CN113607519A - Residual gas analysis device and method based on laser damage sample - Google Patents
Residual gas analysis device and method based on laser damage sample Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 31
- 230000006378 damage Effects 0.000 title claims abstract description 27
- 238000004868 gas analysis Methods 0.000 title claims abstract description 25
- 239000007789 gas Substances 0.000 claims abstract description 48
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052802 copper Inorganic materials 0.000 claims abstract description 23
- 239000010949 copper Substances 0.000 claims abstract description 23
- 238000004458 analytical method Methods 0.000 claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000012360 testing method Methods 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 239000002184 metal Substances 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 230000003068 static effect Effects 0.000 claims abstract description 6
- 238000005086 pumping Methods 0.000 claims description 5
- 229910000838 Al alloy Inorganic materials 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000005357 flat glass Substances 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000005340 laminated glass Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
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Abstract
The invention discloses a residual gas analysis device based on laser damage samples, which comprises a sample chamber, an analysis chamber, an all-metal angle valve, a needle valve, a laser, a full-range vacuum gauge, a cold cathode ionization vacuum gauge, a residual gas analyzer, a molecular pump set, a perforated oxygen-free copper plate, a nitrogen cylinder, a heating belt, a pressure regulator, a thermometer and a power supply. The invention destroys the sample by the external laser of the vacuum system, and has the advantages of accuracy, convenience and convenience, and is beneficial to maintaining the vacuum environment. In the experiment, the residual gas in the sample to be tested is subjected to gas quantity test and component analysis by a static boosting method and a small-hole flow guiding method.
Description
Technical Field
The invention relates to a residual gas analysis device and method based on laser damage samples, and belongs to the technical field of vacuum.
Background
In recent years, the application of vacuum technology is gradually wide, and the vacuum technology relates to various industrial fields. The service life of the glass is closely related to the vacuum degree and the gas composition in the cavity, such as a Micro Electro Mechanical System (MEMS) and a vacuum laminated glass, a Vacuum Insulated Panel (VIP) and the like.
In the existing residual gas analysis technology, a vacuum system internal destruction device is mostly adopted to destroy a sample and release internal gas for analyzing the residual gas amount and components in a closed cavity. The mechanical structures in the vacuum systems mostly have the problems of virtual leakage, air bleeding, difficult operation and the like.
Disclosure of Invention
In order to overcome the defects, the invention provides a residual gas analysis device and a residual gas analysis method based on laser damage samples, wherein a sample to be detected is damaged by an external laser of a vacuum system, the operation is simple, convenient and controllable, and the vacuum degree of the vacuum system is not influenced.
In order to solve the problems, the invention adopts the following technical scheme:
a residual gas analysis device based on laser damage to a sample comprises a sample chamber, an analysis chamber, an all-metal angle valve, a needle valve, a laser, a full-range vacuum gauge, a cold cathode ionization vacuum gauge, a residual gas analyzer, a molecular pump set, an oxygen-free copper plate with holes, a nitrogen cylinder, a heating belt, a pressure regulator, a thermometer and a power supply. The analysis chamber is provided with four flange ports, one of the four flange ports is connected with the air suction pipeline and the flow guide pipeline through a flange tee joint, the other flange port is connected with the molecular pump set through the all-metal angle valve, and the other two flange ports are respectively connected with the residual gas analyzer and the cold cathode ionization vacuum gauge.
A residual gas analytical equipment based on laser destroys sample, including the support frame, the support frame is the cuboid frame, is built by aluminium alloy ex-trusions.
According to the residual gas analysis device based on the laser damage sample, the sample chamber is made of stainless steel, and the volume of the sample chamber is measured by a gas expansion method.
According to the residual gas analysis device based on the laser damage sample, the heating power of the system is controlled through the heating belt and the pressure regulator, and the baking temperature is monitored in real time through the thermocouple.
According to the residual gas analysis device based on the laser damage sample, the pressure change of the sample to be tested before and after damage is tested by the full-range vacuum gauge, and the ionization vacuum gauge ensures that the residual gas analysis device is in the normal working pressure range.
The residual gas analysis device based on the laser damage sample is characterized in that an oxygen-free copper plate with holes is arranged between an all-metal angle valve and a flow guide pipeline, the oxygen-free copper plate is made of TU1 oxygen-free copper, and small holes with different sizes are machined in the center of the oxygen-free copper plate and used for controlling flow guide.
