CN108956227A - A kind of preparation method of the liquid nanometer particulate samples for transmission electron microscope analysis - Google Patents
A kind of preparation method of the liquid nanometer particulate samples for transmission electron microscope analysis Download PDFInfo
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- CN108956227A CN108956227A CN201810715754.3A CN201810715754A CN108956227A CN 108956227 A CN108956227 A CN 108956227A CN 201810715754 A CN201810715754 A CN 201810715754A CN 108956227 A CN108956227 A CN 108956227A
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- sample
- electron microscope
- transmission electron
- liquid
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
- G01Q30/20—Sample handling devices or methods
Abstract
The present invention provides a kind of preparation methods of liquid nanometer particulate samples for transmission electron microscope analysis, comprising the following steps: fluid sample collected is placed in clean polyethylene bottle by step 1)；Step 2 jiggles polyethylene bottle, so that nanoparticle is rocked to being uniformly distributed in liquid medium；Step 3) is immersed in testing liquid sample with the avris that clean tweezers clamp transmission electron microscope carrier net, so that liquid is flooded support grid, and the low speed of certain frequency is kept to shake, and continue 30~40 minutes or so；Support grid is taken out after step 4) step 3) is placed in natural air drying in the vessel of sealing；Support grid after air-drying is sequentially placed into clean sample box by step 5) by the number of sample；Step 6) closes the lid the sample all made, prepares examination with computer.
Description
Technical field
The present invention relates to a kind of transmission electron microscope (Transmission Electron Microscopy, i.e. TEM) samples
Preparation method, more particularly, to a kind of preparation method of liquid nanometer particulate samples for transmission electron microscope analysis, the present invention can
It is related to the field of liquid nanometer sample preparation applied to geoscience, material science, medicine, chemistry, physics etc., is especially applied to
Look for mine field.
Background technique
With the development of nanoparticle precision research, observation and understand the structure of nanoparticle in liquid medium, ingredient,
Form, aggregation characteristic etc. have become component part indispensable in nano science area research, at present for nanoparticle
In observation, transmission electron microscope is essential tool；For fluid sample, the preparation of TEM sample is for nanoparticle
Tem observation is most important, and the preparation process of the nanoparticle TEM sample in conventional liq medium generally comprises the steps: using
Liquid-transfering gun pipette samples are dripped in the support grid of transmission electron microscope, are adsorbed in the nanoparticle in fluid sample in support grid, and stand
2-10 minutes, etc. after support grids fully absorb, sop up moisture extra in support grid with clean filter paper, after natural air drying, use tweezers
It is put in the clean sample box for being covered with clean filter paper, closeing the lid and being put into drying box is dried for standby.
The technology of preparing of conventional liquid nanometer particle TEM sample has a defect, for the physical of sample to be measured
Matter has certain requirement, and generally requiring sample to be tested is the lesser liquid of viscosity, in order to be drawn and titrated with liquid-transfering gun；In reality
In the process of scientific research of border, in order to understand the structure microscopic feature and constituent content feature of a certain based fine particles, sample is tended not to arbitrarily
Change and processing, therefore the technology of preparing restricted application of conventional liquid nanometer particle TEM sample there is no preferable at present
Solution needs a kind of simplicity, strong operability, the technology of preparing of liquid nanometer particle TEM sample applied widely.
Summary of the invention
In view of this, the main object of the present invention is to provide a kind of liquid nanometer particulate samples for transmission electron microscope analysis
Preparation method.
The technical solution adopted by the present invention is that:
A kind of preparation method of the liquid nanometer particulate samples for transmission electron microscope analysis, comprising the following steps:
Fluid sample collected is placed in clean polyethylene bottle by step 1)；
Step 2 jiggles polyethylene bottle, so that nanoparticle is rocked to being uniformly distributed in liquid medium；
Step 3) is immersed in testing liquid sample with the avris that clean tweezers clamp transmission electron microscope carrier net, and liquid is made to flood support grid,
And the low speed of certain frequency is kept to shake, and continue 30~40 minutes or so；
Support grid is taken out after step 4) step 3) is placed in natural air drying in the vessel of sealing；
Support grid after air-drying is sequentially placed into clean sample box by step 5) by the number of sample；
Step 6) closes the lid the sample all made, prepares examination with computer.
