CN206330912U - A kind of vacuum atmosphere processing unit and sample observation system - Google Patents
A kind of vacuum atmosphere processing unit and sample observation system Download PDFInfo
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- 238000012545 processing Methods 0.000 title claims abstract description 55
- 238000005086 pumping Methods 0.000 claims abstract description 153
- 238000010894 electron beam technology Methods 0.000 claims abstract description 44
- 239000000523 sample Substances 0.000 claims description 173
- 238000011282 treatment Methods 0.000 claims description 22
- 238000006073 displacement reaction Methods 0.000 claims description 11
- 238000007789 sealing Methods 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 3
- 238000012360 testing method Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 153
- 239000010408 film Substances 0.000 description 15
- 238000001514 detection method Methods 0.000 description 12
- 238000000034 method Methods 0.000 description 10
- 239000000284 extract Substances 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000010409 thin film Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- 239000012472 biological sample Substances 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 2
- 238000004891 communication Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
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Abstract
The utility model discloses a kind of vacuum atmosphere processing unit, the top of described device is connected with outside electron beam generating device, it is characterised in that described device is axially symmetric structure, and described device includes successively outside from central axial：Central passage, the first bleed-off passage, supply chamber and at least one second pumping chamber；Wherein, the exit of the central passage is provided with aperture of pressure difference, for maintaining the pressure difference of central passage and external environment, and the electron beam for producing the electron beam generating device passes through the central passage；First bleed-off passage is connected with the central passage, for being evacuated to the central passage；The supply chamber top is connected with air supply channel, for being supplied to the region between described device and testing sample；The top of the second pumping chamber is connected with the second bleed-off passage, for being evacuated to the region between described device and testing sample.The invention also discloses a kind of sample observation system.
Description
Technical Field
The utility model relates to a scanning electron microscope field especially relates to a vacuum atmosphere processing apparatus and sample observation system.
Background
The optical microscope has the advantages of simple operation, simple preparation of a sample to be measured, no strict requirement on the external environment and the like in the using process, so that the optical microscope is widely applied to the fields of scientific research, medical treatment, industrial production and the like; however, the resolution of the optical microscope is low due to the limit of the optical diffraction limit, which is about 200 nm. In order to obtain higher resolution, Scanning Electron Microscope (SEM) was invented in the 60's of the 20 th century, and the resolution of SEM can reach several nanometers and even can reach sub-nanometer level.
However, the electron microscope also has a lot of inconveniences in the application process, such as: the sample to be tested is complex to prepare, has strict requirements on the testing environment, and needs to be placed in a high-vacuum sample chamber; therefore, the sample observed by SEM usually requires treatments such as sampling, dehydration, drying, and plating. Thus, large-sized samples, aqueous samples, organic biological samples, etc. are inconvenient to observe using conventional SEM.
In order to facilitate observation of special samples such as aqueous samples and organic biological samples, a novel SEM has been derived, wherein the most typical novel SEM is Environmental Scanning Electron Microscope (ESEM); ESEMs usually have a relatively high pressure sample chamber containing an atmosphere, typically in the range of 0.1 torr to 50 torr, under which conditions the sample to be measured may be an aqueous sample such as a biological sample or a non-conductive sample not suitable for high vacuum; however, the ESEM has a closed sample space, which still has a certain difficulty in observing a sample which is large in size and difficult to divide and sample, and is inconvenient for observing a sample which needs to be measured quickly and is changed frequently.
In order to solve the disadvantages of the ESEM in observing the sample, an Atmospheric Scanning Electron Microscope (ASEM) and an environment with a certain atmosphere and adjustable pressure are proposed in succession; since the ASEM observes a sample in an open environment, the mean free path of electrons in the atmosphere is only tens to hundreds of micrometers, and thus, the working distance of the ASEM is very small. Creating an atmosphere in an open environment by injecting gas into the vicinity of the sample using one or more conduits creates a local gas environment, which has the disadvantage that the pressure of the created local gas environment is not stable and cannot be easily controlled.
Therefore, when a sample is observed by using SEM in an open environment without a sample chamber, how to create a local gas environment required for observing the sample and how to control the pressure of the local gas environment are problems to be solved.
SUMMERY OF THE UTILITY MODEL
In view of this, the embodiments of the present invention desirably provide a vacuum atmosphere processing apparatus and a sample observation system, which can create an ideal local gas environment so that an observed region of a sample is in an ideal observation environment.
The embodiment of the utility model provides a technical scheme is so realized:
an embodiment of the utility model provides a vacuum atmosphere processing apparatus, the top and the outside electron beam of device produce the device and be connected, its characterized in that, the device is the axisymmetric structure, the device outwards includes in proper order from the central axis: the central channel, a first air exhaust channel connected with an external first air exhaust system, an air supply chamber connected with the external air supply system and at least one second air exhaust chamber connected with an external second air exhaust system; wherein,
a pressure difference diaphragm is arranged at the outlet of the central channel and is used for maintaining the pressure difference between the central channel and the external environment and enabling the electron beam generated by the electron beam generating device to be emitted from the central channel and then irradiate on a sample to be measured;
the first air exhaust channel is communicated with the central channel and is used for exhausting air to the central channel;
the bottom end of the air supply chamber is provided with a first air outlet, the top end of the air supply chamber is connected with an air supply channel, and the air supply channel supplies air to the area between the device and the sample to be detected through the air supply chamber;
and a second air outlet is formed in the bottom end of the second air pumping cavity, a second air pumping channel is connected to the top end of the second air pumping cavity, and the second air pumping channel pumps air to the region between the device and the sample to be detected through the air pumping cavity.
In the above scheme, the pressure value of the central channel is less than 10-1And the length of the central channel is less than 100 mm.
In the above scheme, the shape of the channel openings at the bottom of the gas supply chamber and the bottom of the second gas pumping chamber is a hole array or a ring.
In the above scheme, the gas supplied by the device is pure gas or mixed gas.
In the above scheme, the gas supply device further comprises, between the first pumping channel and the gas supply chamber: and the top end of the third pumping cavity is connected with a third pumping channel and is used for pumping the area between the device and the sample to be tested.
