CN101067992A - Apparatus for operating gas and providing for observing under vacuum or low-voltage environment - Google Patents
Apparatus for operating gas and providing for observing under vacuum or low-voltage environment Download PDFInfo
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- CN101067992A CN101067992A CN 200610075899 CN200610075899A CN101067992A CN 101067992 A CN101067992 A CN 101067992A CN 200610075899 CN200610075899 CN 200610075899 CN 200610075899 A CN200610075899 A CN 200610075899A CN 101067992 A CN101067992 A CN 101067992A
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Abstract
This invention relates to a device for operating gas at vacuum or low gas pressure for observation including: a shell with a flat part formed at one side and at least one clapboard in it to divide it into a gas chamber and a buffer chamber, in which, the clapboard of the top underside of the gas chamber is set with an internal hole, an outer hole is set at the top and bottom of the shell separately, the internal hole and the outer hole are coaxial and placed at the flat part, said shell has a pumping hole connected to the buffer chamber and a gas injecting hole connected to the gas chamber.
Description
Technical field
The present invention be with vacuum or environment under low pressure in the operation gaseous material technology relevant, be meant especially a kind of in vacuum or environment under low pressure operating gas and can for observation device.
Background technology
On the observation technology under the micro-scale, be to reach the effect that high magnification amplifies known at present with electron microscope, amplify by ultra-high magnifications by electron microscope, people are by to carry out the related science research of material nanostructure.
The principle of electron microscope is to utilize electron beam to survey object, it must see through the high voltage accelerated electron and utilize the electromagnetic lens method of focusing to reach observation on the nanostructure at vacuum environment following, as shown in figure 20, electron microscope 61 has a sample room 62 (specimen chamber) and can insert for sample, be to be vacuum in this sample room 62, and have in this sample room 62 utmost point piece 66 on (pole piece) and once utmost point piece 66 (polepiece) guarantee electron beam focusing precisely, the distance that this two utmost points piece is 66 is no more than one centimeter usually, the sample of desiring to insert is necessary for solid and could observes under this kind vacuum environment, sample can not be the flowing material of the class of liquid state or gaseous state, otherwise has boiling immediately, volatilization, problems such as loss.
In order to solve foregoing problems, and can make the sample of inserting in the electron microscope can be under the environment that certain gas exists, people such as Hui S W proposed a kind of environmental chamber (Hui S W et al. of may command steam in 1976, Journal of Physics E 9,69,1976), extremely shown in Figure 22 as Figure 21, this kind technology mainly is that sample room 72 repackings of electron microscope 71 are increased, and one water tank 74 is set in these 72 inside, sample room, an and environmental chamber 76, separate with two dividing plates 762 these environmental chamber 76 inside, and form an aqueous vapor layer 764 in central authorities, and form a resilient coating 766 up and down respectively in this aqueous vapor layer 764, the tracheae 741 that this water tank 74 has a controllable temperature is connected in this aqueous vapor layer 764, in order to provide with environmental chamber 76 synthermal steam to this aqueous vapor layer 764, in order to avoid producing when entering aqueous vapor layer 764, steam condenses, lower wall surface is parallel and a perforation 763 is set respectively on this two dividing plate 762 and this environmental chamber 76, this perforation 763 is that the coaxial electron beam that supplies passes, aqueous vapor layer 764 1 side in the middle of this environmental chamber 76 are the sample cells 767 that stretches out, one sample tool 768 stretches to aqueous vapor layer 764 in this environmental chamber 76 by the outside through this sample cell 767, and seal in the wall of this sample tool 768 with O shape ring (769) with this aqueous vapor layer 764, by with aqueous vapor layer 764 with outside isolated.
When operation, steam in this water tank 74 is to keep flowing in this aqueous vapor layer 764, simultaneously this two resilient coating 766 is bled,, avoid steam to flow out these environmental chamber 76 outsides via the perforation 763 of outside from this two resilient coating 766 by extracting out from the steam that these aqueous vapor layer 764 dissipations are come out.By planting technology thus, can keep the pressure of gas about 50torr (holder ear) at the aqueous vapor layer in this environmental chamber 76 764.
Though aforesaid technology can form the steam of utmost point low-pressure at the aqueous vapor layer, yet it has the many places disappearance to have much room for improvement:
One, it must change the original design of electron microscope, and necessary dismounting electron microscope, and not only process is very complicated, must the professional person just can accomplish, its cost is also very expensive, and damages electron microscope again easily, also therefore makes that this technology so far can't volume production.
Two, increase the sample room height of electron microscope, can cause the change of electron beam focusing distance, thereby cause the loss that differs with resolution.
Three, increase gas pressure in the air chamber, can cause gas outermost perforation 763 spill and leakages from Figure 22 thereby can't carry out operation under the normal pressure in air chamber inside to the region of no pressure; Though greatly the exhaust capacity of width of cloth increase surge chamber 766 can overcome this gas spill and leakage problem, but gas is extracted speed out and can be caused gas to produce serious eddy current near inner perforated 763 holes apace, causes electronics multiple scattering problem and causes electron beam imaging or carry out the experiment of electron diffraction smoothly.
Be engaged in associated electrical microscope repacking work in addition in the recent period and be Gai P.L. leader's research group, observed experiment (GaiP.L., the Microscopy﹠amp of gas, solid state reaction under the displaying electron microscope in 2002; Microanalysis 8,21, and 2002).Its design is little with Hui difference, but its shortcoming is that the space between whole pole pieces in the microscope (the 1cm size is arranged usually approximately) served as the air chamber district.So as long as gas pressure continues to increase in the air chamber district, electronics will become quite serious because of the multiple scattering effect that the bump gas molecule produces.So for the design of this 1cm air chamber thickness, operating pressure will cause electronics multiple scattering problem and causes electron beam imaging or carry out the experiment of electron diffraction smoothly up to 1 atmospheric gas in this air chamber.
In addition, the design of Gai P.L. is still identical with Hui S W design idea, air chamber district, buffering area with whole be that microscopical main body must be decomposed in the retrofit process of system could be with these parts installations, so the possibility of volume production is not high.
