CN109799253A - A method of two samples are loaded based on transmission electron microscope common sample platform simultaneously - Google Patents
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Abstract
The invention belongs to transmission electronic microscope technology fields, disclose a kind of method based on two samples of transmission electron microscope common sample platform while loading, according to the different characteristics of pre-detection material, select suitable TEM to support film support grid, and routinely the preparation method of powder sample disperse powder sample in support it is to be measured in support grid；The support grid for having prepared sample is cut in half with blade；And to two samples of well cutting, using homemade TEM sample transfer tool, two samples are transferred to the left and right or upper and lower two sides of sample stage respectively, and record corresponding position；Sample stage is put into TEM, is tested after vacuum reaches test request.The present invention is effectively reduced the number that TEM is varied, reduce vary and vacuum wait time consumption, improve testing efficiency, reduce testing cost；It is beneficial to stabilization of the sample in Electronic Speculum, to facilitate the acquisition of full resolution pricture；It is also advantageous for the stable operation and maintenance of instrument and equipment.
Description
Technical field
The invention belongs to transmission electronic microscope technology field, more particularly to one kind are same based on transmission electron microscope common sample platform
When load two samples method.
Background technique
Currently, the prior art commonly used in the trade is such that
Transmission electron microscope (abbreviation TEM) is can to provide microstructure, structure, ingredient for various micro-, sized materials of receiving
Etc. information, because due to be widely used in numerous ambits such as material, physics, chemistry, biology, information, geology, space flight,
Greatly push the development of nanosecond science and technology.The continuous renewal of TEM technology, the reduction of cost and country with the development of science and technology
Attention to science and technology, domestic colleges and universities and scientific research institutions TEM are more and more in recent years.It is with spherical aberration correction transmission electron microscope
Example, domestic quantity of possessing has reached more than 100 at present.Number of devices quicklys increase, and brings Gospel for scientific research personnel, if
It is standby reservation, quick using relatively convenient is become, test value also relative reduction.However, relative to scientific research personnel increase and
The growth of bring novel nano-material needs test sample quantity to sharply increase to anxiety still aobvious when TEM test machine, in advance
One, it is still ordinary affair that two weeks even carry out reservation for more time.
Transmission electron microscope replaces sample, had both increased sample stage angle measurement as high-vacuum equipment, frequent (usually less than 30min)
The risk of platform and Vacuum ball valve damage etc., is unfavorable for the stable operation and maintenance of equipment.On the other hand, replacement sample needs to spend
Regular hour (time that the product oil (gas) filling device of varying vacuumizes is usually 5-10min), so then increase the time cost of test.
In addition, the drift velocity that sample has just been placed into its sample after transmission electron microscope is very fast, and it is unfavorable for the microstructure of sample, knot of tissue
The acquisition of the observation of structure, especially high-resolution (atomic lattice) image, and pass through the stabilization of certain time (it is generally necessary to a few minutes
Or it is longer, according to different equipment, environment and the technology of operator), it can reach preferable test request.To sum up, it is desirable to obtain
Satisfied test result is obtained, generally requires to spend additional time, if so can be reduced the number of sample replacement, i.e., is once varied
Multiple samples, which can be placed, then can effectively improve testing efficiency, reduce testing cost.
In this context, various grade sample stage comes into being, and 5 sample stages of such as original Gatan company (once can be same
When be put into 5 samples), so once can then be put into multiple samples, to improve testing efficiency, and greatly reduce test
Cost.However, one side multidigit sample stage non-standard configuration, thus high price is needed to purchase again；Another aspect multidigit sample
Platform is limited to transmission electron microscope objective pole shoe space itself, and multiplicity sample platform only has the function of uniclinal at present, thus for requiring to incline
The case where turning different tape spools and carrying out structural analysis is then unable to satisfy requirement.
