CN110987767B - Air pressure micromanipulation system and method for micron-sized particle sample - Google Patents
Air pressure micromanipulation system and method for micron-sized particle sample Download PDFInfo
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- CN110987767B CN110987767B CN201911095672.4A CN201911095672A CN110987767B CN 110987767 B CN110987767 B CN 110987767B CN 201911095672 A CN201911095672 A CN 201911095672A CN 110987767 B CN110987767 B CN 110987767B
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- 239000002245 particle Substances 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000011521 glass Substances 0.000 claims abstract description 25
- 238000003384 imaging method Methods 0.000 claims abstract description 13
- 239000007789 gas Substances 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000012546 transfer Methods 0.000 claims description 6
- 230000035485 pulse pressure Effects 0.000 claims description 5
- 239000000428 dust Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 230000001276 controlling effect Effects 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000002689 soil Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000013618 particulate matter Substances 0.000 claims description 2
- 239000011859 microparticle Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 3
- 239000011707 mineral Substances 0.000 abstract description 3
- 230000005611 electricity Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 230000003068 static effect Effects 0.000 abstract description 2
- 239000011343 solid material Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
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- 238000010249 in-situ analysis Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
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- 238000004519 manufacturing process Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/10—Investigating individual particles
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Abstract
The invention relates to an air pressure microscopic control system and method of micron-sized particle samples, wherein the method comprises the steps of fixing a hollow glass needle point on a clamping rod of a microcontroller, finding a single particle sample to be extracted on a sample table with the particle sample by using a microscope, starting a negative pressure provided by an air pressure system to capture the sample to the needle point tip, releasing the single particle sample adsorbed by static electricity by using pulse positive pressure after the sample table is replaced, and recording and controlling the whole sample moving and controlling process by using a microscopic observation and imaging system. The method is simple and efficient, has high success rate, better solves the problem of transferring and operating single particles of small-size rare samples, and is suitable for various solid materials and minerals. The system has simple structure, is easy to build, and has wide application in the fields of biology, materials, geology and planetry.
Description
[ technical field ]
The invention belongs to the field of microscopic technology of materials and mineral samples, and relates to a system and a method for air pressure microscopic manipulation of a micron-sized particle sample.
[ background art ]
Planetary and space science are receiving increasing attention. However, the size of the particulate matter, interplanetary dust particles and micrometalites samples in the near space are many on the micron scale, e.g., the interplanetary dust and micrometalites size is about 2-150 μm; the Itokawa particle samples collected by Japan falcon number are 30-180 μm, and the research of the samples has important significance for exploring the formation and evolution rule of solar system and the evolution process of planetary system. However, in-situ analysis technologies such as electron microscopy and secondary ion mass spectrometry have no way to perform analysis and test on precious micron-sized samples like conventional samples, mainly because the particle samples are small in size, and attached particles on the surface are usually in submicron level, loose and irregular in surface and difficult to clamp; and the surface layer of the sample can have a space weathering process, which occurs in the range of 200nm at the outermost layer of the sample, so that the surface structure of the sample cannot be damaged during the transfer and handling of the sample.
Aiming at the problem, two ways exist at present, one way is to directly depend on electrostatic adsorption, and the way is simple, but has the problems of uncontrollable electrostatic adsorption, uncharged particles and the like, and the extraction is not firm; and the sample is very difficult to release, and the release can be only carried out in a mode that the glass needle tip is cut off and rubbed on the sample table, so the success rate is low. The second way is the one reported by Yada team of japanese scholars to apply an applied electric field to control the adsorption and release of the sample (Yada et al, 2014). This method is to implant a minute lead in advance in the glass needle tip and the voltage is not good to control the position of release. Therefore, in order to meet the in-situ testing requirements of various micro samples, a set of more universal and more convenient air pressure micromanipulation system and method for micron-sized particle samples needs to be designed.
[ summary of the invention ]
In order to solve the above problems, the present invention overcomes the disadvantages of the prior art, and seeks to design a system and a method for air pressure micromanipulation of a universal type micron-sized particle sample by air pressure control, so as to realize convenient movement and manipulation of a single particle sample.
In order to achieve the purpose, the technical scheme of the invention is as follows: the invention relates to an air pressure micromanipulation system of a micron-sized particle sample, which comprises:
the sample table is used for placing a micron-sized particle sample;
the sample selecting device is used for selecting a single micron-sized particle sample from the micron-sized particle samples on the sample table;
an air pressure system for providing motive force for capturing and releasing the sample selection device;
the microcontroller is used for controlling the sample selection device;
the microscopic observation and imaging system is used for recording and regulating the whole process and realizing the transfer and the operation of a single micron-sized particle sample;
the sample selecting device is fixed to a clamping rod of a microcontroller, the air pressure system is connected with an air inlet at the tail of the sample selecting device, the sample table is arranged at the lower end of the sample selecting device, and the microscopic observation and imaging system is positioned above the sample selecting device.
The sample selecting device is a glass needle point, the glass needle point is hollow, and the tip of the glass needle point is wedge-shaped.
The hollow diameter of the glass needle tip is 5-20 μm.
The microscopic viewing and imaging system is a microscope.
The air pressure system comprises an air bottle, a vacuum pump, an air pressure meter, a timing circuit and a three-way valve;
the gas cylinder is connected with one of the interfaces of the three-way valve through a pipeline, the vacuum pump is connected with the other interface of the three-way valve through a pipeline, the barometer is connected with the third interface of the three-way valve and is connected with the gas inlet of the sample selecting device through a pipeline, and the timing circuit is in control connection with the three-way valve (as shown in fig. 2).
Another object of the present invention is to provide a method of using the above-mentioned operating system, wherein the method specifically comprises the following steps:
s1) placing the sample platform with the particle sample under a microscopic observation and imaging system for observation, and determining the selected particles;
s2) moving the sample selecting device to the position above the selected particles through the operation of the micro-manipulator, starting the negative pressure of the air pressure system, and moving the sample upwards to a safe area after the selected particles are captured from the sample;
s3), replacing the sample table, slowly moving the sample selection device with the selected particles to be close to the surface of the sample table, closing the negative pressure, opening the pulse positive pressure, and releasing the particle sample;
s4) moving the sample selection device with the micromanipulator and exiting.
The particle sample is a small-size and rare solid particle sample to be subjected to in-situ analysis, and the particle size of the particle sample is 10-200 mu m.
The negative pressure of the capturing in the S2) is 0.1-500 psi.
The positive pulse pressure released in the S3) is 0.3-30 psi.
And the gas source adopted by the gas pressure system in the S2) is inert gas, and the inert gas comprises nitrogen, helium or argon.
The invention has the beneficial effects that: due to the adoption of the technical scheme, the particle sample can be captured through negative pressure conveniently and quickly, and the particle sample adsorbed by static electricity is released through pulse positive pressure, so that the transfer and the operation of the particle sample are finally realized. The capturing success rate is high, and the direction and the force of the released particles are controllable. In addition, if the sample is in liquid, the sample can be easily captured into the needle tube by utilizing the capillary suction force or negative pressure of the glass needle point, and the method is also well applied to mineral separation and new material testing. The conception, the specific process, and the technical effects produced by the present invention will be further described in conjunction with the accompanying drawings to fully understand the objects, the features, and the effects of the present invention.
Drawings
FIG. 1 is a schematic structural diagram of an air pressure micromanipulation system for micro-sized particle samples according to the present invention.
FIG. 2 is a schematic diagram of the configuration of a hollow glass needle tip for use in the manipulation system of the present invention.
Fig. 3 is a schematic view of the structure of the pneumatic system of the present invention.
Fig. 4 is a simulated lunar soil particle to be used for test sample movement in the present invention.
Fig. 5 is an image of a sample after movement in the present invention.
FIG. 6 is a diagram of another sample of the present invention placed precisely adjacent to the particle of FIG. 4.
In the figure:
1 microscopic observation and imaging system; 2, a pneumatic system; 3, a glass needle point; 4, a microcontroller; 5, moving the sample stage; 6 particle samples, 2-1 inert gas cylinders, 2-2 vacuum pumps, 2-3 barometers, 2-4 timing circuits and 2-5 three-way valves.
Detailed Description
This is further illustrated by way of example in conjunction with the accompanying drawings.
As shown in fig. 1, the present invention relates to a system for air pressure micromanipulation of a micrometer-sized particle sample, comprising:
the sample table is used for placing a micron-sized particle sample;
the sample selecting device is used for selecting a single micron-sized particle sample from the micron-sized particle samples on the sample table;
an air pressure system for providing motive force for capturing and releasing the sample selection device;
the microcontroller is used for controlling the sample selection device;
the microscopic observation and imaging system is used for recording and regulating the whole process and realizing the transfer and the operation of a single micron-sized particle sample;
the sample selecting device is fixed to a clamping rod of a microcontroller, the air pressure system is connected with an air inlet at the tail of the sample selecting device, the sample table is arranged at the lower end of the sample selecting device, and the microscopic observation and imaging system is positioned above the sample selecting device.
The sample selecting device is a glass needle point, the glass needle point is hollow, and the tip of the glass needle point is wedge-shaped.
The hollow diameter of the glass needle tip is 5-20 μm.
The microscopic viewing and imaging system is a microscope.
The air pressure system comprises an air bottle, a vacuum pump, an air pressure meter, a timing circuit and a three-way valve;
the gas cylinder is connected with one of the interfaces of the three-way valve through a pipeline, the vacuum pump is connected with the other interface of the three-way valve through a pipeline, the barometer is connected with the third interface of the three-way valve and is connected with the gas inlet of the sample selecting device through a pipeline, and the timing circuit is in control connection with the three-way valve (as shown in fig. 2).
Another object of the present invention is to provide a method of using the above-mentioned operating system, wherein the method specifically comprises the following steps:
s1) placing the sample platform with the particle sample under a microscopic observation and imaging system for observation, and determining the selected particles;
s2) moving the sample selecting device to the position above the selected particles through the operation of the micro-manipulator, starting the negative pressure of the air pressure system, and moving the sample upwards to a safe area after the selected particles are captured from the sample;
s3), replacing the sample table, slowly moving the sample selection device with the selected particles to be close to the surface of the sample table, closing the negative pressure, opening the pulse positive pressure, and releasing the particle sample;
s4) moving the sample selection device with the micromanipulator and exiting.
The particle sample is a small-size and rare solid particle sample to be subjected to in-situ analysis, and the particle size of the particle sample is 10-200 mu m.
The negative pressure of the capturing in the S2) is 0.1-500 psi.
The positive pulse pressure released in the step S3) is 0.3-30 psi.
And the gas source adopted by the gas pressure system in the S2) is inert gas, and the inert gas comprises nitrogen, helium or argon.
Example (b):
the method specifically comprises the following steps (the attached figures 4-6 are video screenshots):
step 2, manufacturing a hollow needle tip by using a glass needle tip drawing instrument (as shown in figure 2);
and 4, step 4: moving the sample stage to another position, slowly enabling the glass needle tip to be close to the sample stage by using a microcontroller, when an observation system sees that the glass needle tip gradually focuses and is clearly close to the sample stage, closing an air pressure system to pump air, starting pulse positive pressure to spray nitrogen, setting the pressure to be 0.5psi in advance, and setting the pulse time to be about 100ms, so that the particle sample is released onto the sample stage (as shown in figure 5);
and 5: in order to test repeatability, a plurality of particle samples (22-83 μm) with different sizes are transferred by steps 2 and 3 respectively around the sample (a dashed box in FIG. 6) and are placed in the vicinity of the sample stably to form a triangle (as shown in FIG. 6), and the reliability of the method is proved.
The tip of the glass needle in step 3 is ground in advance to form a wedge shape so as to easily adsorb and release the sample, and the hollow diameter is about 15 μm.