The work of being correlated with the same period is such as Lee T.C. (Lee T.C.et al., Rev.Sci.Instrum.62,1438,1991), Robertson I.M. (Robertson I.M.et al., Microscopy Research﹠amp; Technique 42,260, and 1998) and SharmaR. (Sharma R., Microscopy﹠amp; Microanalysis 7,494,2001) etc., the design of these designs and Gai P.L. much at one, so when all facing air chamber and operating under an atmospheric pressure condition, electron beam can't imaging because of electronics multiple scattering problem or is carried out the experiment of electron diffraction.
In addition, people's such as Hui technology is that the entire environment device is fixed on microscope inside, therefore will make electron beam can seem very difficult and extremely difficulty operation by the coaxial perforation of this environmental device when mounted.And people's such as Gai technology also faces the aligning difficulty of two utmost point pieces 66 up and down simultaneously.Again,, therefore can't adjust the entire environment height of devices because the Environment Design of Hui is fixed design (being fixed in the utmost point piece of below), and the interval chance of accurately focusing that joins that loses and focus.Because above-mentioned many shortcomings, this case inventor is through after constantly studying and testing, we overcome above difficulty finally, and the electron beam that can make electron microscope easily passes through our designed device, and the device that can make us is positioned at the focusing interval of electron microscope, makes in the focusing work more convenient.
Summary of the invention
Main purpose of the present invention be to provide a kind of in vacuum or environment under low pressure operating gas and can be for the device of observation, it can provide the environment to gas observation under the prerequisite that does not change the original design of electron microscope.
A time purpose of the present invention be to provide a kind of in vacuum or environment under low pressure operating gas and can be for the device of observation, it can be than prior art control gaseous pneumatic parameter and the operation that reaches higher pressure more easily.
A further object of the present invention be to provide a kind of in vacuum or environment under low pressure operating gas and can be for the device of observation, it can not influence the resolution of electron microscope.
Another object of the present invention is to provide a kind of in vacuum or environment under low pressure operating gas and can be for the device of observation, it is simple to operate, assembling easily.
Edge is, in order to reach aforementioned purpose, provided by the present invention a kind of in vacuum or environment under low pressure operating gas and can for observation device, include: a housing, one side forms a more flat portion, this enclosure interior has at least one dividing plate, and this enclosure interior is separated to form an air chamber, and at least one surge chamber of the outside formation of this air chamber, the dividing plate of the bottom surface, top of this air chamber is respectively equipped with an endoporus, and the end face of this housing and bottom surface respectively be provided with an outer hole, and this endoporus is with should outer hole coaxial and be positioned at this more flat portion, this housing has an aspirating hole and is communicated in this surge chamber, and has an injecting hole and be communicated in this air chamber.By this, can be under the structure that does not change electron microscope, reaching provides the observing environment with gas, has effects such as easy to assembly, processing ease simultaneously again.
Description of drawings
Fig. 1 is the stereoscopic figure of the present invention's first preferred embodiment;
Fig. 2 is the cross-sectional schematic of the present invention's first preferred embodiment;
Fig. 3 is the enforcement state diagram of the present invention's first preferred embodiment;
Fig. 4 is another enforcement state diagram of the present invention's first preferred embodiment;
Fig. 5 is the cross-sectional schematic of the present invention's second preferred embodiment;
Fig. 6 is the cross-sectional schematic of the present invention's the 3rd preferred embodiment;
The 7th figure is the stereoscopic figure of the present invention's the 3rd preferred embodiment;
Fig. 8 is the horizontal cross-sectional schematic of the present invention's the 3rd preferred embodiment, shows the internal state when overlooking;
Fig. 9 is the cross-sectional schematic of the present invention's the 4th preferred embodiment;
Figure 10 is the partial enlarged drawing of Fig. 9;
Figure 11 is the cross-sectional schematic of the present invention's the 5th preferred embodiment, shows the state that is equipped with in electron microscope simultaneously;
Figure 12 is the exploded cross-sectional schematic of the present invention's the 6th preferred embodiment;
Figure 13 is the assembled sectional view of the present invention's the 6th preferred embodiment;
Figure 14 is the local member schematic diagram of the present invention's the 7th preferred embodiment, shows shell structure;
Figure 15 is the assembled sectional view of the present invention's the 7th preferred embodiment;
Figure 16 is the assembled sectional view of the present invention's the 8th preferred embodiment;
Figure 17 is the assembled sectional view of the present invention's the 9th preferred embodiment;
Figure 18 is the cross-sectional schematic of the present invention's the tenth preferred embodiment;
Figure 19 is the cross-sectional schematic of the present invention's the 11 preferred embodiment.Figure 20 is the sample room schematic internal view of existing electron microscope;
Figure 21 is in the prior art, and environmental chamber is arranged at the view of the electron microscope after the repacking;
Figure 22 is the cross-sectional schematic of existing environmental chamber.
