JPH0448254A - Device and method for detecting desorbed gas - Google Patents

Abstract

PURPOSE:To improve the detecting performance by holding a vacuum chamber under a high vacuum even when measurement is not performed, and taking a sample in and out by using a load lock mechanism so that the vacuum is not destroyed. CONSTITUTION:When the sample 6 is taken in or out by opening a sample insertion hole 14 provided to the space 12 where the load lock mechanism is stored, an opening/closing valve 13 is closed and the vacuum state in the vacuum chamber 1 is not destroyed. Before the fed sample 6 is conveyed to the vacuum chamber 1, the space 12 where the load lock mechanism is stored is evacuated by vacuum pumps 2B and 3B of another system and then the opening/closing valve 13 is opened; and the sample 6 is conveyed into the vacuum chamber 1. The capacity of the space 12 where the load lock mechanism is stored is much smaller than that of the vacuum chamber 1, so that time required for placing the chamber in the vacuum state is short. Further, the possibility that gas enters the vacuum chamber 1 when the opening/closing valve 13 is opened is small.

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention is used for evaluating semiconductor chips. The present invention
In order to heat a sample (semiconductor chip) approximately 9 mm square in vacuum and observe the gas desorbed from the sample using a mass spectrometer, modify the semiconductor manufacturing process based on the observation results and improve the manufacturing yield. Make use of it.

〔overview〕

The present invention provides an apparatus for placing a sample in a vacuum chamber, heating the sample, and analyzing gas desorbed from the sample. By using a load-lock mechanism to take samples in and out without destroying the vacuum, the background noise generated is extremely small and detection performance is dramatically improved.

[Conventional technology]

A semiconductor chip as a sample is placed in a vacuum chamber, the semiconductor chip is irradiated with infrared rays to heat it, the gas desorbed from the semiconductor chip is guided to a mass spectrometer and measured, and the measurement results are used to determine the semiconductor manufacturing process. Techniques for evaluating and correcting processes are known.

This technique is extremely effective for improving the manufacturing yield of semiconductor manufacturing processes.

Conventional equipment for this purpose includes a vacuum chamber with an appropriate stage on which the sample is placed, a quartz glass window in the shell wall of the vacuum chamber, and infrared rays introduced into the vacuum chamber through this window to illuminate the sample. It was designed to heat the Furthermore, in order to take in and out the sample, it was necessary to break the vacuum in the vacuum chamber each time.

[Problem to be solved by the invention]

On the other hand, the semiconductor chip that is the sample is a small object with a thickness of about 1 mm or less on a 10 mm square surface, and it is processed extremely cleanly during the manufacturing process, so it is difficult to heat the sample at that time. The amount of gas desorbed from the sample is extremely small. However, as mentioned above, when the vacuum inside the vacuum chamber is broken, water vapor adheres to the inner walls of the vacuum chamber, the sample stage installed inside the vacuum chamber, and other surfaces, which can be heated during sample measurement. However, the emitted gas becomes background noise, reducing measurement accuracy.

The present invention solves this problem, and aims to provide an apparatus that can significantly reduce background noise that interferes with heating a sample and observing the gas desorbed from the sample.

[Means to solve the problem]

The inventor repeated evaluations to improve this measurement accuracy.

The first point to note is that the atmosphere, which causes background noise, should not be allowed to enter the vacuum chamber. To solve this problem, we decided not only to maintain the vacuum inside the vacuum chamber as samples are taken in and out, but also to keep the vacuum inside the vacuum chamber in a vacuum state for an extremely long period of time when no measurements are being made. In other words, a load-lock mechanism housed in a space whose volume is sufficiently smaller than that of the vacuum chamber is provided, and an on-off valve is used to separate the load-lock mechanism and the vacuum chamber, and only the load-lock mechanism is exposed to vacuum when loading and unloading samples. When the sample is transported to a vacuum chamber, the space in which the load lock mechanism is housed (referred to as "load lock chamber" in the explanation of the example) is separated from the vacuum chamber system. A structure was adopted in which the on-off valve was opened to create a vacuum state by means of means. Here, the separate vacuum means is preferably a vacuum pump that is separate from the vacuum system that maintains the vacuum state of the vacuum chamber, but even if some or all of the vacuum pumps are common, A vacuum system that does not affect the vacuum state of the vacuum chamber even when the vacuum of the load lock mechanism is broken.

