, determine the C F while varying the pressure P u in the cross piping the vacuum, the pressure area of the pressure P u in the vacuum cloth in pipe C F is constant A gas leak micropore filter device for realizing a molecular flow characterized by being calibrated and priced as a region where the molecular flow is realized.
分子流を実現するための前記真空用クロス配管内の圧力領域について、予め、前記真空用クロス配管に接続されたガス導入系から標準混合ガスを導入し、前記微小孔フィルターの下流に接続された真空容器を高真空ポンプでガス種ｉの排気速度ＣPiで排気したとき、前記真空用クロス配管内の全圧Ｐuを前記隔膜真空計で測定し、前記真空用クロス配管内の全圧Ｐuを変えながら前記真空容器のガス種ｉの分圧Ｐdiを分圧真空計で測定し、Ｐdi／Ｐu比が一定となる前記真空用クロス配管内の全圧Ｐ ｕ の圧力領域を、分子流が実現している領域として校正し、さらに、ＣPi・Ｐdiの値と、ＣFi・Ｐu・ｍiの値と、ここで、ＣFiはガス種ｉの前記微小孔フィルターのコンダクタンス、ｍｉは標準混合ガスにおけるガス種ｉの濃度である、を比較して両者が等しくなっている前記真空用クロス配管内の全圧Ｐ u の圧力範囲を、分子流が実現している圧力範囲として校正しかつ値付けされていることを特徴とする分子流を実現するためのガスリーク用微小孔フィルター装置。 A micropore filter made of a sintered compact of fine particles, a vacuum cross pipe connected to the upstream side of the micropore filter, and a vacuum cross pipe connected to measure the pressure in the vacuum cross pipe A gas leak micropore filter device for realizing a molecular flow consisting of a diaphragm vacuum gauge ,
The pressure range of the vacuum cross the pipe to realize the molecular flow, in advance, by introducing a standard gas mixture from the connected gas introduction system to the cross pipe for the vacuum, which is connected downstream of the micropore filter when exhausted by exhaust rate C Pi of the gas species i the vacuum vessel in a high vacuum pump, the total pressure P u in a cross-pipe the vacuum measured by the diaphragm gauge, the total pressure P in the vacuum cloth pipe The partial pressure P di of the gas type i in the vacuum vessel is measured with a partial pressure gauge while changing u , and the pressure region of the total pressure Pu in the vacuum cross pipe where the P di / P u ratio is constant is determined. , calibrated as a region molecular flow is realized, further, the value of C Pi · P di, the value of C Fi · P u · m i , where, C Fi is the microporous filter gas species i Conductance, mi is the concentration of gas species i in the standard gas mixture Was the pressure range of the total pressure P u of the vacuum cloth in the pipe both are equal, the molecular flow, characterized by being calibrated vital pricing as a pressure range of molecular flow is realized A micro leak filter device for gas leak to realize .
分子流を実現するための前記真空用クロス配管内の圧力領域について、予め、前記真空用クロス配管に接続されたガス導入系から標準混合ガスを導入し、前記微小孔フィルターの下流に接続された真空容器を高真空ポンプで排気速度ＣPiで排気し、前記真空用クロス配管内の全圧Ｐuを前記隔膜真空計で測定し、前記真空用クロス配管内の全圧Ｐuを変えながら前記真空容器の全圧Ｐdを全圧真空計で測定し、ＣFi・Ｐu・ｍiの値、ここで、ＣFiはガス種ｉの前記微小孔フィルターのコンダクタンス、ｍiは標準混合ガスにおけるガス種ｉの濃度である、を求め、この求めた値をさらにＣPiで除した値を全てのガス種ｉについて求めて総和し、この総和した値が、前記全圧真空計で測定した前記真空容器の全圧Ｐdと等しくなっている前記真空用クロス配管内の全圧Ｐ u の圧力範囲を分子流が実現している圧力範囲として校正しかつ値付けされていることを特徴とする分子流を実現するためのガスリーク用微小孔フィルター装置。 A micropore filter made of a sintered compact of fine particles, a vacuum cross pipe connected to the upstream side of the micropore filter, and a vacuum cross pipe connected to measure the pressure in the vacuum cross pipe A gas leak micropore filter device for realizing a molecular flow consisting of a diaphragm vacuum gauge ,
For the pressure region in the vacuum cross pipe for realizing the molecular flow, a standard mixed gas was previously introduced from a gas introduction system connected to the vacuum cross pipe and connected downstream of the micropore filter . the vacuum vessel was evacuated by the exhaust rate C Pi at the high vacuum pump, wherein the total pressure P u in the vacuum cloth in the pipe was measured by the diaphragm gauge, the while changing the total pressure P u of the vacuum cross the pipe the total pressure P d of the vacuum container measured by the total pressure vacuum gauge, the value of C Fi · P u · m i , where, C Fi is the conductance of the microporous filter of the gas species i, m i is the standard gas mixture The value obtained by dividing the obtained value by C Pi was obtained for all the gas types i, and the total value was measured with the total pressure vacuum gauge. the vacuum which is equal to the total pressure P d of the vacuum container Total pressure P u gas leak for micropore filter device for realizing the molecular flow, characterized in that molecular flow pressure range is calibrated vital pricing as a pressure range that is realized in the cross pipe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2013097052A JP5963204B2 (en) | 2009-08-28 | 2009-08-28 | Pre-calibrated micro leak filter for gas leak |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2013097052A JP5963204B2 (en) | 2009-08-28 | 2009-08-28 | Pre-calibrated micro leak filter for gas leak |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2009197894A Division JP5419082B2 (en) | 2009-08-28 | 2009-08-28 | Calibration method and calibration device for standard mixed gas leak micropore filter |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2013156273A JP2013156273A (en) | 2013-08-15 |