The embodiment of the utility model provides a still provide a sample observation system, the system includes: a scanning electron microscope, a vacuum atmosphere treatment device and a sample; wherein,
the bottom of a lens barrel of the scanning electron microscope is fixedly connected with the top of the vacuum atmosphere processing device;
the sample is placed at a first distance from the bottom of the vacuum atmosphere treatment device;
the vacuum atmosphere treatment device is of an axisymmetric structure, and comprises the following components from a central shaft to the outside in sequence: the central channel, a first air exhaust channel connected with an external first air exhaust system, an air supply chamber connected with the external air supply system and a second air exhaust chamber connected with an external second air exhaust system;
a pressure difference diaphragm is arranged at the outlet of the central channel and is used for maintaining the pressure difference between the central channel and the external environment and enabling an electron beam generated by the scanning electron microscope to be emitted from the central channel and then irradiate on a sample to be measured;
the first air exhaust channel is communicated with the central channel and is used for exhausting air to the central channel;
the bottom end of the air supply chamber is provided with a first air outlet, the top end of the air supply chamber is connected with an air supply channel, and the air supply channel supplies air to the area between the vacuum atmosphere processing device and the sample through the air supply chamber;
and the top end of the second pumping cavity is connected with a second pumping channel, and the second pumping channel pumps air to the area between the vacuum atmosphere processing device and the sample through the pumping cavity.
In the above scheme, the bottom of the lens barrel of the scanning electron microscope is connected with the top of the vacuum atmosphere processing device through a bolt, and is sealed by a sealing device.
In the above scheme, the pressure value of the central channel is less than 10-1And the length of the central channel is less than 100 mm.
In the above scheme, the shape of the channel openings at the bottom of the gas supply chamber and the bottom of the second gas pumping chamber is a hole array or a ring.
In the above scheme, the gas supplied by the vacuum atmosphere treatment device is pure gas or mixed gas.
In the above scheme, the gas supply device further comprises, between the first pumping channel and the gas supply chamber: and the top end of the third pumping cavity is connected with a third pumping channel and is used for pumping the area between the device and the sample to be tested.
In the above solution, the system further comprises at least one detector, wherein the detector is located below the central channel and embedded at the bottom of the vacuum atmosphere treatment device, or the detector is placed inside the central channel.
In the above solution, the system further comprises a displacement stage connected to the sample for adjusting a first distance between the sample and the vacuum atmosphere treatment device.
In the above scheme, the system further comprises a height adjusting device connected to the scanning electron microscope for adjusting the height of the scanning electron microscope.
The embodiment of the utility model provides a vacuum atmosphere processing apparatus and sample observation system, the top and the outside electron beam of device produce the device and be connected, a serial communication port, the device is the axisymmetric structure, the device outwards includes in proper order from the center shaft: the central channel, a first air exhaust channel connected with an external first air exhaust system, an air supply chamber connected with the external air supply system and at least one second air exhaust chamber connected with an external second air exhaust system; the pressure difference diaphragm is arranged at the outlet of the central channel and used for maintaining the pressure difference between the central channel and the external environment and enabling the electron beam generated by the electron beam generating device to be emitted from the central channel and then irradiate on a sample to be measured; the first air exhaust channel is communicated with the central channel and is used for exhausting air to the central channel; the bottom end of the air supply chamber is provided with a first air outlet, the top end of the air supply chamber is connected with an air supply channel, and the air supply channel supplies air to the area between the device and the sample to be detected through the air supply chamber; and a second air outlet is formed in the bottom end of the second air pumping cavity, a second air pumping channel is connected to the top end of the second air pumping cavity, and the second air pumping channel pumps air to the region between the device and the sample to be detected through the air pumping cavity. Thus, the device is supplied with gas through the gas supply system, the first gas extraction system extracts gas from the central channel, and the second gas extraction system extracts gas from the region between the device and the sample to be measured, so that a local gas environment is formed in the region between the device and the sample to be measured, namely a local space region is formed between the lower surface of the device and the upper surface of the sample to be measured; and controlling the pressure of the gas near the tested area of the sample by adjusting the vacuum pumps, the pumping speeds and the like used by the first pumping system and the second pumping system; therefore, the observed area of the sample is under an ideal observation environment.
Drawings
FIG. 1 is a schematic cross-sectional view of a vacuum atmosphere processing apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of an external structure of a vacuum atmosphere processing apparatus according to an embodiment of the present invention, which is matched with a scanning electron microscope;
fig. 3 is a schematic cross-sectional view of a scanning electron microscope according to an embodiment of the present invention;
FIG. 4a is a schematic view of an end face of a structure of a vacuum atmosphere processing apparatus according to an embodiment of the present invention;
FIG. 4b is a schematic view of the shape of the channel opening of each channel according to the embodiment of the present invention;
fig. 4c is a schematic view of the shape of the channel opening of each channel according to the embodiment of the present invention;
FIG. 5 is a schematic cross-sectional view of a vacuum atmosphere processing apparatus according to an embodiment of the present invention;
FIG. 6 is a schematic cross-sectional view of the three-vacuum atmosphere processing apparatus according to the embodiment of the present invention;
fig. 7 is a schematic structural diagram of a four-sample observation system according to an embodiment of the present invention;
fig. 8 is a schematic view of a scanning electron microscope with a gantry structure according to an embodiment of the present invention;
fig. 9 is a schematic processing flow diagram of an eight-sample observation method according to an embodiment of the present invention.
Detailed Description
The invention is further illustrated by the following figures and examples.