The second point is to locally heat the sample.

In other words, in the conventional device, infrared rays are introduced through a large glass window installed in the shell wall of the vacuum chamber, so that it irradiates and heats areas other than the sample, that is, the shell wall surface of the vacuum chamber and equipment such as the manipulator installed inside the vacuum chamber. It was found that background gas was generated from these. To solve this problem, we decided to place the infrared lamp outside the vacuum chamber and use a glass rod (particularly a quartz glass rod) to introduce infrared light into the sample stage.

The glass rod has a cylindrical shape with a diameter of about 10 to 49 mm, and a length of 150 mm or more.

The third point is that devices not directly related to measurement are not left in the vacuum chamber during measurement. In other words, the sample transport device that extends from the load lock mechanism for loading and unloading the sample into the vacuum chamber, etc.
The structure was such that it was removed from the vacuum chamber during measurements.

The fourth point is that the vacuum chamber is made larger than the sample, so that even if the sample is heated, the walls of the vacuum chamber are not heated, and even if the sample is heated, heat is easily dissipated. If the volume of the vacuum chamber is increased, the desorbed gas will diffuse and become diluted, so there is no point in increasing the size of the vacuum chamber without limit. However, it was extremely effective to move the shell wall of the vacuum chamber away from the sample. Additionally, the vacuum chamber has a metal structure to increase heat conduction. In addition, the inner wall surface of the vacuum chamber is polished,
It has a structure that reflects infrared rays. Polishing the inner wall surface of the vacuum chamber also has the effect of preventing gas adsorption.

[Effect]

When opening the sample insertion port provided in the space in which the load lock mechanism is accommodated to insert or remove a sample, the opening/closing valve is kept closed so that the vacuum state within the vacuum chamber is not destroyed. Before transporting the loaded sample to the vacuum chamber, the space in which the load lock mechanism is housed is evacuated using a separate vacuum pump, the on-off valve is opened, and the sample is transported into the vacuum chamber. Since the volume of the space in which the load lock mechanism is accommodated is sufficiently smaller than the vacuum chamber, the time required to achieve the vacuum state is short. There is also a small possibility that gas will enter the vacuum chamber when the on-off valve is opened.

If the inner diameter of the vacuum chamber is 5 times or more the diameter of the sample stage and the distance from the sample stage to the ceiling is 50 mm or more, this heating operation is performed while the sample is being heated to generate desorption gas. This does not heat the internal walls of the vacuum chamber.

Therefore, background gas or background noise from these parts and the like is hardly generated.

Conversely, the reason why the volume within the vacuum chamber can be increased in this manner is that the vacuum state within the vacuum chamber is not destroyed when a sample is carried in, and the time required to create a high vacuum is short.

The wall structure of the vacuum chamber is a metal tube and metal end plates,
Since the inner wall surface is polished, the heating effect is enhanced by reflecting infrared rays, and furthermore, even if dust enters the interior, it is difficult to adhere to the inner wall surface.

The load lock function has a structure that allows the transport table on which the inserted sample is placed and the movement mechanism of this transport table to be removed from the vacuum chamber, so that gas released from this transport table etc. does not affect the measurement. There is no.

The load lock mechanism is a pinion and rack mechanism,
This pinion rotating shaft is equipped with a sealing structure equipped with double O-rings, and a vacuum is maintained between the double O-rings using a separate vacuum means, so the measurer can rotate the pinion rotating shaft with a knob or the like. Even when the transfer mechanism is operated to move the carrier into the vacuum chamber, no leakage occurs in the space in which the load lock is accommodated.

The heater is an infrared generator placed outside the vacuum chamber, and the generated infrared rays are introduced into the sample stage using a glass rod, so that only the sample stage placed inside the vacuum chamber is heated, and during analysis. There is almost no background noise.

When the vacuum pump includes a magnetically levitated turbomolecular pump, the pressure inside the machine is defined as lQ='torr (ltorr is
1.33 mi! Since it is possible to create an ultra-high vacuum state (J bar), mass spectrometry can be performed with great accuracy.

The inner diameter of the vacuum chamber is five times the diameter of the sample stage.
It is preferable that the distance from the sample stage to the ceiling is 50 mm or more.