[primary clustering symbol description]
10 in vacuum or environment under low pressure operating gas and can for observation device
11 housings, 112 outer holes, 114 glove holes
12 more flat 14 dividing plates of 116 aspirating holes
142 endoporus, 16 air chambers, 166 injecting holes
18 surge chambers, 21 liquid air-capacitor devices, 22 tracheaes
24 outer tubes, 31 sample tools, 32 articles holding tables
34 openings, 36 seals, 41 air extractors
50 in vacuum or environment under low pressure operating gas and can for observation device
11 ' housing, 112 ' outer hole, 116 ', 117 ' aspirating hole
14 ' dividing plate, 142 ' endoporus, 144 ' cushion hole
16 ' air chamber, 18 ' surge chamber
181 ' the upper and lower outer surge chamber
60 in vacuum or environment under low pressure operating gas and can for observation device
11 " housing 112 " outer hole 116 " aspirating hole
142 " endoporus 16 " air chamber 18 " surge chamber
19 inclined clapboards, 192 sub-surge chamber 196 cushion holes
80 in vacuum or environment under low pressure operating gas and can for observation device
81 housings, 811 outer holes, 812 glove holes
813 aspirating holes, 814 aspirating holes, 82 more flat portions
821 surge chambers, 822 outer surge chamber 83 dividing plates
831 cushion holes, 85 sample tools, 851 air injection pipe
852 walls, 853 injecting holes, 86 gas boxes
861 openings, 862 stickers, 863 air chambers
864 endoporus, 87 articles holding tables
The hole is inserted in 91 electron microscopes, 92 sample rooms 94
96 utmost point pieces, 99 samples
A10 in vacuum or environment under low pressure operating gas and can for observation device
The outer hole of a11 housing a12 surge chamber a14
A16 aspirating hole a21 dividing plate a22 air chamber
A24 endoporus a26 injecting hole
The a28 pressure adjusting mechanism
B10 in vacuum or environment under low pressure operating gas and can for observation device
B11 housing b21 dividing plate b22 air chamber
B25 sample tool b29 seal
C10 in vacuum or environment under low pressure operating gas and can for observation device
C11 housing c111 inserting hole c12 surge chamber
Surge chamber in the outer hole c17 dividing plate c18 of c14
C181 aspirating hole c182 gas flow c19 cushion hole
C21 dividing plate c22 air chamber c24 endoporus
C25 sample tool
D10 in vacuum or environment under low pressure operating gas and can for observation device
D11 housing d21 dividing plate d22 air chamber
D24 endoporus d25 sample tool d27 dividing plate
Surge chamber d29 cushion hole in the d28
E10 in vacuum or environment under low pressure operating gas and can for observation device
The outer hole of e11 housing e12 surge chamber e14
E21 dividing plate e22 air chamber e24 endoporus
Surge chamber e29 cushion hole in the e25 sample tool e28
F10 in vacuum or environment under low pressure operating gas and can for observation device
F12 surge chamber f22 air chamber f24 endoporus
The f28 pressure adjusting mechanism
G10 in vacuum or environment under low pressure operating gas and can for observation device
The outer hole of g12 surge chamber g14 g24 endoporus
The g28 pressure adjusting mechanism
The axis that the G electron beam passes through
Ra focuses interval
Embodiment
In order to describe structure of the present invention and characteristics place in detail, lift 11 following preferred embodiments now and cooperate graphic explanation as after, wherein:
As Fig. 1 to shown in Figure 2, the present invention's first preferred embodiment is provided a kind of in vacuum or environment under low pressure operating gas and can consisting predominantly of for the device 10 of observation:
One housing 11, one side forms one more flat 12, this thickness of more flat 12 is approximately less than the distance of 96 of two utmost point pieces up and down in the sample room 92 (being shown in Fig. 3) (specimen chamber) of electron microscope 91, usually this distance is no more than one centimeter, these housing 11 inside have some dividing plates 14, and these housing 11 inside are separated to form an air chamber 16, and form a surge chamber 18 respectively in these air chamber 16 outside upper and lowers, the dividing plate 14 of this bottom surface, air chamber 16 top is respectively equipped with an endoporus 142, and the end face of this housing 11 and bottom surface respectively are provided with an outer hole 112, this endoporus 142 with should be outer hole 112 coaxial and be positioned at this more flat 12, the aperture of this endoporus 142 is to be 10-200um, the aperture of being somebody's turn to do outer hole 112 is to be 20-800um, the aperture of this endoporus 142 is 100um in the present embodiment, the aperture of being somebody's turn to do outer hole 112 is 200um, the aperture of this endoporus 142 is less than the aperture in this outer hole 112, this housing 11 has a glove hole 114 corresponding to this air chamber 16, and make this air chamber 16 be communicated in this housing 11 outsides, and this housing 11 has two aspirating holes 116 and is communicated in respectively this surge chamber 18 respectively, and has an injecting hole 166 and be communicated in this air chamber 16;
The liquid air-capacitor device 21 of one controllable temperature, be positioned at this surge chamber 18 of this housing 11, the tracheae 22 that this liquid air-capacitor device 21 has a controllable temperature is connected in this injecting hole 166, in order to these liquid air-capacitor device 21 interior gases with air chamber 16 uniform temps are provided to this air chamber 16, this gas is to be nitrogen optionally, oxygen, helium, carbon dioxide or other gas or be the mist of the steam of liquid in aforementioned single or several mists and this liquid air-capacitor device 21, this tracheae 22 stretches into the last fragment position that this liquid air-capacitor device 21 and pipe end are positioned at this liquid air-capacitor device 21, as shown in Figure 2, when packing liquid in this liquid air-capacitor device 21, the pipe end of this tracheae 22 is the liquid levels that are higher than liquid in this liquid air-capacitor device 21, and can provide the steam of this liquid, the outer tube 24 that this liquid air-capacitor device 21 has a controllable temperature is communicated in this housing 11 outsides, can liquid be provided or other gas (for example helium and nitrogen etc.) directly is provided for the outside, other gas that this outside provides need be heated to and liquid air-capacitor device 21 equalities of temperature in advance, meeting cold generation with the steam of avoiding liquid air-capacitor device 21 interior these liquid condenses, this in the present embodiment, be to pack into and air chamber 16 synthermal water in this liquid air-capacitor device 21, and provide the saturated steam under this temperature to be depressed in this air chamber 16;
One sample tool 31, has an articles holding table 32, in order to load sample, this articles holding table 32 has an opening 34, this sample tool 31 is by stretching into and be placed in this air chamber 16 via this glove hole 114 outward, and the coaxial axle center that makes this endoporus 142 and this outer hole 112 is by this opening 34, and this sample tool 31 has a seal 36, clogs in the space of 16 of this sample tool 31 and this air chambers.
One air extractor 41 is connected in this two aspirating hole 116, in order to this two surge chamber 18 is bled.
As shown in Figure 2 to Figure 3, the present invention of aforementioned structure, when operation, be to be with the installation of in the sample room 92 of electron microscope 91, the hole 94 of inserting default when it can directly be dispatched from the factory by manufacturer by 92 sides, sample room is inserted, because this height of more flat 12 is less than distance between two utmost point pieces 96 (pole piece) of electron microscope 91, so this more flat 12 can place between this two utmost points piece 96, and make this endoporus 142 and this outer hole 112 be aligned with electron microscope 91 electron beam the path of process; This sample tool 31 that will be mounted with sample 99 is again inserted this air chamber 16 by this glove hole 114, and makes this sample 99 be aligned with this endoporus 142 and this outer hole 112.