In conclusion problem of the existing technology is:
(1) prior art transmission electron microscope common sample platform is when carrying out powder sample test, because test content is relatively simple
It is single, the time is shorter and generally requires frequently replace sample, thus increase time (the frequent time for replacing sample) of test at
This；Simultaneously also increase the damage of components such as sample stage angle measurement platform and Vacuum ball valve risk, be unfavorable for equipment stable operation and
Maintenance；
(2) multidigit sample stage only has the function of uniclinal at present, thus carries out structure for requiring to vert different tape spools
The case where analysis, is then unable to satisfy requirement.
Solve the difficulty and meaning of above-mentioned technical problem:
(1) difficulty: wanting to solve transmission electron microscope common sample platform, once to place multiple samples to be measured and retain sample stage
Double functions of inclining, will be faced with the problem of transmission electron microscope sample table and objective pole shoe narrow space first, if by increasing sample stage
Length and obtain more sample bit spaces, then will lose double functions of inclining of sample, i.e., multidigit sample is difficult to functions of pair inclining
It gets both.
(2) meaning for solving above technical problem is, (e.g., double to incline, heat in the original basic function for guaranteeing sample stage
Deng) in the case where, realization once loads multiple (2 or more) samples, it will help mentions under the premise of guaranteeing test effect
The testing efficiency of highly transmissive Electronic Speculum reduces testing time and economic cost；It is beneficial to user to obtain more data and accelerate
The process of scientific research, work.
Summary of the invention
In view of the problems of the existing technology, the present invention provides one kind is loaded simultaneously based on transmission electron microscope common sample platform
The method of two samples.
The invention is realized in this way a method of two samples are loaded based on transmission electron microscope common sample platform simultaneously,
Specifically includes the following steps:
Step 1: according to the different characteristics of pre-detection material, suitable TEM is selected to support film support grid, and routinely powder
The preparation method of sample disperses powder sample in be measured in support support grid；
Step 2: the support grid for having prepared sample is cut in half with blade, and to two samples of well cutting, is remembered respectively
Record is 1#, 2#；
Step 3: homemade TEM sample transfer tool is utilized, two samples of 1#, 2# are transferred to a left side for sample stage respectively
Two sides (as depicted in figure 3 a) under right or up, and record corresponding position；
Step 4: being put into TEM for sample stage, is tested after vacuum reaches test request.
Further, in step 1, film support grid diameter 3mm.
Further, in step 1, powder sample is nano particle, nano wire, nanometer sheet etc..
Further, support grid is prevented plowing from step 2, in cutting process supports film.
Further, in step 2, to two samples of well cutting, it is recorded as 1#, 2# respectively.
Further, in step 3, in the self-made tool, that is, transmission electron microscope field operator more generally use based on
Infusion niidl is polished and manufactured tool；Tool transfer sample is simple, convenient and is hardly damaged sample；It is shifting
In the process, do not recommend, but still the common transfer for loading sample and carrying out sample with fine tweezers can be used.
Further, in step 4, when test, according to the position of 1#, 2# actual load, corresponding region is found；In this way, complete
At the test that can directly carry out another sample after the test of a sample.
In conclusion advantages of the present invention and good effect are as follows:
This transmission electron microscope sample stowage has inexpensive, safe and reliable, convenient, flexible and applied widely, high-efficient
And the features such as being conducive to the management operating of equipment.Now it is briefly described as follows:
Low cost: in the present invention, without spend sample stage or ancillary equipment purchase or recondition expense, only need to prepare to cut
The blade of support grid is cut, it is usually all very cheap, and can be used for multiple times.In addition, if preparing sample again after support grid is divided into two,
A support grid originally can then be used twice, to reduce the expense of support grid consumptive material.
Safe and reliable: TEM standard sample support grid is that the disk of diameter 3mm still ensures that after being cut in half along support grid
Close to 3mm, annulus periphery has sample stage to support and is compacted by pressure ring the long side of support grid, therefore sample can guarantee surely in Electronic Speculum
Fixed and safety, there is no the danger that sample falls off.Theoretically, repeated segmentation can be carried out to sample support grid, for example is cut into 3
It is a, but on the one hand in view of be divided after support grid area become smaller and influence sample preparation effect and effective viewing area, another party
Face is in view of stability of the sample on sample stage and there is the danger to fall off, therefore it is not recommended that is divided is smaller.
