CN112345419A - Nano bubble in-situ observation device and method - Google Patents
Nano bubble in-situ observation device and method Download PDFInfo
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- 239000002101 nanobubble Substances 0.000 title claims abstract description 75
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000000523 sample Substances 0.000 claims abstract description 110
- 239000012488 sample solution Substances 0.000 claims abstract description 24
- 239000007791 liquid phase Substances 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 238000002347 injection Methods 0.000 claims description 11
- 239000007924 injection Substances 0.000 claims description 11
- 238000005070 sampling Methods 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 238000002474 experimental method Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 230000005540 biological transmission Effects 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 230000000007 visual effect Effects 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000012544 monitoring process Methods 0.000 claims description 2
- 238000009489 vacuum treatment Methods 0.000 claims description 2
- 238000011109 contamination Methods 0.000 claims 1
- 238000000354 decomposition reaction Methods 0.000 claims 1
- 238000007781 pre-processing Methods 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- 238000002604 ultrasonography Methods 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 3
- 238000005259 measurement Methods 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 230000006399 behavior Effects 0.000 description 10
- 235000012055 fruits and vegetables Nutrition 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000009360 aquaculture Methods 0.000 description 1
- 244000144974 aquaculture Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
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- 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
- G01N15/02—Investigating particle size or size distribution
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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
- G01N23/02—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 transmitting the radiation through the material
- G01N23/04—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 transmitting the radiation through the material and forming images of the material
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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
- G01N23/225—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
- G01N23/2251—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 using incident electron beams, e.g. scanning electron microscopy [SEM]
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Abstract
The invention belongs to the technical field of micro-nano particle measurement, and discloses a nano bubble in-situ observation device and a nano bubble in-situ observation method. The device comprises a sample solution preparation system, a sample pretreatment system and an electron microscope observation system. The method visually and accurately obtains the behavior and dynamic change of the micro-nano bubbles in the liquid phase solution, makes up the defects of bubble observation by a scanning electron microscope and an atomic force microscope, and provides a new means for researching the dynamic behavior of the micro-nano bubbles.
Description
Technical Field
The invention belongs to the technical field of micro-nano particle measurement, and relates to a nano bubble in-situ observation device and a nano bubble in-situ observation method.
Background
The micro-nano bubbles are bubbles with the diameter of hundreds of nanometers to tens of micrometers. The bubbles are between micro bubbles and nano bubbles, and have physicochemical characteristics which are not possessed by the conventional bubbles. Compared with the conventional bubbles, the micro-nano bubbles have the advantages of large specific surface area, slow rising speed, high gas dissolution rate and capability of generating a large amount of free radicals. The characteristics of the micro-nano bubbles are widely applied to the aspects of aquaculture, fruit and vegetable cleaning, water environment treatment and the like: the micro-nano bubbles are used for adding oxygen into the water, so that sufficient dissolved oxygen in the water can be maintained for a long time, and the activity and the yield of aquatic products are improved; the ozone-containing nano-bubble water is used for washing the fruit and vegetable products, so that the fruit and vegetable products can be sterilized while the plant types and the original quality are maintained; dirt is removed through the low-frequency rate generated by the continuous increase and the breakage of the micro-nano bubbles in water, and the brain-enlightening is generated through stimulation, so that people feel calm and pleasure while beautifying and protecting skin. The applications are the applications of the micro-nano bubbles in actual life, and in recent years, the real state and the stabilization mechanism of the micro-nano bubbles in a micro scale have become new hot points, such as the behavior of the nano bubbles in a liquid phase environment, the living characteristics of the nano bubbles, and the like. Therefore, a method for directly observing the state of the nanobubbles in the liquid phase environment is urgently needed to be researched.