Then, control the temperature of this housing 11, this dividing plate 14, this liquid air-capacitor device 21, tracheae 22 and this sample tool 31, make that the gas temperature that injects from tracheae 22 is identical with the temperature of this sample tool 31 and these sample tool 31 front end articles holding tables 32 with this air chamber 16.And seeing through this liquid air-capacitor device 21 provides the gas of preset pressure to this air chamber 16, again by bleeding by 41 pairs of these two surge chambers 18 of this air extractor, promptly can be drawn out of via the gas of these endoporus 142 loss in this air chamber 16 to this two surge chamber 18, and can be via these outer hole 112 loss to this housing 11, by charge velocity by the control speed of exhaust and these liquid air-capacitor device 21 gases, can keep gas in this air chamber 16 in a predetermined pressure, by this reach under the vacuum environment in this air chamber 16 effect of operating gas; And the electron beams of electron microscope 91 itself can see through this endoporus 142 and should detect this sample 99 in outer hole 112, by to reach the effect of observation.
Among this first embodiment, as shown in Figure 4, this liquid air-capacitor device 21 also can be located at this housing 11 outsides, be connected in this injecting hole 166 in this housing 11 and utilize this tracheae 22 to be inserted into, this structure not only has with liquid air-capacitor device 21 to be located at outside the function in this housing 11, the gas pressure scope of unsaturated vapor also can be provided simultaneously, be because of liquid air-capacitor device 21 when housing 11 is outside, the temperature control of this liquid air-capacitor device 21 is lower than the temperature of air chamber 16 and sample tool 31 front end articles holding tables 32, and needn't keep equality of temperature with sample articles holding table 32 with air chamber 16 in the housing 11, so can near the sample that is loaded on the articles holding table 32, produce the steam pressure environment that is lower than saturated vapour pressure, and be located at this housing 11 outside persons of being convenient to operation and operate, can at any time the gas injection action be closed, can accurately judge simultaneously the water yield of water level and supply, have extra convenience.
Again, as shown in Figure 5, the present invention's second preferred embodiment is provided a kind of in vacuum or environment under low pressure operating gas and can take off embodiment before mainly generally being same as for the device 50 of observation, difference is:
This housing 11 ' inside is by surge chamber 181 ' outside more forming on by most dividing plates 14 ' above this surge chamber 18 ' of this air chamber 16 ' top, and surge chamber 181 ' outside below this surge chamber 18 ' of this air chamber 16 ' below, more forming, this two surge chamber 18 ' is to correspond respectively to an aspirating hole 116 ', on being somebody's turn to do, outer surge chamber 181 ' then corresponds respectively to another aspirating hole 117 ' down, this aspirating hole 116 ', 117 ' is to be located at this housing 11 ', this two surge chamber 18 ' with should on, down the dividing plate 14 ' between the outer surge chamber 181 ' is to form a cushion hole 144 ' respectively, and coaxial with the outer hole of this endoporus 142 ' and this 112 '; Wherein, the aperture of this cushion hole 144 ' between 10um-400um, and between this endoporus 142 ' and should outside between the aperture in hole 112 '.By this, can pass through to reach the effect of decompression successively, and increase the respectively opereating specification of this surge chamber speed of exhaust by more multi-layered surge chamber 18 ', 181 ', the gas pressure in this air chamber 16 ' can reach higher pressure limit by this.And in the case, must be to the speed of exhaust of outer surge chamber 181 ' on this and the outer surge chamber 181 ' of this time greater than the speed of exhaust to this two surge chamber 18 '.
Before generally being same as, the mode of operation of this second embodiment takes off first embodiment.Increase by two times because of housing 11 ' internal damping number of chambers amount than first embodiment again, make the scope of controlling of this surge chamber gas speed of exhaust bigger and more flexible, in the present embodiment, the speed of exhaust of control surge chamber 18 ' and outer surge chamber 181 ' be respectively 160L/sec and 240L/sec or more than, can be the gas of 760 holder ears or the environment of steam and gas with boost in pressure to the stagnation pressure in the air chamber 16 ' then, and can not cause the vacuum area of gas from the outer hole 112 ' spill and leakage of this housing 11 ' to housing 11 ' outside.
Please consult Fig. 6 to Fig. 8 again, the present invention's the 3rd preferred embodiment is provided a kind of in vacuum or environment under low pressure operating gas and can take off embodiment before mainly generally being same as for the device 60 of observation, difference is:
Each surge chamber 18 " in have more an inclined clapboard 19; and will be respectively this surge chamber 18 " original separated by spaces is two sub-surge chambers 192, respectively this inclined clapboard 19 has a cushion hole 196, and with this endoporus 142 " and should outer hole 112 " coaxial, respectively 192 each correspondences of this sub-surge chamber are located at this housing 11 " on an aspirating hole 116 " can supply to bleed.
Among this 3rd embodiment, by setting by inclined clapboard 19, can not increase housing 11 " increase surge chamber 18 under the condition of height " quantity, that is, more aforementioned first embodiment respectively has more a surge chamber up and down, not only can reach the lifting air chamber 16 that aforementioned second embodiment is disclosed " effect of pressure to 760 holder ear, can make the scope of controlling of this surge chamber gas speed of exhaust big and have more elasticity simultaneously.
As Fig. 9 to shown in Figure 10, the present invention's the 4th preferred embodiment is provided a kind of in vacuum or environment under low pressure operating gas and can consisting predominantly of for the device 80 of observation:
One housing 81, one side forms one more flat 82, these housing 81 inside have two dividing plates 83, and these housing 81 inside are separated to form a surge chamber 821, and respectively form surge chamber 822 outside in these surge chamber 821 outside upper and lowers, the dividing plate 83 that this surge chamber 821 and this two outer surge chamber are 822 respectively has a cushion hole 831, and lay respectively at the top/bottom part of this surge chamber 821, the bottom surface, top of this housing 81 respectively has an outer hole 811 and is communicated in the external world, and this housing 81 has a glove hole 812 and is communicated in this surge chamber 821, and have 813 pairs of two aspirating holes should surge chamber 821, and in addition two aspirating holes 814 respectively to should two outer surge chambers 822;
One sample tool 85 is placed in this surge chamber 821 via this glove hole 812, these sample tool 85 inner air injection pipe 851 that form; One gas box 86, one end has an opening 861, and this gas box 86 is front ends that the part is embedded at this sample tool 85, and is communicated in this air injection pipe 851 with its opening 861, and bonding with a sticker 862, and this sample tool 85 forms a wall 852 around this gas box 86; This sample tool 85 has an injecting hole 853 and is communicated in this air injection pipe 851, one articles holding table 87 is formed in this gas box 86, can form an air chamber 863 in this gas box 86 for putting sample, coat this articles holding table 87, the bottom surface, top of this gas box 86 respectively has an endoporus 864 and is communicated in this surge chamber 821; This endoporus 864, this cushion hole 831 and this outer hole 811 be for coaxial.
Before mainly generally being same as, the mode of operation of this 4th embodiment takes off second embodiment, hold and do not give unnecessary details, wherein, flow into the temperature that these air injection pipe 851 interior gas temperatures must be less than or equal to these air injection pipe 851 walls, by meeting cold condensing with steams of avoiding injecting in this air injection pipe 851.
This 4th embodiment is formed at air chamber 863 in this sample tool 85, so that the preceding air chamber of taking off among first embodiment changes surge chamber into, to have more a surge chamber than first embodiment, can under the condition that does not increase housing 81 height, increase the quantity of surge chamber, not only can reach the effect of lifting air chamber pressure to the 760 holder ear that aforementioned second embodiment disclosed, can make the scope of controlling of this surge chamber gas speed of exhaust big and have more elasticity simultaneously.
Please consult Figure 11 again, the present invention's the 5th preferred embodiment is provided a kind of in vacuum or environment under low pressure operating gas and can be for the device a10 of observation, wherein this vacuum or environment under low pressure are to be the sample room 92 in the electron microscope 91, this sample room 92 is between two utmost point pieces 96 of electron microscope 91, on the axis G that electron beam between this two utmost points piece 96 passes through be comprise one the focusing interval Ra, this operating gas and can for observation device a10 include:
One housing a11, inside has at least one surge chamber a12, this housing a11 in its top and the bottom be respectively equipped with hole a14 outside.
One dividing plate a21 surrounds and forms an air chamber a22, and this dividing plate a21 is respectively equipped with an endoporus a24 corresponding to the top/bottom part of this air chamber a22, and the distance between this two endoporus a24 is less than 0.7mm (millimeter).
This housing a11 and this dividing plate a21 are can be combined, this dividing plate a21 forms this air chamber a22 in the present embodiment in this housing a11, this surge chamber a12 then is formed between this housing a11 and this dividing plate a21, this endoporus a24 is with should outer hole a14 coaxial and contain the axis G that this electron beam passes through, and this surge chamber a12 is covered by this endoporus a24 that is positioned at the top, and this endoporus a24 above being positioned at is with respect to this endoporus a24 of the opposite side (i.e. below) of this air chamber a22, then impose a pressure adjusting mechanism a28, in the present embodiment, this pressure adjusting mechanism a28 is the extension for this surge chamber a12, and be same surge chamber a12, that is this surge chamber a12 is contained this two endoporus a24.This housing a11 has two aspirating hole a16 and is communicated in this surge chamber a12, and this dividing plate a21 has an injecting hole a26 and is communicated in this air chamber a22.Wherein, this air chamber a22 joins in this interval Ra that focuses, that is, the extreme higher position that this housing a11 is arranged in this sample room 92 is the top of being less than or equal to this interval Ra that focuses for this air chamber a22 root edge, and the extreme lower position that this housing a11 is arranged in this sample room 92 is the lowermost end that is greater than or equal to this interval Ra that focuses for the apical margin of this air chamber a22.The position of this air chamber a22 in the present embodiment is the centre for the interval Ra that focuses.Apart from being to make observation more clear, can not being subjected to the blocked up influence of gas-bearing formation and producing the problem of the unclear wash rice of electron scattering image between this two endoporus a24 less than 0.7mm.
Take off first embodiment before the mode of operation of this 5th embodiment generally is same as, by bleed by this aspirating hole a16 and all generally be same as by mode of operation by this injecting hole a26 gas injection before take off first embodiment, identical person holds and does not give unnecessary details.Wherein different persons are for this air chamber a22 must join in this interval Ra that focuses, and can effectively focus to observe after can allowing the sample of inserting be placed in air chamber a22.
Please consult Figure 12 to Figure 13 again, the present invention's the 6th preferred embodiment is provided a kind of in vacuum or environment under low pressure operating gas and can take off the 5th embodiment before mainly generally being same as for the device b10 of observation, difference is:
This dividing plate b21 be with this housing b11 be separable relation, that is surrounded this air chamber b22 that forms by this dividing plate b21 and can be separated with this housing b11 and this surge chamber b12, in the present embodiment, this dividing plate b21 is formed on the sample tool b25, and forms this air chamber b22 between this dividing plate b21 and this sample tool b25.Be to seal between this sample tool b25 and this dividing plate b21 and this housing b11 with at least one seal b29 (for example O shape ring).
The mode of operation of this 6th embodiment is: during use, this dividing plate b21 is placed in this housing b11, sealing part b29 is between this sample tool b25 and this dividing plate b21 and this housing b11 and bring into play the effect that seals.Remaining mode of operation with before take off embodiment generally with, bleed again and method of gas injection also general with, hold and do not give unnecessary details.
Please consult Figure 14 to Figure 15 again, the present invention's the 7th preferred embodiment is provided a kind of in vacuum or environment under low pressure operating gas and can take off the 6th embodiment before mainly generally being same as for the device c10 of observation, difference is:
On this sample tool c25 by this dividing plate c21 surround form this air chamber c22, this housing c11 inside more is separated out surge chamber c18 in some dividing plate c17 with this surge chamber c12 inside again, two cushion hole c19 are located at this dividing plate c17 and lay respectively at surge chamber c18 top/bottom part in this, this cushion hole c19 is coaxial with this endoporus c24 and this outer hole c14, and the both sides of surge chamber c18 are respectively equipped with an aspirating hole c181 in this, and this housing c11 also has two gas flow c182 and is communicated in this two aspirating hole c181 respectively.This housing c11 front side has an inserting hole c111 and is communicated in surge chamber c18 in this, and this sample tool c25 goes up and inserted by this inserting hole c111 by the formed air chamber c22 of this dividing plate c21.
This 7th embodiment structurally mainly more has more surge chamber c18 in than the 6th embodiment, and can have the effect as the increase surge chamber of second embodiment.And the mode of operation of this 7th embodiment with before take off the 6th embodiment generally with, bleed and method of gas injection also general with, hold and do not give unnecessary details.
Please consult Figure 16 again, the present invention's the 8th preferred embodiment is provided a kind of in vacuum or environment under low pressure operating gas and can take off the 6th embodiment before mainly generally being same as for the device d10 of observation, difference is:
Surround the formation one air chamber d22 except going up as the sample tool d25 among the 6th embodiment with this dividing plate d21, this the 8th embodiment more in this sample tool d25 outside surround a dividing plate d27 again and form coat this air chamber d22 one in surge chamber d28, be positioned at outside this dividing plate d27 and be respectively equipped with a cushion hole d29 corresponding to bottom surface, this surge chamber d28 top, this cushion hole d29 is coaxial with this endoporus d24.This housing d11 then with this sample tool d25 on this dividing plate d27 be relation separable or that combine, in use, be to combine with this housing d11.
This 8th embodiment has more surge chamber d28 in than the 6th embodiment, and should be formed on the sample tool d25 by interior surge chamber d28.Before generally being same as, the mode of operation of this 8th embodiment takes off the 6th embodiment and the 7th embodiment, the position that is provided with as for aspirating hole or injecting hole, then visual situation and be located at the side or as ditto take off the 7th embodiment be located at before and after side, hold and no longer give detailed description, bleed and method of gas injection also general with, hold no longer to give and give unnecessary details.
Please consult Figure 17 again, the present invention's the 9th preferred embodiment is provided a kind of in vacuum or environment under low pressure operating gas and can take off the 8th embodiment before mainly generally being same as for the device e10 of observation, difference is:
This housing e11 directly is coated on this dividing plate e21, that is, this housing e11 and this dividing plate e21 are combined on the sample tool e25, this dividing plate e21 is surge chamber e28 in this sample tool e25 goes up formation this air chamber e22 and is somebody's turn to do, this housing e11 forms this surge chamber e12 then and between more outer field this dividing plate e21, this endoporus e24, this cushion hole e29 and should outer hole e14 be coaxial.
The mode of operation of this 9th embodiment is to take off second embodiment before generally being same as, bleed and method of gas injection also general with, hold and do not give unnecessary details.
Please consult Figure 18 again, the present invention's the tenth preferred embodiment is provided a kind of in vacuum or environment under low pressure operating gas and can take off the 5th embodiment before mainly generally being same as for the device f10 of observation, difference is:
This pressure adjusting mechanism f28 is a film, and envelope is located at this endoporus f24 that is positioned at the below, and is different from the pressure adjusting mechanism (it is for combining with surge chamber) of the 5th embodiment.Among this tenth embodiment, this surge chamber f12 only is covered by this endoporus f24 that is positioned at the top.By this, this pressure adjusting mechanism f28 can stop that the interior gas of this air chamber f22 outwards overflows via this endoporus f24 of below, reaches pressure and regulates and the effect that cushions.
The mode of operation of this tenth embodiment is mainly also with preceding to take off the 5th embodiment identical, bleed and method of gas injection also general with, hold and do not give unnecessary details.
Please consult Figure 19 again, the present invention's the 11 preferred embodiment is provided a kind of in vacuum or environment under low pressure operating gas and can take off the 5th embodiment before mainly generally being same as for the device g10 of observation, difference is:
This pressure adjusting mechanism g28 is a film, and envelope is located at the outer hole g14 that is somebody's turn to do that is positioned at the below, and this surge chamber g12 is then contained this two endoporus g24.By this, this pressure adjusting mechanism g28 can stop that the interior gas of this surge chamber g12 outwards overflows via the outer hole g14 that is somebody's turn to do of below, regulates and the effect that cushions and can reach pressure.
Before generally being same as, the occupation mode of this 11 embodiment takes off the 5th embodiment, as for the position that is provided with of aspirating hole or injecting hole, then visual situation and be located at the side or as ditto take off the 7th embodiment be located at before and after side, hold and no longer to give detailed description, bleed and method of gas injection also general with, hold and do not give unnecessary details.
As from the foregoing, the advantage that has of the present invention is:
One, needn't change the original design of electron microscope, the present invention can be directly by electron microscopic The hole of inserting that mirror is reserved when dispatching from the factory is inserted, and it is that single component is inserted, and has solved existing skill Art directly is set in installation complexity on the electron microscope with environmental chamber, is difficult for the problem of volume production, Installation of the present invention is set very simple, only need simple training to get final product, and cost is lower, no Can not damage electron microscope, be the technology that is enough to be applicable to volume production demand on the industry.
Two, install easily owing to the present invention, and can allow the operator be bled by external control easily Speed, gas provide the parameters such as speed, and need not disassemble electron microscope adjustment, so gas The parameter control of pressing is comparatively easy.
Three, the present invention needn't adjust the sample room height of electron microscope, therefore can not cause electricity The change of son bundle focusing distance, and then solved differing or resolution ratio that prior art runs into The problems such as loss.
Four, the path of electron beam by gas is distance between pole piece in the design of front case Or more than, and this case imports the design of a more flat section, so that the thickness of air chamber is as thin as a wafer, can pass through Significantly to shorten electron beam through the distance of gas, therefore do not have because of the electron beam bump too much Gas molecule causes electronics multiple scattering seriously and makes the problem of resolution loss; In addition, originally Invention arranges the multilayer surge chamber outside air chamber design can allow to exist suitably in the different surge chambers Pressure Drop, and can make to this surge chamber gas speed of exhaust to control scope bigger, so The mode of operation of multilayer buffering can improve the gas pressure in this air chamber, reaches one atmospheric Environment.