Example one
The embodiment of the present invention provides a vacuum atmosphere processing apparatus, a cross-sectional view of a composition structure of the vacuum atmosphere processing apparatus 104 is shown in fig. 1, a top of the vacuum atmosphere processing apparatus 104 is connected with a bottom of an external electron beam generating apparatus; the vacuum atmosphere treatment device 104 has an axisymmetric structure, and can be an axisymmetric cylinder, an axisymmetric cuboid, an axisymmetric polygon and the like; thus, the device has a central axis, and the device comprises, in order from the central axis: a central channel 113, a first pumping channel 107 connected to an external first pumping system, a gas supply chamber 106 connected to an external gas supply system and at least one second pumping chamber 108 connected to an external second pumping system; wherein,
a pressure difference diaphragm 109 is arranged at the outlet of the central channel 113 by taking the central axis of the device as the center, and the electron beam generated by the electron beam generating device acts on the surface of the sample 111 after passing through the lens cone 101, the central channel 113 and the pressure difference diaphragm 109; here, the pressure difference diaphragm 109 can make the central passage 113 under a higher vacuum environment to reduce the scattering of the electron beam generated by the electron beam generating device before reaching the surface of the sample 111 to be measured.
One end of the first air exhaust channel 107 is connected with an external first air exhaust system, and the other end is communicated with the central channel 113; the first pumping system may be one or more independently operated vacuum pumps to better control the vacuum atmosphere; the first pumping system pumps air to the central channel 113 through the first pumping channel 107;
the top end of the gas supply chamber 106 is connected with a gas supply channel, one end of the gas supply channel is connected with an external gas supply system, and the gas supply system supplies gas to the gas supply chamber 106 through the gas supply channel, namely supplies gas to an area between the device and a sample; the black dots shown in fig. 1 represent air, the gray dots represent gas supplied from an external gas supply system, and the density of the dots represents the density of gas molecules or the pressure of the gas.
A second air outlet 116 is arranged at the bottom end of the second air pumping chamber 108, a second air pumping channel is connected to the top end of the second air pumping chamber, one end of the second air pumping channel is connected to an external second air pumping system, the second air pumping system can be one or more vacuum pumps working independently, and the second air pumping system pumps air to a region 114 between the device and the sample 111 to be measured through the second air pumping channel;
here, the number of the second pumping chambers 108 may be one or plural, and when the number of the second pumping chambers 108 is plural, the plural second pumping chambers 108 are sequentially distributed outside the gas supply chamber 106 with the center axis of the apparatus as the center.
In the embodiment of the utility model, the air supply system toThe gas supplied to the gas supply chamber 106 may be a pure gas or a mixed gas; wherein the purified gas comprises: he. Ar, N2、H2O、O2And the like; the mixed gas comprises: he and H2Mixed gas of O, etc.;
in a preferred embodiment, the gas supplied by the device is He, since the electron beam generated by the electron beam generating device has a larger mean free path in He than other gases; at the moment, the electron microscope can work under a larger working distance, so that the observation of a large-size sample is more convenient.
In the embodiment of the present invention, a first air outlet 115 is disposed at the bottom end of the air supply chamber 106, and the first air outlet 115 is used for supplying air to the region 114 between the device and the sample 111 to be tested; according to fig. 1, the gas entering the area 114 between the device and the sample 111 to be tested can be extracted from the first pumping channel 107 through the central channel 113 and also from the second pumping chamber 108; thus, gas flows simultaneously to the core region and the second pumping channel, wherein the core region is a region near the observed region 112 of the sample in the device; thus, the central detection area 112 is ensured to be in the set atmosphere, and the surrounding air is prevented from entering the central detection area 112; meanwhile, the air-extracting operation performed on the second air-extracting chamber 108 through the second air-extracting channel can prevent a large amount of air from entering the central detection area, and improve the observation accuracy of the sample 111.
In the embodiment of the present invention, the length of the central channel 113 is the thickness of the device 104 in the embodiment of the present invention, the length of the central channel 113 is as small as possible, and the preferred length thereof is less than 30 mm, and the more preferred length is less than 10 mm.
In the embodiment of the present invention, the preferred value of the pressure of the central channel 113 is less than 10-1Torr, more preferably less than 10-2Torr, most preferably less than 10-3And (4) supporting.
In the embodiment of the present invention, as shown in fig. 1, taking the electron beam generating device as an example of a scanning electron microscope, fig. 2 is an external structural schematic diagram of the vacuum atmosphere processing device in the embodiment of the present invention, the upper surface 105 of the vacuum atmosphere processing device 104 is matched with the lower surface of the lens barrel 101 of the scanning electron microscope, and can be fixedly connected by a bolt, and then sealed by a sealing device such as an O-ring; in this manner, the device 104 is easily installed and removed; the sample 111 in the embodiment of the present invention is basically characterized by a large size and a surface that is approximately planar; in the embodiment of the present invention, the bottom of the lens barrel 101 of the scanning electron microscope is sealed by a film to the high vacuum chamber in the lens barrel 101, the film separates the high vacuum lens barrel 101 from the laboratory environment of one atmosphere, and the film can bear the pressure difference between two sides, and allow the electron beam generated by the scanning electron microscope to pass through the film to the maximum extent; here, the material of the thin film may be a silicon nitride, silicon dioxide, graphene thin film, or the like.
In a specific embodiment, the bottom of the sem is not provided with a vacuum film, but one or more pressure difference diaphragms are used, as shown in fig. 2, a pressure difference diaphragm 203 is provided at the bottom of a barrel 201 of the sem, and the pressure difference diaphragm 203 is arranged symmetrically around an axis 202 of the barrel 201 of the sem.
The embodiment of the utility model provides a vacuum atmosphere processing apparatus's component structure end view, as shown in FIG. 4a, 413a is the entry of the electron beam that scanning electron microscope produced, and 407a is first bleed passage, and 406a is gas supply channel, and 408a is second bleed passage.
In one embodiment, the shape of the channel openings of the channels of the device at the lower surface of the device is shown in fig. 4b and 4 c; as shown in fig. 4b, the channel openings of the gas supply channel 406b and the second pumping channel 408b are circular in shape except for the electron beam outlet 409b of the central channel; as shown in FIG. 4c, the channel openings of the gas supply channel 406c and the second pumping channel 408c are shaped as an array of holes; wherein the shape of the hole includes, but is not limited to, a circle, a square, a polygon, and the like.