Applied widely: this method is suitable for powdery type sample, is suitable for various samples platform and different Electronic Speculum, and retain
Sample stage original function.It is placed in and double inclines on platform, it can be achieved that the two-way of sample is verted；It is placed in multidigit (such as 5) sample
Platform then once places the sample of double amount (10).In fact, a kind of circumference TEM support grid of copper mesh and of the invention of being called
Starting point is similar.But it in contrast, the present invention is more practical, and has the following advantages that.First, the present invention be suitable for it is various not
With the support grid (such as carbon net, micro-grid etc.) for supporting film, it is not required to especially purchase or customize different support film circumference copper mesh and increase warp
Ji and time cost.Second, according to the actual situation, practical sample preparation can be selected complete support support grid prepare sample laggard
Row cutting so guarantees that sample in the central distribution of sample stage viewing area, is conducive to the experiment test in later period；And have an area of copper mesh
It is semicircle copper mesh, and the sample of dispersion is easier to edge region, may will affect the effect of later period test.Certainly, have an area of copper
Net more easily discriminates sample, but is simultaneously non-fully not required to label sample, at least in sample preparation still needs to that sample is marked；And at this
It in invention, only need to be marked then that there is no mistakes to sample in cutting and loading, therefore can be kept away as long as slightly careful
Exempt from obscuring for sample.
Efficient: the present invention can effectively improve TEM testing efficiency.The primary sample size that loads is doubled, is reduced
Half varies the time, and the quantity for improving daily test sample reduces single sample test composition；It is opposite simultaneously to extend
The time interval of replacement sample is conducive to the holding of TEM high vacuum and then facilitates the maintenance of equipment state.
Method provided by the invention may be implemented once to load two samples.The present invention passes through to the various support support grids of TEM
It carries out to hemisect, and the semicircle support grid of two well cuttings is placed in the specific bit of sample stage by cleverly branch mode
It sets.This method is effectively reduced the number that TEM is varied, reduce vary and vacuum wait time consumption, improve test
Efficiency reduces testing cost；It is beneficial to stabilization of the sample in Electronic Speculum, to facilitate the acquisition of full resolution pricture；Also have
Beneficial to the stable operation of instrument and equipment.
By taking this center as an example, to avoid frequently varying situations such as causing equipment vacuum state to be deteriorated in daily test, rule
Fixed replacement sample room every time is usually 4-5 every the sample test amount not less than 40 minutes, such a whole morning, and uses this method
Afterwards, sample test amount can increase to 6-10.For most of feelings for being only concerned the information such as material morphology, partial size, component distributing
Condition varies interval in 40 minutes, if only observing 1 sample often seems more wasteful, and once tests 2 samples, then when
Between it is relatively reasonable, cost reduces nearly half accordingly.
Detailed description of the invention
Fig. 1 is the method stream provided in an embodiment of the present invention based on two samples of transmission electron microscope common sample platform while loading
Cheng Tu.
Fig. 2 is copper mesh cutting provided in an embodiment of the present invention and cutting scalpel.
Fig. 3 is the position that sample provided in an embodiment of the present invention is loaded on sample stage and label schematic diagram.
Fig. 4 is the result schematic diagram of TEM actual observation provided in an embodiment of the present invention.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Application principle of the invention is described in detail with reference to the accompanying drawing；
As shown in Figure 1, provided in an embodiment of the present invention load two samples based on transmission electron microscope common sample platform simultaneously
Method, specifically includes the following steps:
S101: according to the different characteristics of pre-detection material, suitable TEM is selected to support film support grid, and routinely powder-like
The preparation method of product disperses powder sample in be measured in support support grid；
S102: the support grid for having prepared sample is cut in half with blade, and to two samples of well cutting, is recorded respectively
For 1#, 2#；
S103: homemade TEM sample transfer tool is utilized, two samples of 1#, 2# are transferred to the left and right of sample stage respectively
Or upper and lower two sides, and record corresponding position；
S104: being put into TEM for sample stage, is tested after vacuum reaches test request.
In step S101, film support grid diameter 3mm provided in an embodiment of the present invention.