If it is absolutely necessary to break the vacuum, dry nitrogen or dry air is introduced into the area. This prevents the ingress of moisture and other substances that cause background gas. When opening the sample insertion port in the load lock mechanism, dry nitrogen is introduced into the space outside the on-off valve.

〔Example〕

Next, embodiments of the present invention will be described with reference to the drawings.

FIG. 1 is an overall layout diagram of an embodiment of the present invention, FIG. 2 is a system diagram of the embodiment, and FIG. 3 is an explanatory diagram of a load lock mechanism of the embodiment.

In the figure, the desorption gas detection device includes a vacuum chamber 1 and vacuum pumps 2A and 3 that maintain this vacuum chamber in a vacuum.
A, a sample stage 5 placed on the west side of the vacuum chamber 1, a heater 7 for heating the sample 6, which is a semiconductor chip placed on the top surface of the sample stage 5, and a connecting tube 3 between the vacuum chamber 1 and the sample stage 5. and mass spectrometers 9, 10 and 11 connected via

Here, the features of the present invention are as follows: (1) It is covered with a load lock chamber 12 whose volume is sufficiently smaller than that of the vacuum chamber 1, and is equipped with an on-off valve 13 between it and the vacuum chamber 1, and is separate from the vacuum pumps 2A and 3A. The load lock chamber 1 is opened by vacuum pumps 2B and 3B of the system.
The present invention is equipped with a load lock mechanism that maintains the vacuum in the vacuum chamber 1, carries in the sample inserted from the sample insertion port I4, and places it on the sample stage 5 without destroying the vacuum state of the vacuum chamber 1. , the vacuum chamber 1 has an inner diameter approximately 7 times the diameter of the sample stage 5, and the distance between the sample stage 5 and the metal end plate 1Δ, which is the ceiling of the vacuum chamber 1, and the metal end plate 1Δ, which is the ceiling of the vacuum chamber 1, is a space of about 200 mm. ■ The wall structure of the vacuum chamber 1 is composed of a metal cylinder 1c and metal end plates IA and IB, and the inner wall surfaces of each are polished, ■ The load lock mechanism temporarily holds the sample. The transport table 15 to be placed and transported and the rack B16, which is a moving mechanism for the transport table 15, have a structure that allows them to be removed from the inside of the vacuum chamber 1;
7 and a rack portion 16 that meshes with the pinion 17.
A pinion rotating shaft 17A rotated by an external knob 18A is provided with a seal structure including an exhaust collar 20A in which double 01J rings 19A and 19B are arranged at predetermined positions with a spacer 19C. In order to maintain a vacuum inside the vacuum pumps 2A, 3A, 2
B and 3B are equipped with a rotary type vacuum pump 3C which is a separate vacuum means; ■ The heater 7 has an infrared generating lamp 21 placed at one focal point and a transparent quartz glass rod at the other focal point. 4 light receiving surface 4A
The infrared ray generator 7 is provided with a reflective surface 7A having a spheroidal inner surface on which the infrared ray generator 7 is arranged. Other end surface 4B of the light receiving surface 4A
2A of the vacuum pumps is a magnetically levitated turbo-molecular pump, and 2B of the vacuum pumps is a turbo-molecular pump, which allows the vacuum chamber 1 The interior of the load lock chamber 12 can be maintained at a high vacuum state higher than 10-9 torr, and the inside of the load lock chamber 12 can be maintained at a high vacuum state higher than IQ-'torr.

Furthermore, the characteristics of the method for detecting desorbed gas according to the present invention include: (1) While maintaining the vacuum chamber 1 in a high vacuum state, a sample is inserted into and taken out from the sample stage 5 inside the vacuum chamber 1 through the sample insertion port 14; In this detection method, when it is necessary to break the vacuum state, dry nitrogen or dry air is introduced into that part, that is, when the vacuum inside the load lock chamber 12 is broken, the cock 22A is used. When dry nitrogen or dry air is introduced into the interior of the vacuum chamber 1 and the vacuum of the vacuum chamber 1 is to be broken if necessary, the cock 22B
The method is to introduce dry nitrogen or dry air.

Next, the arrangement of this embodiment will be explained using FIG. 1.

Each component of this embodiment is arranged approximately on the disk 23, and includes rotary pumps 3A and 3B of the vacuum pump;
The cooling water tank 24 and the combination unit 25 are arranged outside the disk 23.