At present, micro-nano bubbles mainly act by using a scanning electron microscope and an atomic force microscope. The former can only be used for rapidly freezing a solution sample containing nano bubbles by using liquid nitrogen due to the limitation that a scanning electron microscope cannot use a liquid sample, so that the real behavior of the nano bubbles in a liquid environment can not be observed in situ, and new bubbles can be generated due to rapid freezing to influence an experiment; the latter is through the tapping mode of atomic force microscope, receive the mechanical characteristic of the bubble through the computer, the appearance of describing the bubble indirectly, this method can damage the true appearance of bubble, and have higher requirement to the sensitivity of atomic force microscope device.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and develop a nano-bubble in-situ observation device and a nano-bubble in-situ observation method, which are used for directly observing the real behavior of micro-nano bubbles in a liquid phase environment in situ. The method utilizes the characteristics that a novel sample cell capable of containing liquid and a transmission electron microscope can be amplified by thousands or even tens of thousands of times of amplification, measures the real particle size of the micro-nano bubbles in the liquid phase environment, directly observes the nano bubbles in the liquid phase environment, and can shoot the real behaviors of the micro-nano bubbles in real time. The method can effectively measure the real particle size of the micro-nano bubbles in the liquid phase environment, visually observe the liquid phase behavior of the micro-nano bubbles, make up the defect that a scanning electron microscope and an atomic force microscope cannot directly observe the behavior of the micro-nano bubbles in the liquid phase environment, and provide a more visual observation of the behavior of the micro-nano bubbles in the real liquid phase environment.
The technical scheme of the invention is as follows:
a nano-bubble in-situ observation device comprises a sample solution preparation system, a sample injection system, a sample pretreatment system and an electron microscope observation system;
the sample solution preparation system comprises a micro-nano bubble generating device, an air inlet pipeline, an air inlet control valve, a water inlet pipeline, an air inlet control valve, an air source, a sampling pipeline, a sampling control valve, a reservoir, a water outlet control valve and a water outlet pipeline; the water inlet pipeline, the water outlet pipeline and the sampling pipeline are respectively connected with the reservoir; the gas source is used for providing gas for generating bubbles; the micro-nano bubble generating device is used for preparing micro-nano bubbles; the reservoir is used for containing a liquid environment for generating nano bubbles;
the sample injection system comprises an injector, a sample injection control valve, a sample injection pipeline, a sample pool cover, a sample rod, a sample pool, a sample outlet pipeline and a sample outlet control valve, wherein the injector is used for injecting samples into the pipeline and the sample pool after absorbing the samples from the sampling pipeline; the sample rod is used for containing the sample cell, so that the sample cell is convenient to move; the sample cell cover is used for isolating the sample cell from the external environment and preventing the sample cell from being polluted; the sample cell is used for containing a sample solution; the sample introduction pipeline is used for injecting a sample solution into the sample cell; the sample outlet pipeline is used for discharging redundant samples in the sample pool and indicating that the samples successfully enter the sample pool;
the sample pretreatment system comprises a sample solution, an air extraction pipeline, an air extraction control valve and a vacuum pump, wherein the vacuum pump is used for pumping the sample cell to vacuum, so that gas release is prevented from affecting observation of an electron microscope system and damaging the electron microscope;
the electron microscope observation system comprises an electron microscope device, a data transmission line and a computer, and is used for directly acquiring related data of a sample; the computer is used for receiving signals transmitted by the electron microscope, converting the signals into images for displaying, and monitoring whether each parameter of the electron microscope is in a normal working state.
The invention has the beneficial effects that: the invention provides a nano-bubble in-situ observation device and a nano-bubble in-situ observation method. The method visually and accurately obtains the behavior and dynamic change of the micro-nano bubbles in the liquid phase solution, makes up the defects of bubble observation by a scanning electron microscope and an atomic force microscope, and provides a new means for researching the dynamic behavior of the micro-nano bubbles.
Drawings
FIG. 1 is a flow chart of the operation of the in-situ nanobubble observation device.
Fig. 2(a) is a schematic view of a sample solution preparation system.
Fig. 2(b) is a schematic diagram of a sample injection system.
FIG. 2(c) is a schematic diagram of a sample cell pretreatment system.
FIG. 2(d) is a schematic view of an electron microscope observation system.
In the figure: 1 micro-nano bubble generating device; 2 an air inlet pipeline; 3 an air inlet control valve; 4, a water inlet pipeline; 5, a water inlet control valve; 6, gas source; 7 sampling pipeline; 8 sampling control valve; 9, a water reservoir; 10, a water outlet control valve; 11 water outlet pipeline; 12 an injector; 13 a sample injection control valve; 14 sample introduction pipelines; 15 sample cell cover; 16 a sample rod; 17 a sample cell; 18 a sample outlet pipeline; 19 a sample outlet control valve; 20, sample solution; 21 an air extraction pipeline; 22 a suction control valve; 23 a vacuum pump; 24 electron microscope devices; 25 a data transmission line; 26 computer.