Liquid sample can be the natural water body of acquisition in step (1), or the solution manually prepared, it is unlimited
It can be the sample containing nanoparticle of any liquid in aqueous solution.
Transmission electron microscope carrier net is clamped with clean tweezers or any clean tool for playing clamping action described in step (3)
Edge.
The transmission electron microscope carrier net includes one of copper mesh, molybdenum net, golden net, titanium net, nickel screen, copper mesh and palladium net.
Transmission electron microscope carrier net is clamped using tweezers described in step (3), and the low of certain frequency is kept in testing liquid sample
Speed is shaken, and can also can use mechanically actuated with the same function with manual operation.
The time that transmission electron microscope carrier net keeps the low speed of certain frequency to shake in testing liquid sample is clamped using tweezers to answer
Guarantee at 30~40 minutes, so that particle is contacted with transmission electron microscope carrier net and is adsorbed on above.
In step 5), if persistently to carry out sample preparation using tweezers, need before making next sample with ultrapure
Water cleans tweezers 2~3 times to avoid sample pollution.
The invention has the following advantages that
The technology of preparing of liquid nanometer particle TEM sample by adopting the above technical scheme, the present invention is in conventional water nanoparticle
On the basis of TEM sample sample preparation, the method for adsorbing nanoparticle by improving support grid, modification optimizes conventional sample preparation process, by former
Drop in support grid passive adsorption nanoparticle be optimized for using support grid actively obtain, absorption nanoparticle.The method of the present invention solution
Conventional water nanoparticle TEM sample method for making sample of having determined is unable to satisfy the sample sample preparation demand of viscosity higher, and then can not be direct
The problem of observation analysis is carried out to features such as the ultra microstructures of nanoparticle to liquid contained by it.In addition, method of the invention
It operates simple and easy, it is low in cost, there is very big potential application foreground.
Detailed description of the invention
Fig. 1 is the leaded particle transmission electron microscope shape appearance figure of underground water.
Specific embodiment
Below in conjunction with attached drawing and specific embodiment, the present invention will be described in detail, herein illustrative examples of the invention
And explanation is used to explain the present invention, but not as a limitation of the invention.
Referring to Fig.1, for this purpose, the invention discloses a kind of preparations of liquid nanometer particulate samples for transmission electron microscope analysis
Method, comprising the following steps:
Fluid sample collected is placed in clean polyethylene bottle by step 1)；
Step 2 jiggles polyethylene bottle, so that nanoparticle is rocked to being uniformly distributed in liquid medium；
Step 3) is immersed in testing liquid sample with the avris that clean tweezers clamp transmission electron microscope carrier net, and liquid is made to flood support grid,
And the low speed of certain frequency is kept to shake, and continue 30~40 minutes or so；
Support grid is taken out after step 4) step 3) is placed in natural air drying in the vessel of sealing；
Support grid after air-drying is sequentially placed into clean sample box by step 5) by the number of sample；
Step 6) closes the lid the sample all made, prepares examination with computer, the parameters of Electronic Speculum are as follows: ceiling voltage
200kv, point resolution 0.23nm, lattice resolution 0.14nm, amplification factor x2000-x1500000.
Liquid sample can be the natural water body of acquisition in step (1), or the solution manually prepared, it is unlimited
It can be the sample containing nanoparticle of any liquid in aqueous solution.
Transmission electron microscope carrier net is clamped with clean tweezers or any clean tool for playing clamping action described in step (3)
Edge.
The transmission electron microscope carrier net includes one of copper mesh, molybdenum net, golden net, titanium net, nickel screen, copper mesh and palladium net.
Transmission electron microscope carrier net is clamped using tweezers described in step (3), and the low of certain frequency is kept in testing liquid sample
Speed is shaken, and can also can use mechanically actuated with the same function with manual operation.