The on-off valve 13 is provided with a rotating shaft 26 that opens and closes the slide valve 13A by gripping the slide valve 13A and rotating the slide valve 18B.
This rotating shaft 26 is sealed by a bellows.

The vacuum chamber 1 is communicated with the ionization section 9 of the mass spectrometer via a connecting tube 8 having a large diameter. This connecting pipe 8 is connected to the magnetically levitated turbo molecular pump 2A through a main exhaust pipe 8A. Following the ionization section 9, the excitation section 10 and collector
A ridge portion 11 is provided.

A manipulator 27 is provided in the vacuum chamber 1 at a position facing the load lock mechanism. This manipulator 27 transfers the sample on the conveyance table 15 that has approached the sample stage 5 to the sample stage 5 by the above-mentioned rack section 1G,
It's about to go back.

Next, the operation of each component will be explained individually.

In Fig. 3, in the load lock mechanism, the transport platform 1
5 and the rack section 16 are moved toward the end 12A side of the load-lock chamber 12, and the transport table 15 is located substantially below the sample insertion port 14. At this time, the on-off valve 13 is closed by the slide valve 13A.

When opening the sample insertion port 14, first open the cock 2.
2A is opened, the inside of the load lock chamber 12 is filled with dry nitrogen N2, the sample insertion port 14 is opened, and the sample is placed on the transfer table 15. Next, close cock 22A,
Open cock 22D to perform preliminary exhaust, then open cock 22D.
2C is opened and the inside of the load lock chamber 12 is evacuated.

After the vacuum state becomes almost the same as that of the vacuum chamber 1 according to the vacuum gauge 28A, the on-off valve 13 is opened, and the pinion 17 is rotated using the knob 18A to move the rack section 16 toward the vacuum chamber 1 side. When the transport table 15 approaches a predetermined position on the sample stage 5, the tip of the rack section 16 comes into contact with a stopper 16A provided in the vacuum chamber 1.

The manipulator 27 is used to transfer the sample placed on the carrier 15 to the sample stage 5 in this state.

In FIG. 7 Q: 1) showing a longitudinal cross-sectional view of the manipulator 27, a flange 27B is provided on a sheath body 27A having a strong structure on a metal cylinder IC which is a shell of a vacuum chamber.

Knobs 18C and 18D, which are first and second operating ends, are provided in the atmospheric pressure atmosphere outside this flange 27B.

There is a tubular outer shaft 27C that moves substantially horizontally in a radial direction from the center of the vacuum chamber by operating the knob 18C, which is the first operating end, and a first working end 27E is attached to one end of the shaft 27C via a bearing 27D.

Inside this outer shaft 27C, there is an inner shaft 27F whose relative position changes in the longitudinal direction along the outer shaft 27C.
A knob 18D, which is the second operating end, is located at one end of the outer side of 7F.
is attached, and a second working end 27 is attached to the other end of this inner shaft 27F.
G is provided.

The tip of the outer shaft 27C inside the vacuum chamber and the flange 27B
A first bellows 28A that expands and contracts according to the displacement of the outer shaft 27C is placed between the seat 27H fixed to the seat 27H, and a first bellows 28A that expands and contracts according to the displacement of the outer shaft 27C is placed between the inner shaft 27F and the outer shaft 27C.
Second bellows 2 expands and contracts according to relative displacement with 7F
8B is covered. Further, between the first working end 27E and the second working end 27G, an inverted U-shaped pawl 27 suspended by a leaf spring 27J is attached.

By providing two bellows in this manner, leakage within the vacuum chamber due to operation of each operating end is prevented.

Under normal conditions, that is, without sample exchange,
By operating the knob 18C, both the outer shaft 127C and the inner shaft 27F are pulled out to the right in the figure, the first bellows 28A is compressed, and the first and second working ends 27E and 27G are moved toward the sheath body 27A. being drawn.

As described above, when the transport table 15 of the load lock mechanism is close to the sample stage 5, the knob 18, which is the -th operating end, is pressed.
C, the outer shaft 27C and the inner shaft 27F are inserted into the vacuum chamber, and the claw 27K is moved to the position indicated by the broken line. In the vicinity of the conveyor table 15, the knob 18D is operated so as to push the inner shaft 27F to the left side in the figure with respect to the outer shaft 27C. As a result, the second bellows 28B is extended, and the distance between the first and second working ends 27E and 27G is reduced, so that the leaf spring 27J
is pushed out and descends to the claw 27. Here knob 18C
When the outer shaft 27C and the inner shaft 27F are both moved to the right side in the figure by operating the sample, the sample on the carrier 15 can be transferred onto the sample stage 5. In this way, the sample can be transferred.