Detailed Description
The following detailed description of the invention refers to the accompanying drawings.
The method for observing the dynamic behavior of the micro-nano bubbles in the liquid phase environment by adopting the device comprises the following steps:
the first step is as follows: deionized water is placed in a reservoir 9, the water level can sink over a water outlet pipeline 11 of a micro-nano bubble generator 1, a water inlet control valve 5 and a water outlet control valve 10 are opened, nitrogen is used for passing through the micro-nano bubble generator 1, an air inlet control valve 3 is opened, the micro-nano bubble generator 1 is opened, the micro-nano bubble generator works normally for 10min, the operations are repeated for 3 times, impurities are prevented from being introduced into the micro-nano bubble generator 1, a water storage tank 9 and an experiment pipeline, and a micro-nano bubble solution required by an experiment is prepared;
the second step is that: taking a proper amount of sample by using an injector 12, connecting the injector 12 with a sample inlet pipeline 14 of a sample cell 17, opening a sample inlet control valve 13 and a sample outlet control valve 19, and then injecting the injector 12 properly until the end of a sample outlet pipeline 18 of the sample cell 17 has liquid drops, which indicates that the sample solution is successfully injected into the sample cell 17; the length, width and height of the sample cell are respectively 15 μm, 15 μm and 0.2 μm. The pipe diameters of the sample outlet pipeline and the sample inlet pipeline are 5 mu m, so that the sample solution is prevented from entering the sample cell at an excessive speed and damaging the sample cell.
The third step: the sample cell 17 containing the sample solution 20 obtained in the second step is placed in a vacuum pump 23 for vacuum treatment until the internal pressure of the sample cell 17 is lower than 10-5Taking the sample cell 17 out of the vacuum pump under the MPa, and placing the sample cell in an electron microscope device for observation; the electron microscope used in this example was the FEI Titan cube Themis G3300.
The fourth step: finding a window of the sample cell 17 under a low multiple, switching to observing the micro-nano bubbles under a high multiple after the micro-nano bubbles are observed in a visual field, simultaneously opening a video recording function of an electron microscope through the operation of a computer 26, recording the motion state or form change of the micro-nano bubbles in a liquid environment, and storing a video file after the shooting is finished;
the fifth step: after the experiment is finished, the sample cell 17 is taken out, deionized water is used for replacing a sample solution, the sample cell is washed according to the second step, the washing is repeated for three times, and the sample cell 17 is placed into a dust-free drying box for storage.
Claims (7)
1. A nano-bubble in-situ observation device is characterized by comprising a sample solution preparation system, a sample injection system, a sample pretreatment system and an electron microscope observation system;
the sample solution preparation system comprises a micro-nano bubble generating device (1), an air inlet pipeline (2), an air inlet control valve (3), an air inlet pipeline (4), an air inlet control valve (5), an air source (6), a sampling pipeline (7), a sampling control valve (8), a reservoir (9), a water outlet control valve (10) and a water outlet pipeline (11); the water inlet pipeline (4), the water outlet pipeline (11) and the sampling pipeline (7) are respectively connected with the reservoir (9); the gas source (6) is used for providing gas for generating bubbles; the micro-nano bubble generating device (1) is used for preparing micro-nano bubbles; the reservoir (9) is used for containing a liquid environment for generating nano bubbles;
the sample injection system comprises an injector (12), a sample injection control valve (13), a sample injection pipeline (14), a sample pool cover (15), a sample rod (16), a sample pool (17), a sample outlet pipeline (18) and a sample outlet control valve (19), wherein the injector (12) is used for injecting samples into the pipeline and the sample pool after absorbing the samples from the sampling pipeline (7); the sample rod is used for containing the sample cell, so that the sample cell is convenient to move; the sample cell cover is used for isolating the sample cell from the external environment and preventing the sample cell from being polluted; the sample cell is used for containing a sample solution; the sample introduction pipeline is used for injecting a sample solution into the sample cell; the sample outlet pipeline is used for discharging redundant samples in the sample pool and indicating that the samples successfully enter the sample pool;
the sample pretreatment system comprises a sample solution (20), an air extraction pipeline (21), an air extraction control valve (22) and a vacuum pump (23), wherein the vacuum pump is used for pumping the sample cell to vacuum so as to prevent the gas release from influencing the observation of an electron microscope system and damaging the electron microscope;
the electron microscope observation system comprises an electron microscope device (24), a data transmission line (25) and a computer (26), and is used for directly acquiring related data of a sample; the computer is used for receiving signals transmitted by the electron microscope, converting the signals into images for displaying, and monitoring whether each parameter of the electron microscope is in a normal working state.