The time that transmission electron microscope carrier net keeps the low speed of certain frequency to shake in testing liquid sample is clamped using tweezers to answer
Guarantee at 30~40 minutes, so that particle is contacted with transmission electron microscope carrier net and is adsorbed on above.
In step 5), if persistently to carry out sample preparation using tweezers, need before making next sample with ultrapure
Water cleans tweezers 2~3 times to avoid sample pollution.
The present invention is discussed further with reference to embodiments.
Embodiment 1 is lead-zinc deposit underground water particle method for preparing transmission electron microscopy, specific steps are as follows:
1, the water sample of field acquisition is taken out, is placed in clean polyethylene bottle；
2, polyethylene bottle is jiggled, avoids caused by standing because of water sample being unevenly distributed for nanoparticle in liquid medium；
3, being immersed with the avris (avoiding the grid of nickel screen by breakage) that clean tweezers clamp nickel screen in the water sample of acquisition (makes water
Do not cross nickel screen) and the low speed of certain frequency is kept to shake, and continue 30-40 minutes or so；
4, it after the time reaches, takes out support grid and is placed in natural air drying in the vessel of sealing；
5, the nickel screen after air-drying is sequentially placed into clean sample box by the number of sample, will be used before production sample every time super
Pure water cleans tweezers 2-3 times to avoid sample pollution；
6, the sample all made is closed the lid, prepares examination with computer.
Sample analysis:
After the completion of the processing and preparation work of groundwater sample, nickel screen is all made of the 200kv transmission electricity of test center of Zhongshan University
Mirror carries out observation analysis.The model of transmission electron microscope is JEM-2010HR, the parameters of Electronic Speculum are as follows: ceiling voltage 200kv, point minute
Resolution 0.23nm, lattice resolution 0.14nm, amplification factor x2000-x1500000.
As a result:
By analyzing metalliferous deposit underground water particulate samples, here it is apparent that the wherein pattern and ingredient of nanoparticle
Feature.
Attached drawing 1 is the leaded particle transmission electron microscope shape appearance figure of lead-zinc deposit underground water.
Table 1 is the element composition ratio of this particle.
The EDS of the leaded elementary particle of table 1 analyzes result
Conclusion:
It, can be well from testing liquid using the nanoparticle method for making sample disclosed in this invention for transmission electron microscope analysis
Middle extraction nanoparticle, carrying out transmission electron microscope analysis can be derived that ideal as a result, enormously simplifying sample making course, improve system
The accurate analysis to nanoparticle may be implemented in sample efficiency, can satisfy actual transmission electron microscope analysis needs.
Technical solution disclosed in the embodiment of the present invention is described in detail above, specific implementation used herein
Example is expounded the principle and embodiment of the embodiment of the present invention, and the explanation of above embodiments is only applicable to help to understand
The principle of the embodiment of the present invention；At the same time, for those skilled in the art is being embodied according to an embodiment of the present invention
There will be changes in mode and application range, in conclusion the content of the present specification should not be construed as to limit of the invention
System.
Claims (7)
1. a kind of preparation method of the liquid nanometer particulate samples for transmission electron microscope analysis, it is characterised in that: including following step
It is rapid:
Fluid sample collected is placed in clean polyethylene bottle by step 1)；
Step 2 jiggles polyethylene bottle, so that nanoparticle is rocked to being uniformly distributed in liquid medium；
Step 3) is immersed in testing liquid sample with the avris that clean tweezers clamp transmission electron microscope carrier net, and liquid is made to flood support grid,
And the low speed of certain frequency is kept to shake, and continue 30~40 minutes or so；
Support grid is taken out after step 4) step 3) is placed in natural air drying in the vessel of sealing；
Support grid after air-drying is sequentially placed into clean sample box by step 5) by the number of sample；
Step 6) closes the lid the sample all made, prepares examination with computer.