This operation is performed while observing through a viewing window IE (shown by a broken line in FIGS. 7 et al.) provided in the metal cylinder 1c of the vacuum chamber.

The infrared ray generator 7 is disposed outside and below the vacuum chamber 1, and the infrared rays generated by the infrared ray generator 21 placed at one focal point of the spheroidal reflective surface 7A inside the infrared ray generator 7 are placed at the other focal point. It is absorbed through the light-receiving surface 4A of the quartz glass rod 4, and introduced into the lower surface of the sample stage 5 through the other end surface 4B. The infrared generating lamp 21 is connected to the computer unit 25
A predetermined temperature is applied to the sample stage 5 by the power supplied from the temperature control hole 29 controlled by the temperature control hole 29 . In order to prevent the heat generated by the reflective surface 7A from dissipating to the outside of the infrared ray generator 7, cooling water is supplied from the cooling water tank 24 to the outside of the reflective surface 7A through the pipe 3OA.

FIG. 4 is a diagram of the sample stage. The glass rod 4 is made of transparent quartz glass, and the stage 5 is made of semi-transparent quartz glass. As shown in FIG. 4(b), the lower surface of the sample stage 5 has a fitting portion 5A that fits into the end surface 4B of the glass rod 4, and a fitting portion 5A that fits loosely with the end surface 4B. A hole 5B is provided in the gap and communicates with the atmosphere inside the vacuum chamber.

Thereby, even if the sample stage 5 is heated, the glass rod 4 will not be heated due to its influence. Sample stage 5
The thermocouple 21A is inserted through the hole 5C provided in the upper part of the hole 5C.

A sealing structure is also provided in the portion of the glass rod 4 that penetrates the metal end plate IB of the vacuum chamber. Similar to the seal structure provided on the pinion shaft 17A of the load lock mechanism described above, this seal structure also has double ○ rings 19D and 1 on the exhaust collar 20B.
9E and a spacer 19F are provided to maintain the degree of vacuum inside the vacuum chamber 1.

This exhaust collar 20B is evacuated by a vacuum pump 3c, which is a vacuum means separate from the vacuum pumps that evacuate the vacuum chamber 1 or the four-door lock chamber 12, respectively.

On the other hand, the cooling water that has cooled the infrared ray generator 7 as described above is sent to the cooling water passage 31 provided outside the exhaust collar 20B via the pipe 30B, and then transferred to the cooling water tank via the pipe 30C. It will be sent back on the 24th. In the second case, the sealed portion is cooled, and the maintenance of the vacuum state described above is not hindered by heat.

FIG. 5 is a diagram showing the structure of a mass spectrometer.

As shown in this figure, the ionization chamber 9A in the ionization section 9 is an open type with a plurality of openings 9B, and the ionization section 9 and the vacuum chamber 1 are connected by a connecting pipe 8, which is a thick and short passage. ing.

In general sample introduction to a mass spectrometer, desorption gas generated by the sample 6 placed on the sample stage is once collected and sent to the ionization chamber 9A through a narrow passage. In this method, there is a slight time lag between the time when the desorbed gas is generated and the time when the desorbed gas is ionized by the electrode, making real-time analysis impossible.

In this example, the desorption gas 33G generated from the sample 6 is guided into the ionization section 9 without being accumulated, and enters the ionization chamber 9A through the opening 9B, where it is bombarded by an electron beam from a filament (not shown). Ionized. The ion beam 33E extracted from the ionization chamber 9A by the extraction electrode 9C is deflected by the magnetic field of the iron core 10A of the excitation section 10 and detected by the collector section 11.

Next, referring to FIG. 2, the operating procedure of this embodiment will be explained.

- Close the on-off valve 13, open the cock 22A, and fill the load lock chamber 12 with dry nitrogen N2.

- Open the sample insertion port 14 and insert the sample into the transport platform 15.

- Close the cock 22A and close the sample insertion port 14.