In order to enable the residual gas analyzer to have enough test time to sample and analyze the gas to be tested, the proper small hole conductance needs to be selected to limit the pumping speed of the molecular pump to the residual gas, and the theoretical size of the small holes of the oxygen-free copper plate can be calculated by the following process:
the degree of vacuum in the sample chamber after the sample is destroyed is calculated according to Boyle's law and is recorded as t being 0:
P1(t＝0)V1＝P2V2
in the formula, P1Is the pressure of the sample chamber, V1Is the sample chamber volume, P2Is the internal pressure, V, of the sample to be measured2Is the internal volume of the sample to be measured, and can estimate P after the sample is damaged1The size of (2). During the test, the gas flow through the orifice was:
q＝C×(P1-P3)
wherein C is a small bore conductance, P3Is the analysis chamber vacuum. For the sample chamber, the pumping equation can be listed:
in the formula, QoutThe sample chamber is the background leakage gas. Because the vacuum degree of the analysis chamber is far smaller than that of the sample chamber, the formula can be simplified as follows:
bringing the boundary condition t to 0, P1＝P1(t ═ 0) solving the differential equation yields:
suppose the limiting pressure of the system is PlimThe sampling time of one round of the residual gas analyzer is t0Then, the optional maximum conductance of the small holes on the oxygen-free copper plate can be calculated as follows:
for 20 ℃ air, the flow conductance of the pores under the molecular flow is calculated by the formula:
wherein d is the diameter of the small hole on the oxygen-free copper plate and is unit centimeter. By combining the above two formulas, the size selection of the small hole can be theoretically calculated.
The residual gas analysis method based on laser damage sample utilizes a laser externally arranged on a vacuum system to emit pulse laser to penetrate through an observation window glass, and a sample shell is damaged in a mode of cutting the sample, so that residual gas in the sample shell is released.
The residual gas analysis method based on laser sample destruction can be used for measuring the residual gas amount in the sample by using a static boosting method and a dynamic flow guiding method respectively, and analyzing the residual gas components by keeping the vacuum degree in an analysis cavity within the normal working range of a residual gas analyzer in a small hole difference mode.
Compared with the prior art, the invention has the advantages that:
firstly, the invention uses the pulse laser to punch holes on the surface of the sample to release gas, compared with the existing sample destruction mode, most of the sample destruction modes are vacuum system built-in mechanical structures, virtual leakage generated by gaps between the sample destruction modes, surface gas release and the like can deteriorate the vacuum environment, and the operation is difficult. The invention utilizes the external laser, can not influence the internal vacuum degree of the vacuum system, is convenient to operate and improves the working efficiency.
The device keeps the pressure in the analysis cavity within the safe working range of the residual gas analyzer in a differential mode through the small holes in the oxygen-free copper plate, and the measurement range is large.
And thirdly, the device is mainly used as a standard component, and has simple integral structure, convenient processing and low cost.
And fourthly, the invention can measure the residual gas quantity in the sample by respectively using a static boosting method and a dynamic flow guiding method, refers to the comparison, reduces the error and increases the reliability of the test result.
Drawings
FIG. 1 is a side view of a residual gas analysis apparatus based on laser destruction of a sample;
FIG. 2 is a schematic diagram of a residual gas analysis apparatus based on laser destruction of a sample;
wherein: 1 full-range vacuum gauge, 2 laser, 3 observation windows, 4 samples, 5 sample chambers, 6 needle valves, 7 nitrogen bottles, 8 first angle valves, 9 second angle valves, 10 oxygen-free copper plates with holes, 11 residual gas analyzers, 12 analysis chambers, 13 cold cathode ionization vacuum gauges, 14 third angle valves, 15 molecular pumps and 16 backing pumps.
Detailed Description
As shown in fig. 2, a residual gas analysis device and method based on laser damage sample is characterized in that: the device comprises a full-range vacuum gauge 1, a laser 2, an observation window 3, a sample 4, a sample chamber 5, a needle valve 6, a nitrogen cylinder 7, a first angle valve 8, a second angle valve 9, a perforated oxygen-free copper plate 10, a residual gas analyzer 11, an analysis chamber 12, a cold cathode ionization vacuum gauge 13, a third angle valve 14, a molecular pump 15 and a backing pump 16.