In the embodiment of the present invention, the gas supply system supplies gas to the device, the first gas-extracting system extracts gas from the central channel, and the second gas-extracting system extracts gas from the region between the device and the sample to be measured, so that a local gas environment is formed in the region between the device and the sample to be measured, i.e. a local space region is formed between the lower surface of the device and the upper surface of the sample to be measured; and controlling the pressure of the gas near the tested area 112 of the sample to be changed within the range from one atmosphere to a few tenths of Torr by adjusting the vacuum pumps, the air pumping speeds and the like used by the first air pumping system and the second air pumping system; therefore, the observed area of the sample is under an ideal observation environment.
Example two
The second embodiment of the present invention provides a vacuum atmosphere processing apparatus, wherein a sectional view of a composition structure of the vacuum atmosphere processing apparatus 104 is shown in fig. 5, and a top of the vacuum atmosphere processing apparatus 104 is connected to a bottom of an external scanning electron microscope; the vacuum atmosphere treatment device 104 has an axisymmetric structure, and can be an axisymmetric cylinder, an axisymmetric cuboid, an axisymmetric polygon and the like; thus, the device has a central axis, and the device comprises, in order from the central axis: a central channel 113, a first pumping channel 107 connected to an external first pumping system, a gas supply chamber 106 connected to an external gas supply system, at least one second pumping chamber 108 connected to an external second pumping system, and at least one detector 110; wherein,
a pressure difference diaphragm 109 is arranged at the outlet of the central channel 113 by taking the central shaft of the device as the center, and the electron beam generated by the scanning electron microscope acts on the surface of the sample 111 after passing through the lens cone 101, the central channel 113 and the pressure difference diaphragm 109; here, the pressure difference diaphragm 109 can make the central passage 113 under a higher vacuum environment to reduce scattering of the electron beam generated by the scanning electron microscope before reaching the surface of the sample 111 to be measured.
One end of the first air exhaust channel 107 is connected with an external first air exhaust system, and the other end is communicated with the central channel 113; the first pumping system, which may be one or more independently operated vacuum pumps, pumps the central channel 113 through the first pumping channel 107;
the top end of the air supply chamber 106 is connected with an air supply channel, one end of the air supply channel is connected with an external air supply system, and the air supply system supplies air to the air supply chamber 106 through the air supply channel, namely supplies air to the device; the black dots shown in fig. 5 represent air, the gray dots represent gas supplied from an external gas supply system, and the density of the dots represents the density of gas molecules or the pressure of the gas;
a second air outlet is arranged at the bottom end of the second air pumping chamber 108, a second air pumping channel is connected to the top end of the second air pumping chamber, one end of the second air pumping channel is connected with an external second air pumping system, the second air pumping system can be one or more vacuum pumps working independently, and the second air pumping system pumps air to an area 114 between the device and a sample 111 to be detected through the second air pumping channel;
here, the number of the second pumping chambers 108 may be one or plural, and when the number of the second pumping chambers 108 is plural, the plural second pumping chambers 108 are sequentially distributed outside the gas supply chamber 106 with the central axis of the apparatus as the center;
the detector 110 is located below the central channel 113 and embedded in the bottom of the vacuum atmosphere treatment device 104, or the detector 110 is placed inside the central channel 113.
In the embodiment of the present invention, the detector may be one or more, and may be a secondary electron detector, a back-scattered electron detector, or a gas detector.
In one embodiment, the shape of the detector 110 may be, but is not limited to, a ring shape, such as 410b shown in FIG. 4b and 410c shown in FIG. 4 c.
In one embodiment, as shown in FIG. 5, the bottom surface of the probe 110 coincides with the bottom surface of the device 110 or is embedded inside the device 104 such that the bottom surface of the probe 110 is lower than the bottom surface of the device 104; thus, the probe 110 can be prevented from being contaminated or damaged by the contact of the probe 110 with the sample 111.
In the embodiment of the present invention, the gas supplied to the gas supply chamber 106 by the gas supply system may be pure gas or mixed gas; wherein the purified gas comprises: he. Ar, N2、H2O、O2And the like; the mixed gas comprises: he and H2Mixed gas of O, etc.;
in a preferred embodiment, the gas supplied by the apparatus is He, since the electron beam generated by a scanning electron microscope has a relatively large mean free path in He, in which case the electron microscope can be operated at a large working distance.
In the embodiment of the present invention, a first air outlet 115 is disposed at the bottom end of the air supply chamber 106, and the first air outlet 115 is used for supplying air to the region 114 between the device and the sample 111 to be tested; according to fig. 5, the gas entering the area 114 between the device and the sample 111 to be tested can be extracted from the first pumping channel 107 through the central channel 113 and also from the second pumping chamber 108; thus, gas flows simultaneously to the core region and the second pumping channel, wherein the core region is a region near the observed region 112 of the sample in the device; thus, the central detection area 112 is ensured to be in the set atmosphere, and the surrounding air is prevented from entering the central detection area 112; meanwhile, the air-extracting operation performed on the second air-extracting chamber 108 through the second air-extracting channel can prevent a large amount of air from entering the central detection area, and improve the observation accuracy of the sample 111.
In the embodiment of the present invention, the length of the central channel 113 is the thickness of the device 104, the length of the central channel 113 is as small as possible, and the preferred length is less than 30 mm, and the more preferred length is less than 10 mm.
In the embodiment of the present invention, the preferred value of the pressure of the central channel 113 is less than 10-1Torr, more preferably less than 10-2Torr, most preferably less than 10-3And (4) supporting.
In the embodiment of the present invention, as shown in fig. 5, the upper surface 105 of the device 104 is matched with the lower surface of the lens barrel 101 of the scanning electron microscope, and can be fixedly connected by a bolt, and then sealed by a sealing device such as an O-ring; in this manner, the device 104 is easily installed and removed; the sample 111 in the embodiment of the present invention is basically characterized by a large size and a surface that is approximately planar; in the embodiment of the present invention, the bottom of the lens barrel 101 of the scanning electron microscope is sealed by a film to the high vacuum chamber in the lens barrel 101, the film separates the high vacuum lens barrel 101 from the laboratory environment of one atmosphere, and the film can bear the pressure difference between two sides, and allow the electron beam generated by the scanning electron microscope to pass through the film to the maximum extent; here, the material of the thin film may be a silicon nitride, silicon dioxide, graphene thin film, or the like.