In step S101, powder sample provided in an embodiment of the present invention is nano particle, nano wire, nanometer sheet etc..
In step S101, support film is not scratched in cutting process provided in an embodiment of the present invention.
In step S102, two samples provided in an embodiment of the present invention to well cutting are recorded as 1#, 2# respectively.
In step S104, when test provided in an embodiment of the present invention, according to the position of 1#, 2# actual load, finds and correspond to
Region；In this way, can directly carry out the test of another sample after the test of one sample of completion.
Application principle of the invention is further described combined with specific embodiments below；
Embodiment 1；
Specific embodiments of the present invention are as follows:
(1) according to the different characteristics of pre-detection material, suitable TEM is selected to support film support grid (diameter 3mm), and routinely
The preparation method of powder sample is to be measured in support grid in supporting by powder (nano particle, nano wire, nanometer sheet etc.) sample dispersion；
(2) support grid for having prepared sample is cut in half with blade；It is careful not to scratch in cutting process and supports film, with
Exempt to influence observation.And to two samples of well cutting, it is recorded as 1#, 2# respectively, in order to avoid obscure；
(3) utilize homemade TEM sample transfer tool, respectively by two samples of 1#, 2# be transferred to sample stage left and right (or
Two sides up and down), and record corresponding position；According to personal habits, it is proposed that the installation site of fixed 1#, 2# sample, so
Both the efficiency for loading sample is improved, while also reducing a possibility that obscuring sample；
(4) sample stage is put into TEM, can be tested after vacuum reaches test request；When test, according to 1#, 2# reality
Corresponding region is found in the position of loading；In this way, can directly carry out the survey of another sample after the test of one sample of completion
Examination.
In step (1), guarantee that sample size is sufficient in support grid when the preparation of powder sample and occupy support grid near middle with
Obtain the good result of energy spectrum analysis, it is proposed that sample preparation Shi Xianyong liquid-transfering gun point, which drops to, to be supported among support grid, in setup test
When cut again.Certainly, be save consumptive material, first by support support grid cutting prepare again into two sample also can, such support grid is
It can be used for the preparation of two kinds of samples, the consuming of support grid will reduce half.
In step (1), it is when necessary the quality for ensuring sample preparation, optical microphotograph can be used and observed in advance, usually
Dispersion of the material again in support grid can be preferably seen in the case where being greater than 100 times.
In step (2), since support grid is very thin, only slightly firmly it need to push and cut and can succeed when cutting, it is ensured that cut through
Guarantee the fixed nonvoluntary sliding in support grid position in journey, supports film in order to avoid destroying.It is recommended that using the knife blade with knife handle or similar
Cutter is easy to use in order to avoid accidentally injuring, is not recommended to use scissors, the size for being on the one hand limited to support grid is smaller (diameter 3mm), another party
Face scissors easily deforms support grid.
In step (2), support grid is to hemisect, it is proposed that two halves copper mesh size is consistent as far as possible after cutting but non-absolute requirement.If
There is point of apparent size, is then the enough viewing areas of guarantee, it is proposed that loading sample is the biggish half of selection.
In step (3), self-control transfer tool refers to a kind of tool of the extensive use field TEM sample transfer, the tool
It is to polish syringe needle through infusion niidl and be made.In use, gently inhaling hose end with mouth, and (flattened after processing) with needle end
Close to support grid is supported, support grid can be sucked up by pressure difference and arbitrarily be shifted.The advantages of transfer method, is neither to damage
Wound support support grid again can the placement location of convenient, flexible control support grid on sample stage, the control for facilitating two support grids to place and
Adjustment.In sample loading process, tweezers also can be used but do not recommend, because it is relatively difficult to the relative position of control two halves support grid,
It is relatively more time-consuming.Other samples shift/and loading tool can be selected according to personal use habit.
Loading condition of above-mentioned two semicircle sample on sample stage, it is proposed that fracture is aligned but is not overlapped and slightly reserves
Some gaps for the optical path adjusting in test process to leave some space region.It is such as limited by semicircle size and a small amount of break occurs
Mouth region domain overlapping phenomenon will not influence to observe.