2. the preparation method of the liquid nanometer particulate samples according to claim 1 for transmission electron microscope analysis, feature
Be: liquid sample can be the natural water body of acquisition in step (1), or the solution manually prepared is not limited to
Aqueous solution can be the sample containing nanoparticle of any liquid.
3. the preparation method of the liquid nanometer particulate samples according to claim 1 for transmission electron microscope analysis, feature
It is: clamps transmission electron microscope carrier net with clean tweezers or any clean tool for playing clamping action described in step (3)
Edge.
4. the preparation method of the liquid nanometer particulate samples according to claim 1 for transmission electron microscope analysis, feature
Be: the transmission electron microscope carrier net includes one of copper mesh, molybdenum net, golden net, titanium net, nickel screen, copper mesh and palladium net.
5. the preparation method of the liquid nanometer particulate samples according to claim 1 for transmission electron microscope analysis, feature
It is: clamps the low speed that transmission electron microscope carrier net keeps certain frequency in testing liquid sample using tweezers described in step (3)
It shakes, can also can use mechanically actuated with the same function with manual operation.
6. the preparation method for the liquid nanometer particulate samples of transmission electron microscope analysis according to claim 1 or 5, special
Sign is: clamping the time that transmission electron microscope carrier net keeps the low speed of certain frequency to shake in testing liquid sample using tweezers should protect
Card was at 30~40 minutes, so that particle is contacted with transmission electron microscope carrier net and is adsorbed on above.
7. the preparation method of the liquid nanometer particulate samples according to claim 1 for transmission electron microscope analysis, feature
It is: in step 5), if persistently to carry out sample preparation using tweezers, needs clear with ultrapure water before making next sample
Tweezers are washed 2~3 times to avoid sample pollution.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111257352A (en) * | 2020-02-18 | 2020-06-09 | 中山大学 | Method for predicting blind deposit by using chemical composition data of single nano particles |
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| CN101988874A (en) * | 2009-07-31 | 2011-03-23 | 鸿富锦精密工业（深圳）有限公司 | Preparation method of transmission electron microscope specimen |
| CN102507285A (en) * | 2011-11-14 | 2012-06-20 | 上海大学 | Preparation method of transmission electron microscope sample for detecting second phase particles in alloy |
| CN102735509A (en) * | 2012-06-20 | 2012-10-17 | 大连大学 | Preparation method of transmission electron microscope observation sample of magnetic liquid in magnetic field |
| CN104181175A (en) * | 2014-07-18 | 2014-12-03 | 中山大学 | Water particle geochemical prospecting method and application thereof |
| CN104330422A (en) * | 2014-07-18 | 2015-02-04 | 广州市地质调查院 | Method for discriminating seawater intrusion through micro-particle analysis |
| CN104897452A (en) * | 2015-06-30 | 2015-09-09 | 东南大学 | Production method of transmission electron microscope sample |
-
2018
- 2018-07-03 CN CN201810715754.3A patent/CN108956227A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101988874A (en) * | 2009-07-31 | 2011-03-23 | 鸿富锦精密工业（深圳）有限公司 | Preparation method of transmission electron microscope specimen |
| CN102507285A (en) * | 2011-11-14 | 2012-06-20 | 上海大学 | Preparation method of transmission electron microscope sample for detecting second phase particles in alloy |
| CN102735509A (en) * | 2012-06-20 | 2012-10-17 | 大连大学 | Preparation method of transmission electron microscope observation sample of magnetic liquid in magnetic field |
| CN104181175A (en) * | 2014-07-18 | 2014-12-03 | 中山大学 | Water particle geochemical prospecting method and application thereof |
| CN104330422A (en) * | 2014-07-18 | 2015-02-04 | 广州市地质调查院 | Method for discriminating seawater intrusion through micro-particle analysis |
| CN104897452A (en) * | 2015-06-30 | 2015-09-09 | 东南大学 | Production method of transmission electron microscope sample |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111257352A (en) * | 2020-02-18 | 2020-06-09 | 中山大学 | Method for predicting blind deposit by using chemical composition data of single nano particles |
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Application publication date: 20181207 |