In a specific embodiment, the bottom of the sem is not provided with a vacuum film, but one or more pressure difference diaphragms are used, as shown in fig. 3, a pressure difference diaphragm 203 is provided at the bottom of the tube 201 of the sem, and the pressure difference diaphragm 203 is arranged symmetrically around the axis 202 of the tube 201 of the sem.
The embodiment of the utility model provides a vacuum atmosphere processing apparatus's component structure end view, as shown in FIG. 4a, 413a is the entry of the electron beam that scanning electron microscope produced, and 407a is first bleed passage, and 406a is gas supply channel, and 408a is second bleed passage.
In one embodiment, the shape of the channel openings of the channels of the device at the lower surface of the device is shown in fig. 4b and 4 c; as shown in fig. 4b, the channel openings of the gas supply channel 406b and the second pumping channel 408b are circular in shape except for the electron beam outlet 409b of the central channel; as shown in FIG. 4c, the channel openings of the gas supply channel 406c and the second pumping channel 408c are shaped as an array of holes; wherein the shape of the hole includes, but is not limited to, a circle, a square, a polygon, and the like.
In the embodiment of the present invention, the gas supply system supplies gas to the device, the first gas-extracting system extracts gas to the central channel, and the second gas-extracting system extracts gas to the region 114 between the device and the sample to be measured, so that the region 114 between the device and the sample to be measured forms a local gas environment, i.e. a local space region is formed between the lower surface of the device and the upper surface of the sample to be measured; and controlling the pressure of the gas near the sample measured area 112 by adjusting the vacuum pumps, the pumping speeds, and the like used by the first pumping system and the second pumping system; therefore, the observed area of the sample is under an ideal observation environment.
EXAMPLE III
Based on the vacuum atmosphere treatment device according to the first embodiment and the second embodiment of the present invention, the third embodiment of the present invention further provides a vacuum atmosphere treatment device, and the schematic cross-sectional view of the vacuum atmosphere treatment device is shown in fig. 6, which is a further improvement on the basis of the first embodiment or the second embodiment of the present invention; specifically, the vacuum atmosphere processing apparatus according to the embodiment of the present invention includes a plurality of second pumping chambers 609, and one or more pumping chambers 608 are added between the first pumping channel and the gas supply chamber in the first or second embodiment.
In the embodiment of the utility model provides an in, with the utility model discloses the outside air exhaust system of bleed passage connection can be the vacuum pump of one or more autonomous working to control vacuum atmosphere better.
Because the embodiment of the utility model provides a third vacuum atmosphere processing apparatus be based on the utility model discloses the vacuum atmosphere processing apparatus that embodiment one and embodiment two recorded proposes, consequently, the utility model discloses all characteristics of the vacuum atmosphere processing apparatus that embodiment one and embodiment two recorded all are applicable to the utility model discloses the vacuum atmosphere processing apparatus that embodiment three proposed.
Example four
The embodiment of the utility model provides a fourth provides a sample observation system, the sectional view of the component structure of system, as shown in fig. 5, include: scanning electron microscope 100, vacuum atmosphere treatment device 104, and sample 111; wherein,
the top of the vacuum atmosphere processing device 104 is fixedly connected with the bottom of the scanning electron microscope 100, and the vacuum atmosphere processing device 104 has an axisymmetric structure, and can be an axisymmetric cylinder, an axisymmetric cuboid, an axisymmetric sidebody, or the like; thus, the device has a central axis, and the device comprises, in order from the central axis: a central channel 113, a first pumping channel 107 connected to an external first pumping system, a gas supply chamber 106 connected to an external gas supply system and at least one second pumping chamber 108 connected to an external second pumping system; wherein,
a pressure difference diaphragm 109 is arranged at the outlet of the central channel 113 by taking the central axis of the device as the center, and the electron beam generated by the electron beam generating device acts on the surface of the sample 111 after passing through the lens cone 101, the central channel 113 and the pressure difference diaphragm 109; here, the pressure difference diaphragm 109 can make the central passage 113 under a higher vacuum environment to reduce the scattering of the electron beam generated by the electron beam generating device before reaching the surface of the sample 111 to be measured.
One end of the first air exhaust channel 107 is connected with an external first air exhaust system, and the other end is communicated with the central channel 113; the first pumping system may be one or more independently operated vacuum pumps to better control the vacuum atmosphere; the first pumping system pumps air to the central channel 113 through the first pumping channel 107;
the top end of the gas supply chamber 106 is connected with a gas supply channel, one end of the gas supply channel is connected with an external gas supply system, and the gas supply system supplies gas to the gas supply chamber 106 through the gas supply channel, namely supplies gas to an area between the device and the sample; the black dots shown in fig. 7 represent air, the gray dots represent gas supplied from an external gas supply system, and the density of the dots represents the density of gas molecules or the pressure of the gas.
A second air outlet is arranged at the bottom end of the second air pumping chamber 108, a second air pumping channel is connected to the top end of the second air pumping chamber 108, one end of the second air pumping channel is connected with an external second air pumping system, the second air pumping system can be one or more vacuum pumps working independently, and the second air pumping system pumps air to a region 114 between the device and a sample 111 to be detected through the second air pumping channel;
here, the number of the second pumping chambers 108 may be one or plural, and when the number of the second pumping chambers 108 is plural, the plural second pumping chambers 108 are sequentially distributed outside the gas supply chamber 106 with the center axis of the apparatus as the center.
In the embodiment of the present invention, the gas supplied to the gas supply chamber 106 by the gas supply system may be pure gas or mixed gas; wherein the purified gas comprises: he. Ar, N2、H2O、O2And the like; the mixed gas comprises: he and H2Mixed gas of O, etc.;
in a preferred embodiment, the gas fed by said means is He, since the mean free path of the electron beam generated by the electron beam generating means varies between 100 μm and 5mm in He; at the moment, the electron microscope can work under a larger working distance, so that the observation of a large-size sample is more convenient.