| JP5963204B2 true JP5963204B2 (en) | 2016-08-03 |
Family
ID=49051556
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2013097052A Active JP5963204B2 (en) | 2009-08-28 | 2009-08-28 | Pre-calibrated micro leak filter for gas leak |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP5963204B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5703365B1 (en) | 2013-12-25 | 2015-04-15 | 株式会社ピュアロンジャパン | Manufacturing method of micropore filter |
| CN105675208B (en) * | 2015-02-03 | 2018-01-12 | 中国航天员科研训练中心 | Vacuum and leak rate Multifunctional school standard apparatus |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE602004030117D1 (en) * | 2004-09-17 | 2010-12-30 | Ronald Douglas Collins | Reference gas leak |
-
2009
- 2009-08-28 JP JP2013097052A patent/JP5963204B2/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| JP2013156273A (en) | 2013-08-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5419082B2 (en) | Calibration method and calibration device for standard mixed gas leak micropore filter | |
| JP5761706B2 (en) | Standard micro gas flow rate introduction method | |
| Tison | Experimental data and theoretical modeling of gas flows through metal capillary leaks | |
| US20200402783A1 (en) | Novel partial-pressure mass spectrometer calibration device and method | |
| US11874199B2 (en) | Device and process for determining the size of a leak hole in a sample | |
| JP6725614B2 (en) | Olfactory leak detector with nano-porous membrane | |
| US10254189B2 (en) | Static expansion method | |
| JP6878425B2 (en) | Leak detection using oxygen | |
| JP6630547B2 (en) | Method and apparatus for measuring transmission by mass spectrometry | |
| TWI555974B (en) | Gas permeability measuring device | |
| WO2004066048A1 (en) | Flow control method for clustering fluid and flow control device for clustering fluid | |
| Yoshida et al. | Newly developed standard conductance element for in situ calibration of high vacuum gauges | |
| JP5963204B2 (en) | Pre-calibrated micro leak filter for gas leak | |
| JPH05118972A (en) | Gas diluting system and method of diluting gas | |
| Brewer et al. | A dynamic gravimetric standard for trace water | |
| CN112781804B (en) | SF6 leak rate calibration stepless adjusting device and method | |
| JP5690070B2 (en) | Method and apparatus for measuring moisture concentration in silane gas | |
| Yoshida et al. | Calibration of ultra-fine helium leak rates for leak testing of microelectromechanical systems | |
| JP7219435B2 (en) | Pore size distribution measuring device for nanoporous membrane | |
| Detian et al. | Extension of the range of a constant-conductance flowmeter by a flow divider | |
| US8847156B2 (en) | Gas inlet for a process mass spectrometer | |
| Mohan | Vacuum gauge calibration at the NPL (India) using orifice flow method | |
| JP6122890B2 (en) | Test gas generator | |
| Yoshida et al. | Two-stage flow-dividing system for the calibration of vacuum gauges | |
| JP2006138641A (en) | Gas component analyzer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20130507 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20130515 |
|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20140407 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20140513 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20140603 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20141202 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20150115 |
|
| A02 | Decision of refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A02 Effective date: 20150602 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20160622 |
|
| R150 | Certificate of patent or registration of utility model |
Ref document number: 5963204 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |