CN108896594B - Material secondary electron emission characteristic measurement sample preprocessing device - Google Patents
Material secondary electron emission characteristic measurement sample preprocessing device Download PDFInfo
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- CN108896594B CN108896594B CN201811087187.8A CN201811087187A CN108896594B CN 108896594 B CN108896594 B CN 108896594B CN 201811087187 A CN201811087187 A CN 201811087187A CN 108896594 B CN108896594 B CN 108896594B
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- 239000000463 material Substances 0.000 title claims abstract description 41
- 238000005259 measurement Methods 0.000 title claims abstract description 29
- 238000007781 pre-processing Methods 0.000 title claims description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 95
- 210000004907 gland Anatomy 0.000 claims abstract description 77
- 238000003860 storage Methods 0.000 claims abstract description 77
- 230000033001 locomotion Effects 0.000 claims description 43
- 238000001816 cooling Methods 0.000 claims description 36
- 238000012546 transfer Methods 0.000 claims description 22
- 230000000903 blocking effect Effects 0.000 claims description 20
- 239000000498 cooling water Substances 0.000 claims description 18
- 230000005540 biological transmission Effects 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000009413 insulation Methods 0.000 claims description 16
- 238000007789 sealing Methods 0.000 claims description 13
- 230000009471 action Effects 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 8
- 238000005485 electric heating Methods 0.000 claims description 7
- 238000010926 purge Methods 0.000 claims description 3
- 238000005192 partition Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 8
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 238000013461 design Methods 0.000 description 11
- 238000012360 testing method Methods 0.000 description 10
- 238000007872 degassing Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 239000002826 coolant Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 238000005086 pumping Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000003749 cleanliness Effects 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000011358 absorbing material Substances 0.000 description 1
- 230000004308 accommodation Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000001073 sample cooling Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a sample pretreatment device for measuring secondary electron emission characteristics of materials, which comprises a vacuum cavity, a vacuum pump, a heating device and a control device, wherein the heating device comprises a bottom barrel and a gland; the device also comprises a driving part, wherein the driving part is used for driving the gland to move along the direction of the opening end of the bottom barrel; the device also comprises a sample storage table, wherein when the gland is buckled on the opening end of the bottom barrel, the sample storage table is positioned in a space surrounded by the bottom barrel and the gland; the vacuum chamber also comprises a grabbing and transferring part and a gate part, wherein the gate part is used as a channel between the closed space and the outer side of the vacuum chamber; the heating device is used for heating a space surrounded by the bottom barrel and the gland. The pretreatment device not only can effectively eliminate the influence of the adsorption gas and the volatile organic pollutants on the surface of the sample on the measurement of secondary electron emission characteristics of the material, but also can effectively avoid secondary pollution in the process of transferring the sample from the pretreatment cavity to the measurement cavity.
Description
Technical Field
The invention relates to the technical field of vacuum baking equipment, in particular to a sample pretreatment device for measuring secondary electron emission characteristics of materials.
Background
When an electron beam with certain energy bombards a solid material, electrons are emitted from the surface of the material, and the phenomenon is called secondary electron emission phenomenon of the solid material. The ratio of the number of secondary electrons emitted from the surface of a material to the number of primary incident electrons is called the secondary electron emission coefficient, which is a characteristic surface parameter of the material. The secondary electron emission coefficient of the surface of the material and the energy spectrum distribution of the emitted secondary electrons are not only related to factors such as the type of the material, the energy of the incident electrons, the incidence angle of the electrons and the like, but also can be influenced by the surface state of the material such as the surface roughness and the surface cleanliness of the sample, especially the surface cleanliness of the sample to be tested, if the surface of the sample is covered by the adsorbed impurity gas or the volatile organic contaminant, the test result of the secondary electron emission characteristic will deviate from the actual condition of the material to be tested seriously.
The existing secondary electron emission coefficient measuring device is not provided with a special baking and degassing pretreatment system, after a sample to be measured is subjected to solvent cleaning, a baking oven is used for baking and degassing pretreatment of the sample, the baking and degassing temperature of the treatment mode is low, the degassing effect is not ideal, and in the transferring process of the sample from the baking oven to a testing cavity, the problem of secondary pollution caused by exposing the atmosphere exists. Some devices are provided with sample injection systems, so that sample injection of a plurality of samples can be realized, heating wires are arranged on a sample test bench to heat and degas samples to be tested, and a certain in-situ degassing effect is achieved.
Disclosure of Invention
Aiming at the problems that the material for secondary electron emission characteristic measurement has insufficient temperature or secondary pollution after pretreatment when the surface pretreatment is carried out in the prior art, the invention provides a sample pretreatment device for secondary electron emission characteristic measurement of the material, which can not only effectively eliminate the influence of the adsorption gas and the volatile organic pollutants on the surface of a sample on the secondary electron emission characteristic measurement of the material, but also effectively avoid the secondary pollution in the process of transferring the sample from a pretreatment cavity to a measurement cavity by adopting the structural design.
The technical means of the scheme is that the sample pretreatment device for measuring secondary electron emission characteristics of materials comprises a vacuum cavity with a closed space, a vacuum pump connected with the closed space, and a heating device, wherein the heating device comprises a barrel-shaped bottom barrel and a gland used as a sealing plate at the opening end of the bottom barrel, and the heating device is positioned in the closed space;
the device also comprises a driving part arranged on the vacuum cavity, wherein the driving part is connected with the gland through a motion transmission piece and is used for driving the gland to move along the direction of the opening end of the bottom barrel;
The sample storage table is arranged on the pressing cover, and is positioned in a space surrounded by the bottom barrel and the pressing cover when the pressing cover is buckled on the opening end of the bottom barrel;
the device also comprises a grabbing and transferring part and a gate part which are fixed on the vacuum cavity, wherein the gate part is used as a channel between the closed space and the outer side of the vacuum cavity, and the on-off state of the channel is adjustable;
after the sample storage table moves out of the bottom barrel along with the gland under the action of the driving part, the grabbing and transferring part grabs the sample on the sample storage table, and the grabbing and transferring part transfers the grabbed sample to the outer side of the closed space through the gate part;
the heating device is used for heating a space surrounded by the bottom barrel and the gland.
Specifically, in this scheme, the vacuum pump that sets up is as the vacuum generator in airtight space, promptly through the mode of evacuation, obtains the vacuum environment in the vacuum cavity. As a person skilled in the art, if the space enclosed in the heating device after the gland is matched with the bottom barrel is a closed space, then vacuum pumping is performed before the gland is not matched with the bottom barrel, and if the space enclosed in the heating device after the gland is matched with the bottom barrel is a non-closed space, then vacuum pumping treatment can be performed on the space in the vacuum cavity after the sample is mounted on the sample storage table. In this way, the space which is surrounded by the heating device and used for accommodating the sample storage table is a vacuum environment under the action of the vacuum pump.
In this scheme, set up to sample storage platform installs on the gland, the gland can cooperate with the end bucket under the effect of drive portion, so sample storage platform is located the region that heating device encloses, and heating device is used for heating the space that end bucket and gland both enclose, like this, compare in prior art at the vacuum chamber that is used for sample radioactivity characteristic measurement, because the vacuum environment that is enclosed by end bucket, the gland can, satisfy sample storage platform and its sample hold the function on, need not be like the vacuum chamber that is used for sample secondary electron emission characteristic measurement still need consider when volume design holds sample plummer, secondary electron collector, electron gun etc. so adopt above scheme, consider the heat transfer ability of vacuum environment and compare in atmospheric environment heat transfer ability worse characteristic, set up specific heating device form and be used for heating the sample, can make the baking temperature to the sample by current about 200 ℃ improve to more than 500 ℃ easily, so adopt this scheme, can not only improve pretreatment efficiency through the form that improves the baking temperature, can also can be through improving the form that the baking temperature and can cause the effective pollutant on the surface of the sample and can be polluted with the surface of the volatile nature of measuring and the surface of the more effective carrier gas can be avoided.
Meanwhile, in the scheme, the device is arranged to comprise a driving part for driving the gland so as to change the matching relation between the gland and the bottom barrel, so that the state of the heating device can be that: the sample storage table is in a state of being convenient for placing the sample, the sample is baked, and the sample storage table is in a state of being convenient for taking out the sample. Simultaneously set up to still including snatching transfer portion, snatch the transfer portion more above and snatch the sample through the preliminary treatment after shifting out in the bottom bucket in the sample storage platform and transport to gate portion, when specifically using, through setting up to one side of gate portion for above the enclosure space, the opposite side is for being used for carrying out secondary electron emission characteristic measuring's measurement vacuum space to the sample, gate portion opens the back promptly, gate portion is as the passageway of two vacuum spaces of intercommunication, so when carrying out the transfer of preliminary treatment after the sample, there is not the problem that leads to secondary pollution with atmospheric environment contact, so structural design of this scheme can effectively avoid the sample to shift to the measurement chamber in-process by the preliminary treatment chamber and receive secondary pollution.
As a person skilled in the art, the above gate part only needs to be opened when the sample is transferred after pretreatment, so that the gate plate on the gate part can be regarded as a part of the cavity wall of the vacuum cavity, and the gate part can achieve the corresponding purpose by adopting the gate plate valve in the prior art. The driving part can be arranged to comprise a power part as a power source, the motion transmission part can comprise a motion state conversion device and a motion transmission device, and the motion transmission part can be designed to comprise a gear toothed plate when the power part is a motor and outputs torque, and the gear is meshed with the toothed plate, so that the rotary motion can be converted into linear reciprocating motion; the novel gland driving mechanism can be arranged to be a motion transmission piece, and comprises a threaded rod and a sliding block in threaded connection with the threaded rod, wherein the threaded rod is collinear with the motor axis and is driven by the motor to rotate around the axis of the threaded rod, the sliding block is prevented from being restrained along with the rotation of the threaded rod by the aid of the sliding block, and the rotating direction of the threaded rod can be controlled, so that the sliding block moves towards a specific direction along the axis direction of the threaded rod to drive the gland to move. The power part is provided with a pneumatic driving device and a hydraulic driving device which can output linear motion, and the power transmission part is provided with a connecting rod corresponding to the position between the piston rod and the gland.
The grabbing and transferring parts need to complete grabbing and transferring actions when working, as a person skilled in the art can adopt the mode that grippers, such as mechanical arms, are arranged at the end parts of the grabbing and transferring parts, and the corresponding transferring actions can adopt magnetic rods to realize the functions except the mode that the driving parts drive the gland to displace in space.
The above snatch transfer portion and drive portion all need set up the power supply, for the vacuum environment in doing benefit to the vacuum cavity, if avoid forming the air release source in the vacuum cavity, the contaminated medium enters into the vacuum cavity, it is preferable to set up to above the power supply all is located the outside of vacuum cavity, like this, corresponding power supply can be fixed on the outer wall of vacuum cavity through flange, corresponding motion transmission piece or need stretch into the member between the vacuum cavity and vacuum cavity cooperation position setting up packing seal, O shape circle etc. can guarantee that vacuum cavity and external sealed isolation.
The further technical scheme is as follows:
because the measured sample may have the inconsistent problem of volume, shape and size, in order to make this preprocessing device have better adaptability and can accomplish the preliminary treatment of a plurality of samples simultaneously, set up to: the sample storage table is of a columnar structure, and a plurality of slots are formed in the side face of the sample storage table. By adopting the scheme, the plurality of slots can be matched with the plurality of sample trays, namely, the sample is fixed on the sample tray by inserting the sample tray into the slots, so that the volume, the shape and the like of the sample do not influence the mounting mode of the sample on the sample storage table, and the adaptability of the pretreatment device to the sample is improved; the slots are multiple, so that the slots are matched with the sample trays, and a plurality of samples can be fixed on the sample storage table to improve the pretreatment efficiency of the device.
As a specific implementation mode of the driving part and the grabbing and transferring part, the driving part drives the gland to do linear reciprocating motion, the grabbing and transferring part drives the grabbing end on the grabbing and transferring part to do linear reciprocating motion, and the grabbing and transferring part and the gate part are in opposite arrangement relation on the vacuum cavity. By adopting the scheme, when the position transfer of the sample in the space is completed, the driving part and the grabbing and transferring part can achieve the corresponding purpose through linear motion, so the scheme has the characteristics of simple structure and convenient manufacture and maintenance. As a person skilled in the art, since the sample has to be transferred between the drive section and the gripping and transferring section, the above two straight-line reciprocations need to have an intersection point at which the above transfer is effected. Preferably, in order to reduce the mutual influence of the motion of the driving part and the grabbing and transferring part, the motion directions of the two straight reciprocating motions can be set to be mutually perpendicular, if the motion output by the driving part is located in the vertical direction, the motion output by the grabbing and transferring part is located in the horizontal direction, further, if the driving part is arranged at the top of the vacuum cavity, the grabbing and transferring part and the gate part are arranged on the side surface of the vacuum cavity, the side surface where the grabbing and transferring part is located and the side surface where the gate part is located are a pair of opposite side surfaces, the heating device is arranged at the bottom of the vacuum cavity, the opening end of the bottom barrel faces upwards, after the sample is preprocessed in the heating device, the sample moves upwards to the point where the grabbing and transferring part can grab along with the gland, and after the grabbing and transferring part finishes grabbing the sample, the gland continues to move upwards to provide a motion channel for the movement of the working front end of the grabbing and transferring part.
In order to improve the heat utilization rate and the pretreatment efficiency of samples, the bottom barrel and the pressing cover are respectively provided with a heat insulation layer, after the pressing cover is matched with the bottom barrel as a closing plate at the opening end of the bottom barrel, the heat insulation layers on the bottom barrel and the pressing cover enclose a closed space, and the sample storage table is positioned in the closed space. By adopting the scheme, after the gland is matched with the bottom barrel, the corresponding sample can be heated in a vacuum space insulated from the outside. By adopting the scheme, if the heating device is an electric heating device comprising an electric heating wire, the heating wire is arranged at the inner side of the heat insulation layer.
As a technical scheme capable of realizing forced cooling, no matter a heat insulation layer exists or is not arranged, heat can not be completely prevented from being transferred to the outside by the heating device, and the technical scheme is as follows: the side wall of the bottom barrel is of a dividing wall type structure comprising an outer barrel and an inner barrel, the outer barrel is sleeved on the outer side of the inner barrel, a gap is formed between the outer barrel and the inner barrel, the side wall further comprises a water-cooling upper blocking plate serving as a gap upper end sealing plate and a water-cooling lower blocking plate serving as a gap lower end sealing plate, the water-cooling upper blocking plate, the water-cooling lower blocking plate, the outer barrel and the inner barrel enclose a cooling water accommodating cavity, and the side wall further comprises a water inlet pipe with one end connected with the cooling water accommodating cavity and a water outlet pipe with one end connected with the cooling water accommodating cavity. In this scheme, inner tube and urceolus all can set up to be tubular structure, and water-cooling upper closure plate and water-cooling lower closure plate can set up to be cyclic annular, and above four enclose into the inclosed cooling water that holds the endothermic medium and hold the chamber, through inlet tube and outlet pipe to import and export fluid in the cooling water holds the chamber for reach above-mentioned forced cooling function. By adopting the scheme, more heat can be effectively prevented from being emitted into the vacuum space outside the heating device, so that the temperature of the vacuum space outside the heating device can be controlled, the sealing performance of the vacuum cavity and corresponding parts on the vacuum cavity can be protected, and a sample after pretreatment can be naturally cooled to room temperature and then enters the vacuum cavity for measurement through the gate part. As a person skilled in the art, if the heat insulation layer is arranged on the bottom barrel, the side wall comprising the cooling water accommodating cavity is preferably arranged on the outer side of the heat insulation layer, namely, the heat insulation layer is arranged on the inner side of the inner barrel for improving the heat utilization rate and the pretreatment efficiency. As a person skilled in the art, although the technical terms are defined as a water-cooling upper blocking plate, a water-cooling lower blocking plate, a cooling water accommodating cavity, a water inlet pipe and a water outlet pipe in the scheme, in practice, if gas is adopted as the corresponding cooling medium, other liquids can realize the corresponding forced cooling effect, so that the corresponding cooling medium is the same or equivalent to the scheme when the corresponding cooling medium is gas or other liquids.
In order to reduce the heat transferred from the heating device to the vacuum cavity to improve the heat utilization rate and the pretreatment efficiency, the device is provided with: the bottom barrel is fixed on the vacuum cavity through a plurality of rod pieces. Specifically, the rod piece can be arranged to comprise a connecting screw rod and a positioning rod, the positioning rod is used for achieving the primary fixing of the relative positions of the bottom barrel and the vacuum cavity through the mode that the two ends of the positioning rod are respectively inserted into the bottom barrel and the vacuum cavity, and the final fixing of the relative positions of the bottom barrel and the vacuum cavity is achieved through the tensioning mode of the connecting screw rod. If the bottom barrel is installed on the bottom surface of the vacuum cavity, the opening end of the bottom barrel faces upwards, the bottom barrel can be provided with grooves for inserting positioning rods on the bottom surface of the vacuum cavity and the bottom surface of the bottom barrel, and the relative positions of the bottom barrel and the vacuum cavity are finally fixed through tensioning of the connecting screws. As a person skilled in the art, the two ends of the positioning rod can be connected with the bottom barrel and the vacuum cavity in a clamping manner, and at the moment, the connecting screw can achieve the relative position fixation of the bottom barrel and the vacuum cavity in a manner of extruding to two sides.
As a heating device proposal with high heating speed and easy control of power, the heating device is an electric heating device. When the scheme is adopted, the vacuum cavity is preferably provided with the power supply wire holder as an integrated design.
As an implementation scheme which is convenient for placing a sample to be treated into a sample storage table and conveniently observing the internal working state of the vacuum cavity in the pretreatment process, the device is set as follows: the vacuum chamber is characterized by further comprising an observation window serving as a local wall surface of the vacuum chamber, wherein the observation window is made of a light-permeable material, and the observation window is used as a detachable wall surface or an openable wall surface on the vacuum chamber. In this scheme, but above light-transmitting material is used for observing the behavior of this device promptly, and above observation window is as dismantling the wall or can open the wall on the vacuum cavity, promptly after the observation window dismantles or open the back, is as putting into the operation hole of waiting to handle the sample to the sample storage bench. As a person skilled in the art, the above observation window may adopt a connection scheme of a manhole flange and a hand hole flange on a pressure vessel in the prior art.
As an integrated design, a purge valve is also included that is mounted on the vacuum chamber. As a person skilled in the art, the above air release valve can be connected with the vacuum cavity through an air release valve interface arranged on the vacuum cavity, and the above air release valve is used as a pressure equalizing device for the internal space of the vacuum cavity and the external environment.
For the convenience of detecting the heating temperature of the heating device, set as: a thermocouple for measuring the temperature of the heating device is also included.
The invention has the following beneficial effects:
in this scheme, set up to sample storage platform installs on the gland, the gland can cooperate with the end bucket under the effect of drive portion, so sample storage platform is located the region that heating device encloses, and heating device is used for heating the space that end bucket and gland both enclose, like this, compare in prior art at the vacuum chamber that is used for sample radioactivity characteristic measurement, because the vacuum environment that is enclosed by end bucket, the gland can, satisfy sample storage platform and its sample hold the function on, need not be like the vacuum chamber that is used for sample secondary electron emission characteristic measurement still need consider when volume design holds sample plummer, secondary electron collector, electron gun etc. so adopt above scheme, consider the heat transfer ability of vacuum environment and compare in atmospheric environment heat transfer ability worse characteristic, set up specific heating device form and be used for heating the sample, can make the baking temperature to the sample by current about 200 ℃ improve to more than 500 ℃ easily, so adopt this scheme, can not only improve pretreatment efficiency through the form that improves the baking temperature, can also can be through improving the form that the baking temperature and can cause the effective pollutant on the surface of the sample and can be polluted with the surface of the volatile nature of measuring and the surface of the more effective carrier gas can be avoided.
Meanwhile, in the scheme, the device is arranged to comprise a driving part for driving the gland so as to change the matching relation between the gland and the bottom barrel, so that the state of the heating device can be that: the sample storage table is in a state of being convenient for placing the sample, the sample is baked, and the sample storage table is in a state of being convenient for taking out the sample. Simultaneously set up to still including snatching transfer portion, snatch the transfer portion more above and snatch the sample through the preliminary treatment after shifting out in the bottom bucket in the sample storage platform and transport to gate portion, when specifically using, through setting up to one side of gate portion for above the enclosure space, the opposite side is for being used for carrying out secondary electron emission characteristic measuring's measurement vacuum space to the sample, gate portion opens the back promptly, gate portion is as the passageway of two vacuum spaces of intercommunication, so when carrying out the transfer of preliminary treatment after the sample, there is not the problem that leads to secondary pollution with atmospheric environment contact, so structural design of this scheme can effectively avoid the sample to shift to the measurement chamber in-process by the preliminary treatment chamber and receive secondary pollution.
Drawings
FIG. 1 is a schematic diagram of a sample pretreatment apparatus for measuring secondary electron emission characteristics of a material according to an embodiment of the present invention;
FIG. 2 is a partial cross-sectional view of an embodiment of a sample pretreatment apparatus for measuring secondary electron emission characteristics of a material according to the present invention, the cross-sectional view reflecting the structure of a driving part and the connection relationship between the driving part and a sample storage stage;
FIG. 3 is a schematic view showing a partial structure of an embodiment of a sample pretreatment apparatus for measuring secondary electron emission characteristics of a material according to the present invention, the schematic view reflecting the structure of a bottom barrel, and the view port being positioned at the lower front of the bottom barrel;
FIG. 4 is a schematic view of a partial structure of an embodiment of a sample pretreatment apparatus for measuring secondary electron emission characteristics of a material according to the present invention, the schematic view reflecting the structure of a bottom barrel and the intended bottom view of the bottom barrel;
FIG. 5 is a partial cross-sectional view of an embodiment of a sample pretreatment apparatus for measuring secondary electron emission characteristics of a material according to the present invention, the cross-sectional view reflecting the structure of a bottom barrel and the connection relationship with a vacuum chamber;
fig. 6 is a partial cross-sectional view of an embodiment of a sample pretreatment apparatus for measuring secondary electron emission characteristics of a material according to the present invention, the cross-sectional view reflecting the structure of a bottom tub and the connection relationship with a vacuum chamber.
Reference numerals in the drawings are respectively: 1. the device comprises a power part, 2, a motion transmission part, 3, a connecting flange, 4, a gland, 5, a sample storage table, 6, a sample tray, 7, a thermocouple, 8, a water-cooling upper blocking plate, 9, an inner cylinder, 10, a bottom barrel, 11, an outer cylinder, 12, a water-cooling lower blocking plate, 13, a positioning rod, 14, a vacuum cavity, 15, a groove body, 16, a connecting screw, 17, a water inlet pipe, 18, a water outlet pipe, 19, a relief valve interface, 20, a power wire holder, 21, a relief valve, 22, a driving part, 23, a grabbing and transferring part, 24, a gate part, 25 and a vacuum pump.
Detailed Description
The present invention will be described in further detail with reference to examples, but the structure of the present invention is not limited to the following examples.
Example 1:
as shown in fig. 1 to 6, a sample pretreatment device for measuring secondary electron emission characteristics of materials comprises a vacuum cavity 14 with a closed space, a vacuum pump 25 connected with the closed space, and a heating device, wherein the heating device comprises a barrel-shaped bottom barrel 10 and a gland 4 serving as an opening end sealing plate of the bottom barrel 10, and the heating device is positioned in the closed space;
the device further comprises a driving part 22 arranged on the vacuum cavity 14, wherein the driving part 22 is connected with the gland 4 through a motion transmission piece 2, and the driving part 22 is used for driving the gland 4 to move along the direction of the opening end of the bottom barrel 10;
The device also comprises a sample storage table 5 arranged on the gland 4, wherein when the gland 4 is buckled on the open end of the bottom barrel 10, the sample storage table 5 is positioned in a space surrounded by the bottom barrel 10 and the gland 4;
the vacuum chamber further comprises a grabbing and transferring part 23 and a gate part 24 which are fixed on the vacuum chamber 14, wherein the gate part 24 is used as a channel between the closed space and the outer side of the vacuum chamber 14, and the on-off state of the channel is adjustable;
after the sample storage table 5 moves out of the bottom barrel 10 along with the gland 4 under the action of the driving part 22, the grabbing and transferring part 23 grabs the sample on the sample storage table 5, and the grabbing and transferring part 23 transfers the grabbed sample to the outer side of the closed space through the gate part 24;
the heating device is used for heating the space surrounded by the bottom barrel 10 and the gland 4.
Specifically, in this embodiment, the vacuum pump 25 is provided as a vacuum generator for the closed space, that is, a vacuum environment is obtained in the vacuum cavity 14 by means of vacuumizing. As a person skilled in the art, if the space enclosed in the heating device after the cooperation of the gland 4 and the bottom barrel 10 is a closed space, then the vacuum pumping is performed before the gland 4 is not mated with the bottom barrel 10, and if the space enclosed in the heating device after the cooperation of the gland 4 and the bottom barrel 10 is an unsealed space, then the vacuum pumping treatment can be performed on the space in the vacuum chamber 14 after the sample is mounted on the sample storage table 5. In this way, the space enclosed by the heating device for accommodating the sample storage stage 5 is made to be a vacuum environment by the vacuum pump 25.
In this scheme, set up to sample storage platform 5 install on gland 4, gland 4 can cooperate with end bucket 10 under the effect of drive portion 22, make sample storage platform 5 be located the region that heating device encloses, and heating device is used for heating the space that end bucket 10 and gland 4 enclose, like this, compare in prior art in the vacuum chamber that is used for sample radioactivity measurement, because the vacuum environment that is enclosed by end bucket 10, gland 4 can, satisfy the accommodation function to sample storage platform 5 and sample on it, need not be like the vacuum chamber that is used for sample secondary electron emission characteristic measurement still need consider when the volume design and hold sample plummer, secondary electron collector, electron gun etc. so the adoption scheme above, consider the heat transfer ability of vacuum environment and compare in atmospheric environment heat transfer ability worse characteristic, set up specific heating device form and be used for heating the sample, can make the baking temperature to the sample by current about 200 ℃ to improve more than 500 ℃ easily, so, adopt this scheme, can not only can not be through improving the pre-treatment temperature, can also be the effective form of influence on the surface of the sample is polluted by the volatile material through the improvement of the baking temperature, and can also be more effective to the form is the noise-absorbing material is avoided to the surface is polluted to the measurement.
Meanwhile, in the scheme, the driving part 22 is arranged to drive the gland 4 so as to change the matching relation between the gland 4 and the bottom barrel 10, so that the state of the heating device can be that: the sample storage table 5 is in a state of facilitating sample placement, a sample baking state, and the sample storage table 5 is in a state of facilitating sample removal. Meanwhile, the device is arranged to further comprise a grabbing and transferring part 23, the grabbing and transferring part 23 grabs a pretreated sample after the sample storage platform 5 is moved out of the bottom barrel 10 and transfers the sample to the gate part 24, when the device is used specifically, one side of the gate part 24 is the closed space, the other side of the gate part is the measurement vacuum space for secondary electron emission characteristic measurement of the sample, namely, after the gate part 24 is opened, the gate part 24 is used as a channel for communicating the two vacuum spaces, so that the problem of secondary pollution caused by contact with the atmospheric environment is avoided when the sample is transferred after pretreatment, and the structural design of the device can effectively avoid secondary pollution in the process of transferring the sample from the pretreatment cavity to the measurement cavity.
As a person skilled in the art, the above gate part 24 only needs to be opened when the sample is transferred after pretreatment, so that the gate plate on the gate part 24 can be regarded as a part of the cavity wall of the vacuum cavity 14, and the gate part 24 can achieve the corresponding purpose by adopting the gate valve in the prior art. The above driving part 22 may be configured to include the power part 1 as a power source, the above motion transmission member 2 may include a motion state conversion device, a motion transmission device, and a torque output when the power part 1 is a motor, where the motion transmission member 2 may be configured to include a gear-toothed plate, and the gear is meshed with the toothed plate, so that rotational motion may be converted into linear reciprocating motion; the motion transmission member 2 can also comprise a threaded rod and a sliding block in threaded connection with the threaded rod, the threaded rod is in line with the axis of the motor and is driven by the motor to rotate around the axis of the motor, the sliding block can be prevented from rotating along with the threaded rod by providing constraint of the sliding block, and the rotating direction of the threaded rod can be controlled, so that the sliding block moves along the axis direction of the threaded rod towards a specific direction to drive the gland 4 to move. The power part 1 is provided with a pneumatic driving device and a hydraulic driving device which can output linear motion, and the power transmission part is provided with a connecting rod corresponding to the position between the piston rod and the gland 4.
The above grabbing and transferring part 23 needs to complete grabbing and transferring actions when working, as a person skilled in the art can adopt a gripper such as a mechanical arm at the end of the grabbing and transferring part 23, and the corresponding transferring actions can adopt a magnetic rod to realize the functions besides adopting the mode that the above driving part 22 drives the gland 4 to displace in space.
The above grabbing and transferring part 23 and the driving part 22 are both required to be provided with power sources, so as to be beneficial to the vacuum environment in the vacuum cavity 14, for example, an air release source is avoided from being formed in the vacuum cavity 14, a pollution medium enters into the vacuum cavity 14, and the above power sources are preferably arranged to be located on the outer side of the vacuum cavity 14, so that the corresponding power sources can be fixed on the outer wall of the vacuum cavity 14 through the connecting flange 3, and the corresponding motion transmission parts 2 or rod members required to extend into the space between the vacuum cavity 14 and the matching position of the vacuum cavity 14 are provided with packing seals, O-shaped rings and the like, so that the vacuum cavity 14 can be ensured to be sealed and isolated from the outside.
Example 2:
as shown in fig. 1 to 6, this embodiment is further defined on the basis of embodiment 1: because the measured sample may have the inconsistent problem of volume, shape and size, in order to make this preprocessing device have better adaptability and can accomplish the preliminary treatment of a plurality of samples simultaneously, set up to: the sample storage table 5 is in a columnar structure, and a plurality of slots are arranged on the side face of the sample storage table 5. By adopting the scheme, the plurality of slots can be matched with the plurality of sample trays 6, namely, the sample is fixed on the sample tray 6 by inserting the sample tray 6 into the slots, so that the volume, the shape and the like of the sample do not influence the mounting mode of the sample on the sample storage table 5, and the adaptability of the pretreatment device to the sample is improved; the number of slots is multiple, so that the slots are matched with the sample trays 6, and a plurality of samples can be fixed on the sample storage table 5 to improve the pretreatment efficiency of the device.
As a specific implementation manner of the driving part 22 and the grabbing and transferring part 23, the driving part 22 drives the gland 4 to do linear reciprocating motion, the grabbing and transferring part 23 drives the grabbing end on the grabbing and transferring part to do linear reciprocating motion, and the grabbing and transferring part 23 and the gate part 24 are in a right opposite arrangement relationship on the vacuum cavity 14. By adopting the scheme, when the position transfer of the sample in the space is completed, the driving part 22 and the grabbing and transferring part 23 can achieve the corresponding purpose through linear motion, so the scheme has the characteristics of simple structure and convenient manufacture and maintenance. As a person skilled in the art, since the sample has to be transferred between the drive section 22 and the gripping and transferring section 23, the above two straight reciprocating movements need to have an intersection point at which the above transfer is achieved. Preferably, in order to reduce the mutual influence of the movements of the driving part 22 and the grabbing and transferring part 23, the directions of the movements of the two straight line reciprocating movements can be set to be mutually perpendicular, if the movement output by the driving part 22 is in the vertical direction, the movement output by the grabbing and transferring part 23 is in the horizontal direction, further, if the driving part 22 is arranged at the top of the vacuum cavity 14, the grabbing and transferring part 23 and the gate part 24 are arranged at the side of the vacuum cavity 14, the side where the grabbing and transferring part 23 is arranged and the side where the gate part 24 is arranged are a pair of opposite sides, the heating device is arranged at the bottom of the vacuum cavity 14, the opening end of the bottom barrel 10 is upward, after the sample is preprocessed in the heating device, the sample moves upward along with the gland 4 to the point where the grabbing and transferring part 23 can grab, and after the grabbing and transferring part 23 grabs the sample, the gland 4 continues to move upward to provide a movement channel for the working front end of the grabbing and transferring part 23 to move towards the gate part 24.
In order to improve the heat utilization rate and the pretreatment efficiency of samples, the bottom barrel 10 and the gland 4 are respectively provided with a heat insulation layer, after the gland 4 is matched with the bottom barrel 10 as an opening end sealing plate of the bottom barrel 10, the heat insulation layers on the bottom barrel 10 and the gland 4 enclose a closed space, and the sample storage table 5 is positioned in the closed space. By adopting the scheme, after the gland 4 is matched with the bottom barrel 10, the corresponding sample can be heated in a vacuum space insulated from the outside. By adopting the scheme, if the heating device is an electric heating device comprising an electric heating wire, the heating wire is arranged at the inner side of the heat insulation layer.
As a technical scheme capable of realizing forced cooling, no matter a heat insulation layer exists or is not arranged, heat can not be completely prevented from being transferred to the outside by the heating device, and the technical scheme is as follows: the side wall of the bottom barrel 10 is of a dividing wall type structure comprising an outer barrel 11 and an inner barrel 9, the outer barrel 11 is sleeved on the outer side of the inner barrel 9, a gap is formed between the outer barrel 11 and the inner barrel 9, the side wall further comprises a water-cooling upper blocking plate 8 serving as a sealing plate at the upper end of the gap and a water-cooling lower blocking plate 12 serving as a sealing plate at the lower end of the gap, the water-cooling upper blocking plate 8, the water-cooling lower blocking plate 12, the outer barrel 11 and the inner barrel 9 enclose a cooling water accommodating cavity, and the side wall further comprises a water inlet pipe 17 with one end connected with the cooling water accommodating cavity and a water outlet pipe 18 with one end connected with the cooling water accommodating cavity. In this scheme, inner tube 9 and urceolus 11 all can set up to be tubular structure, and water-cooling upper closure plate 8 and water-cooling lower closure plate 12 can set up to be cyclic annular, and four above enclose into have the inclosed cooling water that holds the endothermic medium and hold the chamber, through inlet tube 17 and outlet pipe 18 to the leading-in and leading-out fluid in the cooling water holds the chamber for reach above-mentioned forced cooling function. By adopting the scheme, more heat can be effectively prevented from being emitted into the vacuum space outside the heating device, so that the temperature of the vacuum space outside the heating device can be controlled, the sealing performance of the vacuum cavity 14 and corresponding parts on the vacuum cavity 14 are protected, and a sample after pretreatment can be naturally cooled to room temperature and then enters the vacuum cavity for measurement through the gate part 24. As a person skilled in the art, if the bottom tub 10 is provided with a heat insulation layer, the above side wall including the cooling water accommodating chamber is preferably disposed outside the heat insulation layer, i.e. the heat insulation layer is mounted on the inner side of the inner tub 9 for improving heat utilization efficiency and pretreatment efficiency. As a person skilled in the art, although the technical terms are defined as the water-cooling upper blocking plate 8, the water-cooling lower blocking plate 12, the cooling water accommodating cavity, the water inlet pipe 17 and the water outlet pipe 18 in this scheme, in fact, if gas is adopted as the corresponding cooling medium, other liquids can also realize the corresponding forced cooling effect, so that the corresponding cooling medium is the same or equivalent scheme as that of this scheme when gas and other liquids are adopted as the corresponding cooling medium.
To reduce the heat transferred from the heating device to the vacuum chamber 14 to improve the heat utilization and pretreatment efficiency, it is provided that: the bottom tub 10 is fixed to the vacuum chamber 14 by a plurality of bars. Specifically, the rod may include a connecting screw 16 and a positioning rod 13, where the positioning rod 13 is inserted into the bottom barrel 10 and the vacuum cavity 14 at two ends respectively to fix the relative positions of the bottom barrel 10 and the vacuum cavity 14, and then the connecting screw 16 is used to tighten the relative positions of the bottom barrel 10 and the vacuum cavity 14. If the bottom barrel 10 is mounted on the bottom surface of the vacuum cavity 14, the opening end of the bottom barrel 10 faces upwards, and the bottom surface of the vacuum cavity 14 and the bottom surface of the bottom barrel 10 are provided with the groove bodies 15 for inserting the positioning rods 13, and the connecting screw rods 16 are used for realizing final fixing of the relative positions of the bottom barrel 10 and the vacuum cavity 14 in a tensioning mode. As a person skilled in the art, the two ends of the positioning rod 13 may also be connected to the bottom barrel 10 and the vacuum cavity 14 by a clamping manner, and the connecting screw 16 may be pressed to two sides to fix the relative positions of the bottom barrel 10 and the vacuum cavity 14.
As a heating device proposal with high heating speed and easy control of power, the heating device is an electric heating device. In this embodiment, as an integrated design, it is preferable to provide the vacuum chamber 14 with a power supply connection base 20.
As an implementation scheme for facilitating the placement of a sample to be processed on the sample storage table 5 and facilitating the observation of the internal working state of the vacuum chamber 14 during the pretreatment process, the following is set: the vacuum chamber further comprises an observation window serving as a local wall surface of the vacuum chamber 14, wherein the observation window is made of a light-permeable material, and the observation window is used as a detachable wall surface or an openable wall surface on the vacuum chamber 14. In this scheme, the above light-permeable material is used for observing the working condition of the device, and the above observation window is used as a detachable wall surface or an openable wall surface on the vacuum cavity 14, i.e. after the observation window is detached or opened, as an operation hole for placing the sample to be processed on the sample storage table 5. As a person skilled in the art, the above observation window may adopt a connection scheme of a manhole flange and a hand hole flange on a pressure vessel in the prior art.
As an integrated design, a purge valve 21 is also included, mounted on the vacuum chamber 14. As a person skilled in the art, the above air release valve 21 can be connected to the vacuum chamber 14 through the air release valve interface 19 provided on the vacuum chamber 14, and the above air release valve 21 serves as a pressure equalizing device for the internal space of the vacuum chamber 14 and the external environment.
For the convenience of detecting the heating temperature of the heating device, set as: a thermocouple 7 for measuring the temperature of the heating means is also included.
Example 3:
the embodiment provides a concrete implementation mode of a sample pretreatment device for measuring secondary electron emission characteristics of materials, wherein a vacuum movable platform is connected to the top of the periphery of a vacuum cavity 14, the vacuum movable platform is a driving part 22, a gate valve which is arranged in the middle and is a gate part 24 and a molecular pump which is a vacuum pump 25 are arranged opposite to a magnetic rod which is a grabbing and transferring part 23, and a deflation valve 21 and a power supply wire holder 20 which is a heating control power supply introduction point are connected to the bottom of the vacuum cavity 14; the upper portion of the vacuum cavity 14 is provided with a vacuum moving platform, the output end of the vacuum moving platform is positioned at the lower end, the sample storage platform 5 and the gland 4 are connected to the lower end of the vacuum moving platform, the bottom barrel 10 is positioned right below the gland 4, the opening end of the bottom barrel 10 faces upwards, and the bottom barrel 10 and the gland 4 are both provided with heat insulation materials serving as heat shields.
When sample injection operation is carried out, firstly, a sample to be detected after solvent cleaning treatment is fixed on a sample tray 6, a quick door opening observation window is opened, a vacuum movable platform drives a sample storage table 5 to be opposite to the quick door opening observation window, five sample mounting stations are arranged on the sample storage table 5, the five sample trays 6 which are sheet-shaped and provided with tabletting thereon are sequentially inserted into sample storage grids of the sample mounting stations, then, a deflation valve 21 and the quick door opening observation window are closed, and a backing pump and a molecular pump are opened for vacuum pumping; the vacuum degree in the vacuum cavity 14 reaches 10 -3 In the Pa level, the vacuum moving platform drives the sample storage platform 5 to descend into the annular heater of the bottom barrel 10, so that the upper part and the lower part form a heat shielding structure: gland4 and the bottom barrel 10 are combined into a whole, namely the whole sample storage table 5 is wrapped in the annular heater; the water cooler and the heater control power supply are turned on, the heating speed, the constant temperature and the constant temperature time of sample heating are set according to the difference of sample materials to be tested, the sample is subjected to baking and degassing pretreatment, heating is automatically stopped after baking is finished, the heating control power supply is turned off, and the sample is naturally cooled to room temperature; before the secondary electron emission characteristic test of the sample is started, the sample storage table 5 is driven by the vacuum movable platform to rise to the position right opposite to the front end of the magnetic rod of the grabbing transfer part 23, the sample storage table is rotated to enable the sample tray 6 to be right opposite to the manipulator at the front end of the magnetic rod, the manipulator grabs the sample tray 6 to take out the sample from the sample storage table 5, and the vacuum movable platform drives the sample storage table 5 to continuously rise to the height which does not block the movement of the magnetic rod; opening a gate valve between the pretreatment device and the measuring chamber, feeding a sample into a sample test carrier in the measuring chamber by a magnetic rod, then withdrawing the magnetic rod, closing the gate valve, and testing secondary electron emission characteristics of the sample in the measuring chamber; after the test is finished, the gate valve is opened, the magnetic rod withdraws the sample tray together with the sample, the vacuum movable platform drives the sample storage table to descend to the position where the empty storage grid faces to the manipulator at the front end of the magnetic rod, the sample tray is put back into the sample storage table, then the position of the sample storage table 5 is moved, and the manipulator grabs the next sample to be tested; after the transmission, test and recovery of five samples to be tested are sequentially completed according to the steps, a gate valve and a vacuum pump power supply are closed, after a vacuum pump 25 is stopped, a deflation valve 21 connected with a nitrogen cylinder is opened, so that the air pressure in a vacuum cavity 14 is restored to atmospheric pressure, a quick-opening observation window is opened, a sample storage table 5 is moved to be opposite to the quick-opening observation window by a vacuum movable platform, five samples which are subjected to test are sequentially taken out, and then the whole processes of sample introduction, baking and degassing pretreatment, sample feeding, test and sample replacement are all completed.
Five sample storage grids are arranged on the side face of the sample storage table 5, each sample storage grid is a groove for the sample tray 6 to be inserted, samples with the sizes of 20mm multiplied by 2mm are fixed on the upper surface of the sample tray through pressing sheets on the sample tray, and five samples to be tested can be placed in the sample storage table 5 along with the sample tray 6 at a time; the sample storage table 5 is connected with the bottom of the gland 4 through a three-layer heat shielding structure above, the gland 4 is connected with a vacuum movable platform arranged at the top of the vacuum cavity, and the vacuum movable platform drives the sample storage table 5 to move up and down and rotate in the vacuum cavity 14.
The outer layers of the annular heater and the heat shielding mechanism are water-cooling sleeves, the inside of the annular heater and the heat shielding mechanism is provided with a heater, and the annular heater and the heat shielding mechanism are respectively connected to a blind flange at the bottom; the outer side of the bottom barrel 10 is also provided with three layers of heat shields, and the bottom barrel 10, the outer three layers of heat shields and the outermost water-cooling sleeve are of a coaxial structure; the water-cooling upper blocking plate 8, the inner cylinder 9, the outer cylinder 11, the water-cooling lower blocking plate 12, the water inlet pipe 17 and the water outlet pipe 18 form a complete water-cooling sleeve, cooling water circulates in the water-cooling sleeve through a water-cooling machine, heat dissipated by a heating device can be taken away, excessive temperature rise of other parts of the vacuum cavity 14 is avoided, and the whole water-cooling sleeve is fixed on a blind flange together by the water inlet pipe, the water outlet pipe and the positioning rod 13; the periphery of the heating device is provided with three heat shielding layers, and the heating device is integrally formed and then fixed on a flange supporting ring of the blind flange by a connecting screw 16; winding armoured heating wires inside the heating device to form a heating furnace, heating and baking the whole sample storage table 5 which is lowered into the heating device in a vacuum state, arranging K-type thermocouples at three positions which are positioned near the sample storage table in the heating furnace and are separated by 120 degrees from top to bottom, and connecting thermocouple temperature measuring signals and heating furnace wires to a heating furnace control power supply by a thermocouple wire holder and a power supply wire holder 20; the temperature uniformity of the heating zone in the heating furnace can be controlled to be +/-10 ℃ after the temperature rising speed, the constant temperature and the constant temperature time are set through the feedback of the K-type thermocouple. The heating furnace control power supply automatically monitors the heat preservation temperature, the temperature uniformity and the timely sample temperature in the sample cooling process, and after heating, the heating is automatically stopped and naturally cooled to the room temperature.
The foregoing is a further detailed description of the invention in connection with specific preferred embodiments, and it is not intended that the invention be limited to these descriptions. Other embodiments of the invention, which are apparent to those skilled in the art to which the invention pertains without departing from the technical solution of the invention, shall be covered by the protection scope of the corresponding invention.
Claims (10)
1. The device for pre-treating the material secondary electron emission characteristic measurement sample comprises a vacuum cavity (14) with a closed space, a vacuum pump (25) connected with the closed space and a heating device, and is characterized in that the heating device comprises a barrel-shaped bottom barrel (10) and a gland (4) serving as an opening end sealing plate of the bottom barrel (10), and the heating device is positioned in the closed space;
the device further comprises a driving part (22) arranged on the vacuum cavity (14), wherein the driving part (22) is connected with the gland (4) through a motion transmission piece (2), and the driving part (22) is used for driving the gland (4) to move along the direction of the opening end of the bottom barrel (10);
the device also comprises a sample storage table (5) arranged on the gland (4), wherein when the gland (4) is buckled on the opening end of the bottom barrel (10), the sample storage table (5) is positioned in a space surrounded by the bottom barrel (10) and the gland (4);
The vacuum chamber is characterized by further comprising a grabbing and transferring part (23) and a gate part (24) which are fixed on the vacuum chamber (14), wherein the gate part (24) is used as a channel between the closed space and the outer side of the vacuum chamber (14), and the on-off state of the channel is adjustable;
after the sample storage table (5) is moved out of the bottom barrel (10) along with the gland (4) under the action of the driving part (22), the grabbing and transferring part (23) grabs the sample on the sample storage table (5), and the grabbing and transferring part (23) transfers the grabbed sample to the outer side of the closed space through the gate part (24);
the heating device is used for heating a space surrounded by the bottom barrel (10) and the gland (4).
2. A sample pretreatment apparatus for measuring secondary electron emission characteristics of materials according to claim 1, wherein the sample storage table (5) has a columnar structure, and a plurality of slots are provided on a side surface of the sample storage table (5).
3. A sample pretreatment apparatus for measuring secondary electron emission characteristics of materials according to claim 2, wherein said driving part (22) drives said pressing cover (4) to reciprocate linearly, and said gripping and transferring part (23) drives said gripping end thereon to reciprocate linearly, and said gripping and transferring part (23) is disposed in a facing relationship with said gate part (24) on said vacuum chamber (14).
4. The sample pretreatment apparatus for measuring secondary electron emission characteristics of materials according to claim 1, wherein heat insulation layers are arranged on the bottom barrel (10) and the gland (4), and after the gland (4) is matched with the bottom barrel (10) as an opening end sealing plate of the bottom barrel (10), the heat insulation layers on the bottom barrel (10) and the gland (4) enclose a closed space, and the sample storage table (5) is positioned in the closed space.
5. The sample pretreatment device for measuring secondary electron emission characteristics of materials according to claim 1, wherein the side wall of the bottom barrel (10) is of a partition wall type structure comprising an outer barrel (11) and an inner barrel (9), the outer barrel (11) is sleeved outside the inner barrel (9), a gap is formed between the outer barrel (11) and the inner barrel (9), the side wall further comprises a water-cooling upper blocking plate (8) serving as an upper end sealing plate of the gap and a water-cooling lower blocking plate (12) serving as a lower end sealing plate of the gap, the water-cooling upper blocking plate (8), the water-cooling lower blocking plate (12), the outer barrel (11) and the inner barrel (9) form a cooling water accommodating cavity, and the sample pretreatment device further comprises a water inlet pipe (17) with one end connected with the cooling water accommodating cavity and a water outlet pipe (18) with one end connected with the cooling water accommodating cavity.
6. A material secondary electron emission characteristics measurement sample pretreatment apparatus according to claim 1, wherein the bottom barrel (10) is fixed to the vacuum chamber (14) by a plurality of rods.
7. A material secondary electron emission characteristics measurement sample pretreatment apparatus according to claim 1, wherein said heating means is an electric heating means.
8. The device for pre-processing a sample for measuring secondary electron emission characteristics of a material according to claim 1, further comprising an observation window as a local wall surface of the vacuum chamber (14), wherein the observation window is made of a light-permeable material, and the observation window is used as a detachable wall surface or an openable wall surface on the vacuum chamber (14).
9. A material secondary electron emission characteristics measurement sample pretreatment apparatus according to claim 1, further comprising a purge valve (21) mounted on the vacuum chamber (14).
10. A material secondary electron emission characteristics measurement sample pretreatment apparatus according to any of claims 1 to 9, further comprising a thermocouple (7) for measuring the temperature of the heating means.
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| CN113263757A (en) * | 2021-04-22 | 2021-08-17 | 中国科学院上海硅酸盐研究所 | Large-area thin film material ground pretreatment device and method for spaceflight |
| CN116120134A (en) * | 2022-12-13 | 2023-05-16 | 中国兵器装备集团自动化研究所有限公司 | Explosive preheating device |
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