Claims (28)
- One kind in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that including:One housing, one side forms a flat portion, this enclosure interior has at least one dividing plate, and this enclosure interior is separated to form an air chamber, and at least one surge chamber of the outside formation of this air chamber, the dividing plate of the bottom surface, top of this air chamber is respectively equipped with an endoporus, and the end face of this housing and bottom surface respectively are provided with an outer hole, this endoporus is with should outer hole coaxial and be positioned at this flat portion, and this housing has an aspirating hole and is communicated in this surge chamber, and has an injecting hole and be communicated in this air chamber.
- According to claim 1 described in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that more including: a liquid air-capacitor device is connected in this injecting hole with a tracheae, in order to provide gas to this air chamber.
- According to claim 2 described in vacuum or environment under low pressure operating gas and can be for the device of observation, it is characterized in that: described this gas is to be steam, or specific gas, perhaps is steam and the mixing of specific gas.
- According to claim 3 described in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that: described this specific gas is nitrogen or oxygen or carbon dioxide or inert gas or its mixture.
- According to claim 2 described in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that: described this liquid air-capacitor device is positioned at this surge chamber.
- According to claim 2 described in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that: described this liquid air-capacitor device is to be positioned at this outside.
- According to claim 1 described in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that more including: a sample tool, has an articles holding table, this articles holding table has an opening, this housing has a glove hole and is communicated in this air chamber, this sample tool is to be stretched into and be placed in this air chamber via this glove hole by the outside, and make the coaxial axle center in this endoporus and this outer hole pass through this opening, this sample tool has a seal, clogs the space between this sample tool and this air chamber.
- According to claim 1 described in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that more including: an air extractor is connected in this aspirating hole.
- According to claim 1 described in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that: the aperture of described this endoporus is to be 10-200um, aperture that should outer hole is to be 20-800um, and respectively the aperture of this endoporus less than the aperture in this outer hole respectively.
- According to claim 1 described in vacuum or environment under low pressure operating gas and can it is characterized in that for the device of observation: the thickness of described this flat portion is less than the distance of two utmost point interblocks about in the sample room of electron microscope.
- 11. according to claim 10 described in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that: in described this housing be more outside the upper and lower of this surge chamber forms on one respectively surge chamber and once outside surge chamber, this surge chamber and this are gone up outer surge chamber and all corresponding aspirating hole of the outer surge chamber of this time, this aspirating hole is to be located at this housing, dividing plate between this surge chamber and this upper and lower outer surge chamber is to form a cushion hole respectively, and coaxial with this endoporus and this outer hole.
- 12. according to claim 11 described in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that: the aperture of described this cushion hole between 10um-400um, and the aperture of this cushion hole between this endoporus and should outside between the aperture in hole.
- 13. according to claim 11 described in vacuum or environment under low pressure operating gas and can it is characterized in that for the device of observation: the described speed of exhaust that should go up the speed of exhaust of outer surge chamber and the outer surge chamber of this time greater than this surge chamber.
- 14. according to claim 1 described in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that: have more an inclined clapboard in described respectively this surge chamber, respectively the original separated by spaces of this surge chamber is two sub-surge chambers, respectively this inclined clapboard has a cushion hole, and with this endoporus and should outer hole coaxial, respectively this sub-surge chamber is to the aspirating hole on should housing.
- 15. one kind in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that: include:One housing, one side forms a more flat portion, this enclosure interior has at least one dividing plate, and this enclosure interior is separated to form a surge chamber, and form surge chamber outside in this surge chamber is outside, this surge chamber and the dividing plate that is somebody's turn to do between outer surge chamber have at least two cushion holes, and lay respectively at the top/bottom part of this surge chamber, the bottom surface, top of this housing respectively has an outer hole and is communicated in the external world, and this housing has a glove hole and is communicated in this surge chamber, and has two aspirating holes respectively to should surge chamber and should outer surge chamber;One sample tool, be placed in this surge chamber an inner air injection pipe, the gas box of forming of this sample tool via this glove hole, one end has an opening, this gas box is the front end that the part is embedded at this sample tool, and with its open communication in this air injection pipe, this sample tool has an injecting hole and is communicated in this air injection pipe, one articles holding table is formed in this gas box, for putting sample, form an air chamber in this gas box, the bottom surface, top of this gas box respectively has an endoporus and is communicated in this surge chamber; This endoporus, this cushion hole and this outer hole be for coaxial.
- 16. according to claim 15 described in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that: between described this gas box and this sample tool is bonding with a sticker.
- 17. according to claim 15 described in vacuum or environment under low pressure operating gas and can it is characterized in that for the device of observation: described this sample tool forms a wall around this gas box.
- 18. one kind in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that: described this vacuum or environment under low pressure are to be the sample room in the electron microscope, this sample room is between two utmost point pieces of electron microscope, the axle that electron beam between this two utmost points piece passes through is online to be to comprise a focusing interval, and this operating gas and the device that can supply to observe include:One housing, inside have at least one surge chamber, this housing to be less than its top or bottom wherein one be provided with hole outside;At least one dividing plate surrounds and forms an air chamber, and this dividing plate is respectively equipped with an endoporus corresponding to the bottom surface, top of this air chamber;This housing and this dividing plate make up, and make this endoporus coaxial with this outer hole, and make this surge chamber contain at least one this endoporus, the aforementioned endoporus of being contained impose a pressure adjusting mechanism with respect to this endoporus or this outer Kong Ze of the opposite side of this air chamber, and this endoporus be to contain the axis that electron beam passes through with being somebody's turn to do outer hole, this housing has an aspirating hole and is communicated in this surge chamber, and this dividing plate has an injecting hole and is communicated in this air chamber; Wherein, this air chamber is to join in this focusing interval.
- 19. according to claim 18 described in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that: the extreme higher position that described this housing is arranged in this sample room is to be less than or equal to the interval top of this focusing for this air chamber root edge, and the extreme lower position that this housing is arranged in this sample room is the lowermost end that is greater than or equal to this focusing interval for the apical margin of this air chamber.