The pulse pressure in step 4 should not be too large, so as to prevent the sample from releasing too far.
The sample stage in the step 4 can be replaced by other sample stages, for example, a standard aluminum-based nail-type sample stage combined with a scanning electron microscope, then the sample is placed and numbered, and the study on the appearance, the components and the isotopes of single particles can be carried out at the later stage.
The above description is only a preferred embodiment of the present invention, and the present invention is not limited to the above embodiment. The atmospheric pressure micromanipulation system and method of micron order granule sample described in this embodiment, its overall step is relatively simple, and the practicality is good, especially solved small-scale, rare sample can receive good effect when can not be handled with other modes, made up for prior art's not enough.
Claims (4)
1. A method for air pressure micromanipulation of micron-sized particle samples, which is suitable for the transfer and manipulation of near space particulate matter, interplanetary dust particles or micrometallite samples, and a manipulation system for realizing the method comprises:
a sample table for placing a particle sample;
the sample selecting device is used for selecting single particle samples from the microparticle samples on the sample stage;
the air pressure system is used for providing power for the sample selecting device, capturing negative pressure for particles and releasing positive pulse pressure for particles;
the microcontroller is used for controlling the sample selection device;
the microscopic observation and imaging system is used for recording and regulating the whole process and realizing the transfer and the operation of a single micron-sized particle sample;
the method comprises the following steps of:
s1) placing the sample platform with the solid particle sample under a microscopic observation and imaging system for observation, and determining the selected single particle sample;
s2) moving the sample selecting device to the position above the selected particles through the operation of the micro-manipulator, starting the negative pressure of the air pressure system, and moving the sample upwards to a safe area after the selected particles are captured from the sample; the captured negative pressure is 0.1-500 psi;
s3) replacing the sample stage, slowly moving the sample selection device with the selected particles to approach the surface of the sample stage, closing the negative pressure, starting the pulse positive pressure, wherein the pulse time is 100ms, and releasing the particle sample; the released positive pulse pressure is 0.3-30 psi;
s4) moving the sample selection device with the micromanipulator and exiting;
the air pressure system comprises an air bottle, a vacuum pump, an air pressure meter, a timing circuit and a three-way valve;
the gas cylinder is connected with one interface of the three-way valve through a pipeline, the vacuum pump is connected with the other interface of the three-way valve through a pipeline, the barometer is connected with the third interface of the three-way valve and is connected with the gas inlet of the sample selecting device through a pipeline, and the timing circuit is in control connection with the three-way valve;
the sample selecting device is a glass needle point, the interior of the glass needle point is hollow, the diameter of the glass needle point is 5-20 mu m, and the tip of the glass needle point is wedge-shaped.
2. The method of claim 1, wherein the microscopic viewing and imaging system is a microscope.
3. The method as claimed in claim 1, wherein the S1) particle sample is micron-sized particle substances such as lunar soil and interplanetary dust which can not contact water and can not destroy the surface structure, and the particle size is 10-200 μm.
4. The method as claimed in claim 1, wherein the gas source used in the gas pressure system in S2) is an inert gas, and the inert gas comprises nitrogen, helium or argon.
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| CN111537192A (en) * | 2020-05-22 | 2020-08-14 | 中国计量大学 | Particle release device with precise timing and spatial positioning |
| CN114279907B (en) * | 2021-12-14 | 2022-11-15 | 中国科学院地质与地球物理研究所 | Nondestructive screening system and method for lunar dust particle sample |
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| CN105911686A (en) * | 2016-06-21 | 2016-08-31 | 浙江大学 | Improved micro suction pipe processing system based on optical microscope |
| CN107649226A (en) * | 2017-09-21 | 2018-02-02 | 上海大学 | A kind of preparation method of micro pipette and micro pipette |
| CN107941832B (en) * | 2017-10-26 | 2019-01-25 | 中国科学院地质与地球物理研究所 | A kind of preparation method of micron order pre solar grain transmission electron microscope sample |
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