The sample chamber 5 is provided with five flange interfaces, one flange interface is provided with an observation window 3, the other four flange interfaces are respectively connected with the full-range vacuum gauge 1, a first angle valve 8, a second angle valve 9 and a needle valve 6, the other end of the needle valve 6 is connected with a pressure reducing valve of a nitrogen cylinder 7, the first angle valve 8 is connected with an air suction pipeline, the second angle valve 9 is connected with a flow guide pipeline, the analysis chamber 12 is provided with four flange ports, one flange port is connected with the air suction pipeline and the flow guide pipeline through a flange tee joint, one flange port is connected with a molecular pump 15 through a third angle valve 14 and then connected with a backing pump 16, and the other two flange ports are respectively connected with a residual gas analyzer 11 and a cold cathode ionization vacuum gauge 13.
The residual gas analysis device and method based on laser damage samples are provided with a support frame, wherein the support frame is a cuboid frame and is built by aluminum alloy sections, and the support frame is used for supporting the whole system and is convenient to heat and bake. The device is heated and baked by using a heating belt and a voltage regulator (not shown in the figure) to control the heating power, and the baking temperature is monitored by using a thermocouple in real time. The laser lens is positioned vertically above the observation window of the sample chamber, so that pulse laser can be conveniently emitted to destroy the sample. An oxygen-free copper plate 10 with holes is arranged between the all-metal angle valve 9 and the flow guide pipeline and is used for controlling flow guide. A series of oxygen-free copper plates 10 with holes are processed, the replacement is convenient, and the oxygen-free copper plates can be selected according to the air quantity in different samples. The analysis chamber 12 is connected with the needle valve 6 through a flange welded stainless steel pipe and a Shiviaoke collar, and is used for introducing nitrogen to protect a vacuum system. In addition, the connection of the rest parts is ultrahigh vacuum flange connection, the sealing performance is good, and the high-temperature baking can be borne.
The method for testing the residual gas quantity and analyzing the components of the sample is completed according to the following steps: opening a first angle valve 8, a second angle valve 9 and a third angle valve 14, closing a needle valve 6, opening a full-range vacuum gauge 1, opening a pre-pump 16 to pre-pump the vacuum system, observing the display of the full-range vacuum gauge 1, and opening a molecular pump 15 to pump the vacuum system to the limit pressure when the display is less than 10 Pa. Uniformly winding a heating belt on a vacuum system pipeline and a residual gas analyzer, inserting thermocouples into a plurality of positions to monitor the temperature in real time, uniformly wrapping aluminum foils, adjusting the voltage of a voltage regulator from low to high to control the temperature to be about 200 ℃, continuing for more than 24 hours until the system is pumped to the limit pressure, stopping heating, and waiting for the system to be pumped to the limit vacuum degree after the temperature is reduced to the room temperature. And (3) closing the first angle valve 8, the second angle valve 9 and the third angle valve 14, opening the needle valve 6, filling the nitrogen protection chamber, quickly opening the observation window 3, resealing the sample chamber 5 after putting the sample 4, and pumping the system to the limit vacuum degree again according to the operation. For the static boosting method, the first angle valve 8 and the second angle valve 9 are closed, the indication change of the full-range vacuum gauge 1 is recorded, the indication change is the background vacuum degree change of the sample chamber 5, and the first angle valve 8 is opened to re-pump the sample chamber 5 to the limiting pressure. Set up 2 parameters of laser instrument, set up the cutting path into circularly, adjust the radius according to the sample size, set up suitable laser power and translation rate, the observation window can be ablated to the too high power, crosses lowly then can lead to the interior gas of sample can not be released in the twinkling of an eye, uses 3 glasses of acetone and alcohol clean observation window to laser sees through destruction sample 4 better. And closing the first angle valve 8, emitting laser pulses to destroy the sample 4, preventing the glass surface temperature of the observation window 3 from being overhigh by air cooling and interrupting the laser pulses at intervals, observing and recording the indication change of the full-range vacuum gauge 1, and processing data to obtain a gas measurement test result in the sample by the static pressure-increasing method. For the dynamic flow guiding method, the first angle valve 8 is closed, the indication changes of the full-range vacuum gauge 1 and the cold cathode ionization vacuum gauge 13 are recorded, the background deflation of the sample chamber 5 can be obtained through calculation, and the first angle valve 8 is opened to re-pump the sample chamber 5 to the limit pressure. Opening a first angle valve 8, destroying the sample 4 by using a laser 2, observing and recording the indication changes of the full-range vacuum gauge 1 and the cold cathode ionization vacuum gauge 13, simultaneously opening a residual gas analyzer 11 to analyze the components of the gas to be detected, and processing data to obtain the residual gas quantity test and component analysis results in the dynamic flow guide method sample.