In the embodiment of the present invention, the bottom end of the air supply chamber 106 is provided with an air outlet 115, and the air outlet 115 is used for supplying air to the area 114 between the device and the sample 111 to be tested; according to fig. 1, the gas entering the area 114 between the device and the sample 111 to be tested can be extracted from the first pumping channel 107 through the central channel 113 and also from the second pumping chamber 108; thus, gas flows simultaneously to the core region and the second pumping channel, wherein the core region is a region near the observed region 112 of the sample in the device; thus, the central detection area 112 is ensured to be in the set atmosphere, and the surrounding air is prevented from entering the central detection area 112; meanwhile, the air-extracting operation performed by the second air-extracting chamber 108 can prevent a large amount of air from entering the central detection area, and improve the observation accuracy of the sample 111.
In the embodiment of the present invention, the length of the central channel 113 is the thickness of the device 104 in the embodiment of the present invention, the length of the central channel 113 is as small as possible, and the preferred length thereof is less than 30 mm, and the more preferred length is less than 10 mm.
In the embodiment of the present invention, the preferred value of the pressure of the central channel 113 is less than 10-1Torr, more preferably less than 10-2Torr, most preferably less than 10-3And (4) supporting.
In the embodiment of the present invention, as shown in fig. 7, taking the electron beam generating device as an example of a scanning electron microscope, the upper surface 105 of the vacuum atmosphere processing device 104 is matched with the lower surface of the lens barrel 101 of the scanning electron microscope, and can be fixedly connected by a bolt, and then sealed by a sealing device such as an O-ring; in this manner, the device 104 is easily installed and removed; the sample 111 in the embodiment of the present invention is basically characterized by a large size and a surface that is approximately planar; in the embodiment of the present invention, the bottom of the lens barrel 101 of the scanning electron microscope is sealed by a film to the high vacuum chamber in the lens barrel 101, the film separates the high vacuum lens barrel 101 from the laboratory environment of one atmosphere, and the film can bear the pressure difference between two sides, and allow the electron beam generated by the scanning electron microscope to pass through the film to the maximum extent; here, the material of the thin film may be a silicon nitride, silicon dioxide, graphene thin film, or the like.
In a specific embodiment, the bottom of the sem is not provided with a vacuum film, but one or more pressure difference diaphragms are used, as shown in fig. 3, a pressure difference diaphragm 203 is provided at the bottom of the tube 201 of the sem, and the pressure difference diaphragm 203 is arranged symmetrically around the axis 202 of the tube 201 of the sem.
The embodiment of the utility model provides a vacuum atmosphere processing apparatus's component structure end view, as shown in FIG. 4a, 413a is the entry of the electron beam that scanning electron microscope produced, and 407a is first bleed passage, and 406a is gas supply channel, and 408a is second bleed passage.
In one embodiment, the shape of the channel openings of the channels of the device at the lower surface of the device is shown in fig. 4b and 4 c; as shown in fig. 4b, the channel openings of the gas supply channel 406b and the second pumping channel 408b are circular in shape except for the electron beam outlet 409b of the central channel; as shown in FIG. 4c, the channel openings of the gas supply channel 406c and the second pumping channel 408c are shaped as an array of holes; wherein the shape of the hole includes, but is not limited to, a circle, a square, a polygon, and the like.
In the embodiment of the present invention, the gas supply system supplies gas to the device, the first gas-extracting system extracts gas from the central channel, and the second gas-extracting system extracts gas from the region between the device and the sample to be measured, so that a local gas environment is formed in the region between the device and the sample to be measured, i.e. a local space region is formed between the lower surface of the device and the upper surface of the sample to be measured; and controlling the pressure of the gas near the tested area 112 of the sample to be changed within the range from one atmosphere to a few tenths of Torr by adjusting the vacuum pumps, the air pumping speeds and the like used by the first air pumping system and the second air pumping system; therefore, the observed area of the sample is under an ideal observation environment.
EXAMPLE five
Based on the sample observation system provided by the fourth embodiment of the present invention, the fifth embodiment of the present invention further provides a sample observation system, wherein at least one detector 110 is added on the basis of the sample observation system shown in fig. 7; wherein the detector 110 is located below the central channel 113 and embedded in the bottom of the vacuum atmosphere processing device 104, or the detector 110 is located inside the central channel 113.
In the embodiment of the present invention, the detector may be one or more, and may be a secondary electron detector, a back-scattered electron detector, or a gas detector.
In one embodiment, the shape of the detector 110 may be, but is not limited to, a ring shape, such as 410b shown in FIG. 4b and 410c shown in FIG. 4 c.
In one embodiment, as shown in FIG. 5, the bottom surface of the probe 110 coincides with the bottom surface of the device 110 or is embedded inside the device 104 such that the bottom surface of the probe 110 is lower than the bottom surface of the device 104; thus, the probe 110 can be prevented from being contaminated or damaged by the contact of the probe 110 with the sample 111.
In the embodiment of the utility model provides an in, with the utility model discloses the outside air exhaust system of bleed passage connection can be the vacuum pump of one or more autonomous working to control vacuum atmosphere better.
Because the embodiment of the utility model provides a five sample observation system be based on the utility model discloses the sample observation system of four records provides, consequently, the utility model discloses all characteristics of the sample observation system of four records all are applicable to the utility model provides a five sample observation systems that provide.
EXAMPLE six
Based on the sample observation systems provided by the fourth embodiment and the fifth embodiment of the present invention, the sixth embodiment of the present invention further provides a sample observation system, wherein an air-extracting channel is added on the basis of the sample observation system provided by the fourth embodiment or the fifth embodiment; the embodiment of the utility model provides a six each passageway cross-section of sample observation system can refer to figure 6, include: an evacuation channel 607 communicating with the central channel 613 for evacuating said central channel; pumping channels 608 and 609 connected to an external pumping system for pumping the area between the device and the sample to be tested; and a gas supply chamber 606 connected to the external gas supply passage 605.