・Open cock 22D and remove rotary vacuum pump 3C.
Pre-exhaust.

- Close the cock 22D, open the cock 22C, and exhaust the inside of the load lock chamber 12 with the turbo molecular pump 2B.

- Check the ultimate pressure in the load lock chamber 12 using the vacuum gauge 32A, and open the on-off valve 13.

- Rotate the pinion 17 with the knob 18A, and move the transport platform 15 into the vacuum chamber 1 with the stopper 1 using the rack part 16.
6A, and then move the transport platform 15 to the sample stage 5.
to the side.

- Using the manipulator 27, transfer the sample 6 on the transport platform 15 onto the sample stage 5.

- Separate the manipulator 27 from the sample stage l.

- Pull the conveyor table 15 etc. back into the load lock chamber 12.

- Close the on-off valve 13.

- Check the ultimate vacuum level of the vacuum chamber etc. using the vacuum gauge 32B.

- Load a temperature increase program that controls the temperature control section 29 etc. on the computer unit 25.

- The computer unit 25 sets the mass number of the desorbed gas to be measured by the mass spectrometer.

・Start analysis (raise the temperature and import the temperature signal into the computer unit, and at the same time import the ion current signal of the set mass number).

・Analysis and measurement completed.

- Open the on-off valve 13, place the carrier 15 next to the stage 5, and use the manipulator 27 to transfer the sample onto the carrier.

- Raise the transport platform 15 etc. into the load lock chamber 12 and close the opening valve.

- Open the cock 22A and fill the load lock chamber 12 with dry nitrogen N2.

・Open the sample insertion port 14 and replace the sample.

-Meanwhile, the computer unit 25 processes the analysis data and prints out a relationship diagram (pyrogram) between ion current and temperature.

The results of pyrograms analyzed according to the present embodiment according to the above operating procedure are shown in FIGS. 8(a) and 8(a).

In this figure, the vertical axis is the relative value of the ionic current. Figure 8 (a
) l: As shown, the ion current value is almost constant even in the flat parts before and after the peak values of mass number M=18 (If20) and mass M"28 (C2H4). This is due to noise. This means that the contamination of M-
18 and M=28 values remain unchanged. This indicates that there is no background noise due to gases released from sources other than the sample.

As a comparative example, FIG. 8(C) shows an example of analysis and measurement that is said to be the best recent example reported at the American Institute of Electrical and Electronics Engineers (IEEE) conference held in April 1990. In this figure, the vertical axis is arranged to be the absolute value of the ion current, but for example, in the curve for M = 18, the flat 3BL part on the high temperature side of the peak value is sloped more than the flat part on the low temperature side, as shown by the broken line. are doing. This is considered to be an effect of background noise.

FIG. 9 is a family diagram of another embodiment of the present invention.

Since this is almost the same as the example shown in FIG. 2, detailed explanation will be omitted. In detail, only the piping system and valves are slightly different.

[Effect of ribbing]

As described above, according to the present invention, background noise is generated to an extremely low level during mass spectrometry detection of desorbed gas from a sample. Measurements are performed reliably in real time. With the present invention, inconveniences in each manufacturing process of samples such as semiconductor chips can be clearly pointed out.

This has the effect of significantly reducing the defective rate in the semiconductor production process and greatly improving the yield.

[Brief explanation of the drawing]