2. The apparatus as claimed in claim 1, wherein the sample solution preparation system is capable of preparing bubbles with a particle size ranging from 90nm to 40 μm.
3. The device for in-situ observation of liquid phase behavior of micro-nano bubbles based on the transmission electron microscope as claimed in claim 1, wherein the height of the sample cell in the sample injection system is customized according to experimental working condition requirements; the pipe diameters of the sample outlet pipeline and the sample inlet pipeline are 5 mu m, so that the sample solution is prevented from entering the sample cell at an excessively high speed and damaging the sample cell.
4. The apparatus as claimed in claim 1, wherein the sample pre-processing system and the vacuum pump are capable of increasing the pressure in the sample cell to 10%-5And MPa, gas is prevented from damaging an electron microscope, and meanwhile, micro-nano bubbles are prevented from being broken due to too low internal pressure.
5. The apparatus for in-situ observation of nanobubbles according to claim 1, wherein the electron microscope is capable of being used to install a sample rod.
6. The in-situ nano-bubble observation device according to claim 2, wherein the micro-nano-bubbles generated in the sample solution preparation system can be prepared by stirring, ultrasound or rapid decomposition of hydrate, and the operation in ultra-clean environment is ensured to prevent impurity contamination.
7. The device and the method for in-situ observation of the nanobubbles according to any one of claims 1 to 6 are characterized by comprising the following steps:
the first step is as follows: deionized water is placed in a reservoir (9), the water surface height can sink a water outlet pipeline (11) of a micro-nano bubble generator (1), a water inlet control valve (5) and a water outlet control valve (10) are opened, nitrogen is used to pass through the micro-nano bubble generator (1), an air inlet control valve (3) is opened, the micro-nano bubble generator (1) is opened, the micro-nano bubble generator is enabled to normally work for more than 10min, repeated operation is carried out for at least 3 times, impurities cannot be introduced into the micro-nano bubble generator (1), the reservoir (9) and an experiment pipeline, and then a micro-nano bubble solution required by an experiment is prepared;
the second step is that: taking the prepared micro-nano bubble sample solution by using an injector (12), connecting the injector with a sample inlet pipeline (14) of a sample cell (17), opening a sample inlet control valve (13) and a sample outlet control valve (19), and injecting the injector (12) until the end of a sample outlet pipeline (18) of the sample cell (17) drops, which indicates that the sample solution is successfully injected into the sample cell (17);
the third step: putting the sample cell (17) containing the sample solution (20) obtained in the second step into a vacuum pump (23) for vacuum treatment, and pumping until the internal pressure of the sample cell (17) is lower than 10-5Taking the sample cell (17) out of the vacuum pump under the MPa, and placing the sample cell into an electron microscope device for observation;
the fourth step: finding a window of the sample cell (17) under a low multiple, switching to a high multiple to observe the micro-nano bubbles after observing the micro-nano bubbles in a visual field, simultaneously opening a video recording function of an electron microscope through the operation of a computer (26), recording the motion state or form change of the micro-nano bubbles in a liquid environment, and storing a video file after shooting is finished;
the fifth step: and after the experiment is finished, taking out the sample pool (17), replacing the sample solution with deionized water, washing the sample pool according to the second step, and storing the sample pool (17) in a dust-free drying box.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113184699A (en) * | 2021-05-19 | 2021-07-30 | 中南大学 | Generation device and observation method of interface nano bubbles |
| CN113405768A (en) * | 2021-06-16 | 2021-09-17 | 北京化工大学 | Airflow field PIV tracer particle preparation device and method based on nanobubble technology |
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Application publication date: 20210209 |