Claims (9)
1. A residual gas analysis device based on laser destroys sample which characterized in that: the device comprises a sample chamber, an analysis chamber, an all-metal angle valve, a needle valve, a laser, a full-range vacuum gauge, a cold cathode ionization vacuum gauge, a residual gas analyzer, a molecular pump set, an oxygen-free copper plate with holes, a nitrogen cylinder, a heating belt, a pressure regulator, a thermometer and a power supply; the analysis chamber is provided with four flange ports, one of the four flange ports is connected with the air suction pipeline and the flow guide pipeline through a flange tee joint, the other flange port is connected with the molecular pump set through the all-metal angle valve, and the other two flange ports are respectively connected with the residual gas analyzer and the cold cathode ionization vacuum gauge.
2. A laser damage sample based residual gas analysis apparatus according to claim 1, wherein: the support frame is a cuboid frame and is constructed by aluminum alloy sections.
3. A laser damage sample based residual gas analysis apparatus according to claim 1, wherein: the sample chamber is made of stainless steel, and the volume of the sample chamber is measured by a gas expansion method.
4. A laser damage sample based residual gas analysis apparatus according to claim 1, wherein: the system controls the heating power through a heating belt and a voltage regulator, and utilizes a thermocouple to monitor the baking temperature in real time.
5. A laser damage sample based residual gas analysis apparatus according to claim 1, wherein: the full-range vacuum gauge tests the pressure change of the sample to be tested before and after the sample to be tested is damaged, and the ionization vacuum gauge ensures that the residual gas analyzer is in the normal working pressure range.
6. A laser damage sample based residual gas analysis apparatus according to claim 1, wherein: an oxygen-free copper plate with holes is arranged between the all-metal angle valve and the flow guide pipeline, the oxygen-free copper plate is made of TU1 oxygen-free copper, and small holes with different sizes are machined in the center of the oxygen-free copper plate and used for controlling flow guide.
7. The method of claim 1, wherein the method comprises: in order to ensure that the residual gas analyzer has enough test time to sample and analyze the gas to be tested, a proper small hole conductance is selected to limit the pumping speed of the molecular pump to the residual gas, and the theoretical size of the small holes of the oxygen-free copper plate can be calculated by the following process:
the degree of vacuum in the sample chamber after the sample is destroyed is calculated according to Boyle's law and is recorded as t being 0:
P1(t＝0)V1＝P2V2 (1)
in the formula (1), P1 is the pressure of a sample chamber, V1 is the volume of the sample chamber, P2 is the internal pressure of the sample to be measured, V2 is the internal volume of the sample to be measured, and the size of P1 after the sample is damaged can be estimated; during the test, the gas flow through the orifice was:
q＝C×(P1-P3) (2)
in formula (2), C is the pore conductance, P3 is the analysis chamber vacuum; for the sample chamber, the pumping equation can be listed:
in the formula (3), Qout is the background leakage gas of the sample chamber; since the vacuum degree of the analysis chamber is far smaller than that of the sample chamber, the formula (2) is simplified as follows:
the differential equation is solved under the condition that the boundary condition t is 0 and the boundary condition P1 is P1(t is 0), so that:
assuming that the limiting pressure of the system is Plim and the sampling time of one round of the residual gas analyzer is t0, the selectable maximum conductance of the small holes on the oxygen-free copper plate is calculated as follows:
for 20 ℃ air, the flow conductance of the pores under the molecular flow is calculated by the formula:
in the formula (7), d is the diameter of a small hole in the oxygen-free copper plate and is unit centimeter; and (4) combining the above two formulas to calculate the size selection of the small hole.
8. The method of claim 1, wherein the method comprises: a laser device arranged outside the vacuum system is used for emitting pulse laser to penetrate through an observation window glass, a sample shell is damaged in a sample cutting mode, and residual gas in the sample shell is released.
9. The method of claim 1, wherein the method comprises: and respectively measuring the residual gas quantity in the sample by using a static boosting method and a dynamic flow guiding method, and analyzing the residual gas components by keeping the vacuum degree in the analysis cavity within the normal working range of the residual gas analyzer in a small hole differential mode.
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