Because the embodiment of the utility model provides a six sample observation system be based on the utility model discloses the sample observation system of four or five records in embodiment proposes, consequently, the utility model discloses all characteristics of the sample observation system of six records in embodiment all are applicable to the utility model provides a sample observation system that four or five records in embodiment proposed.
EXAMPLE seven
Based on the sample observation systems provided by the fourth embodiment, the fifth embodiment and the sixth embodiment of the present invention, a seventh embodiment of the present invention further provides a sample observation system, wherein the sample observation system further comprises a displacement table connected with the sample and/or a height adjustment device connected with the scanning electron microscope; wherein the displacement stage is used for adjusting a first distance between the sample and the vacuum atmosphere processing device, and the height adjusting device is used for adjusting the height of the scanning electron microscope; the displacement table is a displacement adjusting device which can randomly adjust the distance between the sample and the vacuum atmosphere processing device.
In the embodiment of the present invention, the height adjusting device may be a gantry structure or a mechanical arm, and the height of the scanning electron microscope can be adjusted by the gantry structure or the mechanical arm, so as to adjust the working distance of the scanning electron microscope; fig. 8 shows a schematic view of a scanning electron microscope with a gantry structure, where 801 is a scanning electron microscope, 802 is a gantry structure, and 803 is a sample.
In the embodiment of the utility model provides an in, through adjusting the displacement platform of being connected with the sample, and/or through adjusting scanning electron microscope's working distance is adjusted to high adjusting device.
Because the embodiment of the utility model provides a seventh sample observation system be based on the utility model discloses the sample observation system of four, five or six records in embodiment proposes, consequently, the utility model discloses all characteristics of the sample observation system of seven records all are applicable to the utility model provides a four, five or six sample observation systems that propose in embodiment.
Example eight
Based on the utility model discloses above-mentioned vacuum atmosphere processing apparatus and sample observation system of embodiment, the embodiment of the utility model provides an eight provides a sample observation method, sample observation method is applied to the utility model provides an arbitrary sample observation system of four to embodiment seven, the processing procedure of sample observation method, as shown in fig. 9, including following step:
101, forming a local gas environment in a region between the vacuum atmosphere processing device and the sample through a first pumping channel, a gas supply chamber and at least one second pumping chamber, and controlling the pressure of the region between the vacuum atmosphere processing device and the sample;
specifically, the first air pumping system pumps air to the central channel through the first air pumping channel, the air supply system supplies air to the vacuum atmosphere processing device through an air supply channel connected to the top end of the air supply chamber, and the second air pumping system pumps air to the region between the vacuum atmosphere processing device and the sample through the at least one second air pumping chamber, so as to form a local gas environment in the region between the vacuum atmosphere processing device and the sample; and controlling the pressure of the gas near the tested area of the sample by adjusting the vacuum pumps, the air pumping speeds and the like used by the first air pumping system and the second air pumping system.
Here, the air-extracting system may be one or more vacuum pumps working independently, and thus, the air-extracting system may be a one-stage air-extracting system or a multi-stage air-extracting system; the gas supplied by the gas supply system can be pure gas or mixed gas; wherein the purified gas comprises: he. Ar, N2、H2O、O2And the like; the mixed gas comprises: he and H2And mixed gas of O, etc.
In a preferred embodiment, the second pumping chamber may be one or a plurality of second pumping chambers, and when the second pumping chambers are a plurality of second pumping chambers, the plurality of second pumping chambers are sequentially distributed outside the gas supply chamber with the central axis of the apparatus as the center.
In a preferred embodiment, the gas supplied by the apparatus is He, since the electron beam generated by a scanning electron microscope has a relatively large mean free path in He, in which case the electron microscope can be operated at a large working distance.
According to the embodiment of the present invention, the gas pumping system and the gas supply system enable gas to flow to the core area and the second pumping chamber simultaneously, wherein the core area is an area near the observed area of the sample in the device; therefore, the central detection area is ensured to be in the set atmosphere, and surrounding air is prevented from entering the central detection area; meanwhile, the air exhaust operation executed by the second air exhaust channel can prevent a large amount of air from entering the central detection area, and the observation precision of the sample is improved.
And 102, enabling the electron beam generated by the scanning electron microscope to act on the sample in the local gas environment through a pressure difference diaphragm at the outlet of the central channel so as to observe the sample.
In a preferred embodiment, the first pumping channel of the vacuum atmosphere processing apparatus and the gas supply chamber further comprise: the top end of the third pumping cavity is connected with a third pumping channel; accordingly, when performing step 101, the method further comprises:
101', the third pumping system pumps the region between the vacuum atmosphere processing device and the sample through the third pumping channel.
In a preferred embodiment, the sample observation system further comprises at least one detector located below the central channel and embedded in the bottom of the vacuum atmosphere processing apparatus, or at least one detector placed inside the central channel; correspondingly, the method further comprises the following steps:
103, detecting a signal generated after the electron beam acts on the sample by using the detector to obtain a scanning electron microscope image;
here, the detector may be one or more, and may be a secondary electron detector, a backscattered electron detector, or a gas detector; the shape of the detector may be, but is not limited to, a ring, as shown in FIG. 4b at 310b and FIG. 4c at 310 c; as shown in fig. 5, the bottom surface of the probe 110 coincides with the bottom surface of the device 110 or is embedded inside the device 104, such that the bottom surface of the probe 110 is lower than the bottom surface of the device 104; thus, the probe 110 can be prevented from being contaminated or damaged by the contact of the probe 110 with the sample 111. In a preferred embodiment, the sample observation system further comprises a displacement stage connected to the sample, and/or a height adjustment device connected to the scanning electron microscope; correspondingly, the method further comprises the following steps:
step 104, further adjusting parameters of the sample observation system to obtain an ideal scanning electron microscope image;
in particular, the first distance between the sample and the device is further adjusted, and/or the pumping rate of the gas supply system and the pumping system is adjusted, and/or the kind of the supplied gas is adjusted according to the quality of the scanning electron microscope image; until obtaining the ideal scanning electron microscope image;
here, the first distance between the sample and the vacuum atmosphere treatment device is adjusted by a displacement stage, and/or the height of the scanning electron microscope is adjusted by a height adjustment device;
wherein the displacement stage is used for adjusting a first distance between the sample and the vacuum atmosphere processing device, and the height adjusting device is used for adjusting the height of the scanning electron microscope; the height adjusting device can be a gantry structure or a mechanical arm, and the height of the scanning electron microscope can be adjusted through the gantry structure or the mechanical arm so as to adjust the working distance of the scanning electron microscope; fig. 8 shows a schematic view of a scanning electron microscope with a gantry structure, where 801 is a scanning electron microscope, 802 is a gantry structure, and 803 is a sample.