FIG. 1 is an overall layout diagram of an embodiment of the present invention, (a) is a front view, and (b) is a plan view. FIG. 2 is a system diagram of the same embodiment. FIG. 3 is an explanatory diagram of the load lock mechanism of the same embodiment, (a
) is an external perspective view, (b) is an internal configuration diagram, and (C) is a seal structure diagram. FIG. 4 is a sample stage diagram, (a) is an overall diagram, and (a) is a stage diagram. FIG. 5 is a structural diagram of a mass spectrometer. Figure 6 is a diagram of the manipulator, (a) is a plan view, and (a) is a plan view.
is a longitudinal cross-sectional view. Figure 7 is a diagram (pyrogram diagram) showing an example of the analysis results.
. FIG. 8 is a system diagram according to an embodiment of the present invention. 1...Vacuum chamber, IA, IB...Metal end plate thereof, IC...Metal tube, ID, IE...Peep window, 2A...
...Magnetic levitation turbo molecular pump, 2B...Turbo molecular pump, 3A, 3B, 3C...Rotary type vacuum pump, 4...Glass rod made of transparent quartz glass, 4A
... Light receiving surface, 4B... Other end surface, 5... Sample stage, 5A... Fitting part, 5B, 5C... Hole, 6...
・Sample, 7...Infrared generator which is a heater, 7A・
...Reflecting surface, tail...Connecting pipe, 8A...Main exhaust pipe, 9.
10.11... Ionization section, excitation section, collector section of mass spectrometer, 9A... Ionization chamber, 9B...
Opening, 9C... Extraction electrode, IOA... Iron core, 12
... Load lock chamber, 12A ... its end,
13... Open/close valve, 13A... Slide valve, 14...
・Sample insertion port, 15...transport platform, 16...rack section, 16A...stopper, 17...pinion, 17A
...Pinion shaft, 18A, 18B...Knob, 18
C, 18D...knobs, which are the first and second operating ends of the manipulator, 19A, 19B, 19D, 1
9E...0 link, 19C119F...spacer,
19G... Cylindrical body, 2OA, 20B, 20C... Exhaust collar, 21... Infrared generating lamp, 21A... Thermocouple, 22A, 22B, 22C, 22D... Cock,
23...Disc, 24...Cooling water tank, 25.
... Computer unit, 26 ... Rotating shaft, 27.
... Manipulator, 27A... Sheath body, 27B...
Flange, 27C...outer shaft, 27F...inner shaft, 27
D... Bearing, 27E, 27G... First and second working end, 27H... Seat, 27J... Leaf spring, 27K...
...Claw, 27L...Spring, 28A, 28B...Bellows, 30A, 30B, 30C...Pipe, 31...
・Cooling water passage, 32A, 32B...Vacuum gauge, 33G・
...Desorption gas, 33E...Ion beam.

Claims (1)

[Claims] 1. A vacuum chamber, a vacuum pump that maintains the vacuum chamber in a vacuum, a sample stage placed in the vacuum chamber, and a heater that heats the sample placed on the sample stage. and a mass spectrometer connected to the inside of the vacuum chamber, which is housed in a space sufficiently smaller in volume than the vacuum chamber, and has an on-off valve between it and the vacuum chamber, A vacuum is maintained by a vacuum means separate from the vacuum pump, and a load lock mechanism is provided to carry and place the sample on the sample stage without destroying the vacuum state of the vacuum chamber. Released gas detection device. 2. The desorbed gas detection device according to claim 1, wherein the vacuum chamber has an inner diameter that is 5 times or more the diameter of the sample stage, and a distance from the sample stage to the inner wall surface of the vacuum chamber is 50 mm or more. 3. The desorbed gas detection device according to claim 1, wherein the vacuum chamber has a wall structure composed of a metal tube and a metal end plate, and the inner wall surfaces of the metal tube and the metal end plate are polished. 4. The desorbed gas detection device according to claim 1, wherein the load lock mechanism has a structure that allows the carrier and the moving mechanism of the carrier to retreat from the vacuum chamber. 5. The load lock mechanism includes a pinion and a rack mechanism, the pinion rotating shaft is provided with a sealing structure equipped with double O-rings, and a vacuum is provided to maintain a vacuum in the space formed between the double O-rings. 5. The desorption gas detection device according to claim 4, further comprising means. 6. The heater is an infrared generator and is disposed outside the vacuum chamber, and the sample stage includes a glass rod that introduces the infrared rays generated by the infrared generator into the vacuum chamber. The desorption gas detection device described above. 7. The desorbed gas detection device according to claim 1, wherein the vacuum pump includes a magnetically levitated turbomolecular pump. 8. The desorbed gas according to claim 1, wherein the vacuum chamber has an inner diameter of about 5 times or more and about 20 times or less of the diameter of the sample stage, and a distance from the sample stage to the ceiling of about 50 mm or more and 500 mm or less. detection device. 9. In a desorption gas detection method in which a sample is heated in a vacuum chamber and the desorption gas generated from the sample is observed using a mass spectrometer, the desorption gas is A method for detecting a desorbed gas, characterized in that the sample is taken in and taken out. 10. The method for detecting a desorbed gas according to claim 9, characterized in that when it is necessary to break the vacuum state, dry nitrogen or dry air is introduced into that part. Method.