- 20. according to claim 18 described in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that: described this dividing plate is to separate with this housing, that is to be surrounded this air chamber that forms by this dividing plate be to separate with this housing, is to seal with at least one seal between this dividing plate and this housing.
- 21. according to claim 20 described in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that: formed this air chamber of described this dividing plate is to be formed on the sample tool.
- 22. according to claim 21 described in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that: described this enclosure interior more is separated out surge chamber in some dividing plates with this surge chamber inside again, two cushion holes are located at this dividing plate and are laid respectively at surge chamber top/bottom part in this, this cushion hole is coaxial with this endoporus and this outer hole, and the both sides of surge chamber are respectively equipped with an aspirating hole in this, and this housing also has two gas flows and is communicated in this two aspirating hole respectively; This housing has an inserting hole and is communicated in surge chamber in this, is to be inserted by this inserting hole by the formed air chamber of this dividing plate on this sample tool.
- 23. according to claim 21 described in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that: be that this dividing plate with plural number forms this air chamber on this sample tool, an and interior surge chamber that forms this air chamber of coating, this dividing plate that coats surge chamber in this is respectively equipped with a cushion hole corresponding to bottom surface, surge chamber top in this, and this cushion hole is coaxial with this endoporus.
- 24. according to claim 23 described in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that: described this housing and this dividing plate are to be combined on the sample tool, this dividing plate be on this sample tool, form this air chamber and coat this air chamber should in surge chamber, this housing then and form between this dividing plate of surge chamber in this and form this surge chamber, this endoporus, this cushion hole and should outer hole be coaxial.
- 25. according to claim 18 described in vacuum or environment under low pressure operating gas and can be for the device of observation, it is characterized in that: described this pressure adjusting mechanism is to be a film, envelope is located at this endoporus.
- 26. according to claim 18 described in vacuum or environment under low pressure operating gas and can be for the device of observation, it is characterized in that: described this pressure adjusting mechanism is to be a film, envelope is located at this outer hole.
- 27. according to claim 18 described in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that: described this pressure adjusting mechanism is the extension for this surge chamber, and be same surge chamber, promptly this surge chamber is contained this two endoporus, this housing then is respectively equipped with hole outside in its end face and bottom surface, and it should outer hole be coaxial that this endoporus reaches.
- 28. according to claim 18 described in vacuum or environment under low pressure operating gas and can for observation device, it is characterized in that: the distance between described this two endoporus is less than 0.7 millimeter.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610075899 CN101067992A (en) | 2006-04-26 | 2006-04-26 | Apparatus for operating gas and providing for observing under vacuum or low-voltage environment |
| EP06009356A EP1722397A1 (en) | 2005-05-09 | 2006-05-05 | Device for operating with gas in vacuum or low-pressure environment of electron microscopes and for observation of the operation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610075899 CN101067992A (en) | 2006-04-26 | 2006-04-26 | Apparatus for operating gas and providing for observing under vacuum or low-voltage environment |
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| Publication Number | Publication Date |
|---|---|
| CN101067992A true CN101067992A (en) | 2007-11-07 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610075899 Pending CN101067992A (en) | 2005-05-09 | 2006-04-26 | Apparatus for operating gas and providing for observing under vacuum or low-voltage environment |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102142347A (en) * | 2011-01-28 | 2011-08-03 | 北京航空航天大学 | Sample chamber of electron microscope |
| CN103348439A (en) * | 2011-03-04 | 2013-10-09 | 株式会社日立高新技术 | Electron microscope sample holder and sample observation method |
| CN107389455A (en) * | 2017-09-05 | 2017-11-24 | 中国工程物理研究院流体物理研究所 | The heat sink and method of sample initial temperature in being compressed for Magnetic driving oblique wave |
| CN109187595A (en) * | 2018-09-27 | 2019-01-11 | 南京宁智高新材料研究院有限公司 | The device of local equivalents pressure caused by micro- gas beam in a kind of measurement transmission electron microscope |
| CN114324338A (en) * | 2022-01-10 | 2022-04-12 | 西南石油大学 | Online microscopic identification system for solid phase generation of high-pressure wax-containing oil-gas mixed transportation |
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2006
- 2006-04-26 CN CN 200610075899 patent/CN101067992A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102142347A (en) * | 2011-01-28 | 2011-08-03 | 北京航空航天大学 | Sample chamber of electron microscope |
| CN102142347B (en) * | 2011-01-28 | 2012-12-12 | 北京航空航天大学 | Sample chamber of electron microscope |
| CN103348439A (en) * | 2011-03-04 | 2013-10-09 | 株式会社日立高新技术 | Electron microscope sample holder and sample observation method |
| CN103348439B (en) * | 2011-03-04 | 2016-09-28 | 株式会社日立高新技术 | Ultramicroscope sample mount and sample observation method |
| CN107389455A (en) * | 2017-09-05 | 2017-11-24 | 中国工程物理研究院流体物理研究所 | The heat sink and method of sample initial temperature in being compressed for Magnetic driving oblique wave |
| CN109187595A (en) * | 2018-09-27 | 2019-01-11 | 南京宁智高新材料研究院有限公司 | The device of local equivalents pressure caused by micro- gas beam in a kind of measurement transmission electron microscope |
| CN109187595B (en) * | 2018-09-27 | 2021-05-11 | 南京宁智高新材料研究院有限公司 | Device for measuring local equivalent pressure caused by micro gas beams in transmission electron microscope |
| CN114324338A (en) * | 2022-01-10 | 2022-04-12 | 西南石油大学 | Online microscopic identification system for solid phase generation of high-pressure wax-containing oil-gas mixed transportation |
| CN114324338B (en) * | 2022-01-10 | 2023-11-03 | 西南石油大学 | Online microcosmic identification system for high-pressure wax-containing gas mixed transportation solid phase generation |
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Effective date of registration: 20071012 Address after: Xinshi County, Tainan, Taiwan Applicant after: Contrel Semiconductor Technology Co., Ltd. Address before: Kaohsiung County of Taiwan Province Applicant before: Li Binghuan |
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Open date: 20071107 |