In the embodiment of the utility model provides an in, through adjusting the displacement platform of being connected with the sample, and/or through adjusting scanning electron microscope's working distance is adjusted to high adjusting device.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention.
Claims (14)
1. A vacuum atmosphere processing apparatus, the top of the apparatus being connected to an external electron beam generating means, wherein the apparatus is of an axisymmetric configuration, the apparatus comprising, in order from a central axis: the central channel, a first air exhaust channel connected with an external first air exhaust system, an air supply chamber connected with the external air supply system and at least one second air exhaust chamber connected with an external second air exhaust system; wherein,
a pressure difference diaphragm is arranged at the outlet of the central channel and is used for maintaining the pressure difference between the central channel and the external environment and enabling the electron beam generated by the electron beam generating device to be emitted from the central channel and then irradiate on a sample to be measured;
the first air exhaust channel is communicated with the central channel and is used for exhausting air to the central channel;
the bottom end of the air supply chamber is provided with a first air outlet, the top end of the air supply chamber is connected with an air supply channel, and the air supply channel supplies air to the area between the device and the sample to be detected through the air supply chamber;
and a second air outlet is formed in the bottom end of the second air pumping cavity, a second air pumping channel is connected to the top end of the second air pumping cavity, and the second air pumping channel pumps air to the region between the device and the sample to be detected through the air pumping cavity.
2. The apparatus of claim 1, wherein the pressure value of the central passage is less than 10-1And the length of the central channel is less than 100 mm.
3. The device according to claim 1 or 2, wherein the passage openings at the bottom of the gas supply chamber and the bottom of the second gas pumping chamber are in the shape of an array of holes or a ring.
4. The device according to claim 1 or 2, wherein the gas fed by the device is a pure gas or a mixed gas.
5. The apparatus of claim 1 or 2, further comprising, between the first pumping channel and the gas supply chamber: and the top end of the third pumping cavity is connected with a third pumping channel and is used for pumping the area between the device and the sample to be tested.
6. A sample observation system, the system comprising: a scanning electron microscope, a vacuum atmosphere treatment device and a sample; wherein,
the bottom of a lens barrel of the scanning electron microscope is fixedly connected with the top of the vacuum atmosphere processing device;
the sample is placed at a first distance from the bottom of the vacuum atmosphere treatment device;
the vacuum atmosphere treatment device is of an axisymmetric structure, and comprises the following components from a central shaft to the outside in sequence: the central channel, a first air exhaust channel connected with an external first air exhaust system, an air supply chamber connected with the external air supply system and a second air exhaust chamber connected with an external second air exhaust system;
a pressure difference diaphragm is arranged at the outlet of the central channel and is used for maintaining the pressure difference between the central channel and the external environment and enabling an electron beam generated by the scanning electron microscope to be emitted from the central channel and then irradiate on a sample to be measured;
the first air exhaust channel is communicated with the central channel and is used for exhausting air to the central channel;
the bottom end of the air supply chamber is provided with a first air outlet, the top end of the air supply chamber is connected with an air supply channel, and the air supply channel supplies air to the area between the vacuum atmosphere processing device and the sample through the air supply chamber;
and the top end of the second pumping cavity is connected with a second pumping channel, and the second pumping channel pumps air to the area between the vacuum atmosphere processing device and the sample through the pumping cavity.
7. The system according to claim 6, wherein the bottom of the lens barrel of the scanning electron microscope is connected with the top of the vacuum atmosphere processing device through a bolt, and is sealed by a sealing device.
8. System according to claim 6 or 7, characterized in that the pressure value of the central channel is less than 10-1And the length of the central channel is less than 100 mm.
9. A system according to claim 6 or 7, wherein the passage openings at the bottom of the gas supply chamber and the bottom of the second gas extraction chamber are in the shape of an array of holes or a ring.
10. The system according to claim 6 or 7, wherein the gas supplied by the vacuum atmosphere treatment device is a pure gas or a mixed gas.
11. The system of claim 6 or 7, further comprising, between the first pumping channel and the gas supply chamber: and the top end of the third pumping cavity is connected with a third pumping channel and is used for pumping the area between the device and the sample to be tested.
12. The system according to claim 6 or 7, characterized in that it further comprises at least one probe, which is positioned below the central channel and is embedded in the bottom of the vacuum atmosphere treatment device, or which is placed inside the central channel.
13. The system according to claim 6 or 7, further comprising a displacement stage connected to the sample for adjusting a first distance between the sample and the vacuum atmosphere processing device.
14. The system of claim 6 or 7, further comprising a height adjustment device coupled to the scanning electron microscope for adjusting a height of the scanning electron microscope.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201621260039.8U CN206330912U (en) | 2016-11-23 | 2016-11-23 | A kind of vacuum atmosphere processing unit and sample observation system |
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| CN201621260039.8U CN206330912U (en) | 2016-11-23 | 2016-11-23 | A kind of vacuum atmosphere processing unit and sample observation system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106680305A (en) * | 2016-11-23 | 2017-05-17 | 聚束科技（北京）有限公司 | Vacuum atmosphere processing device as well as sample observing system and sample observing method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106680305A (en) * | 2016-11-23 | 2017-05-17 | 聚束科技（北京）有限公司 | Vacuum atmosphere processing device as well as sample observing system and sample observing method |
| CN106680305B (en) * | 2016-11-23 | 2023-08-04 | 聚束科技（北京）有限公司 | Vacuum atmosphere treatment device, sample observation system and method |
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