In step (1), sample stage, can be can arbitrarily load the sample stage that TEM standard supports support grid, can be common
Uniclinal, it is double incline, multidigit sample stage or crucible type specimen heating holder etc., and the quantity of filled sample is sample standard setting-out
Several twice.
If sample needs to recycle after test, it may be convenient to be recycled according to the position of installation, and be unlikely to obscure.
In the whole preparation process of above-mentioned sample, the position making sure to keep in mind the label of sample to be distinguished and being loaded on sample stage,
In order to avoid obscuring.Even if also suggesting that attention in the larger situation of two kinds of test samples (pattern, structure or ingredient) diversity ratio itself
It distinguishes, in order to avoid for sample is distinguished and carries out unnecessary time-consuming when TEM is tested.
After sample stage is put into TEM, relative position is fixed.It can be very square by the sample analog position that software provides
Just region and corresponding sample locating for the sample observed by discrimination is current.Therefore, fixed (or habitual) by 1#, 2# sample
After product installation, the opposite region tested every time will be constant.For the first time, test when for mark sample stage physical location in simulation
The corresponding relationship of illustrated position can only load half of support grid or choose two samples to differ greatly to obtain as label
Then the later period with this use, no longer needs to line flag after corresponding relationship.
Embodiment 2；
Artificial gold (SnS) nanometer sheet provided in an embodiment of the present invention and two kinds of nano-silicon (Si) ball different samples are once put into
The sample stage and specific implementation method observed is described in detail.
Two ultra-thin carbon branch are dispersed by method prepared by powder sample respectively respectively by SnS nanometer sheet and Si nanosphere
It holds spare in film support grid, and is respectively labeled as 1#, 2#.
As shown in Fig. 2, respective double of the cutting schematic diagram of two samples of 1#, 2# provided in an embodiment of the present invention.
As shown in figure 3, sample provided in an embodiment of the present invention is loaded into position and label on sample stage.
Note: a, pictorial diagram；B, illustraton of model；C, the docking situation of two semicircle support grids under TEM.
As shown in Fig. 3 (a) and (b), two samples of 1#, 2# are respectively taken into half of support grid, and place respectively by self-made tool
In the left and right sides of sample stage viewing area, and make a record.
As shown in Fig. 3 (c), sample is fitted into TEM, after vacuum reaches requirement, situation is placed to sample and is checked.
As shown in figure 4, the result schematic diagram of TEM actual observation provided in an embodiment of the present invention.
Note: a is region and the shape appearance figure of 1# sample；B is region and the shape appearance figure of 2# sample.
As shown in figure 4, observing respectively two samples, after the analysis for completing a sample, another is transferred to
With the test of complete paired samples.
Although in this example, the embodiment of the present invention shows only SnS nanometer sheet and two kinds of different materials of Si nanosphere
While in loading and TEM and carrying out observation analysis.However, it will be apparent that this method can very easily be generalized to various samples
Test case in, no matter whether sample has apparent difference (as long as Care Mark different sample and its actually placing
Position).In actual test, two samples of same user can be not only placed in TEM by the present invention simultaneously, can also be incited somebody to action
The sample of different user (when sample has odd number) is placed in Electronic Speculum.
Generally speaking, this method not only ensure that the quality of test but also improve testing efficiency, reduced testing cost, therefore
It is worth being promoted in the TEM test process of conventional powdery type sample.
In actual experiment, test, in most cases everybody be more pay close attention to the partial size of nano material, pattern, crystal phase,
The simple informations such as ingredient without the analysis of fine structure, therefore are tested simply, the time required to the test of single sample relatively
Short, such case is relatively more in related fieldss such as chemical synthesis nano material, biomaterials.Due to sample need the amount seen compared with
It is more, therefore more concerned with the cost of test, it is desirable to the observation of more Multi-example is completed within the same time.For this purpose, having invented primary same
When place two samples method.It is significant on the basis of guaranteeing test effect by the implementation of this method by taking center as an example
Improve the efficiency of test.For protection equipment, it is specified that replacing the time of sample every time must not be lower than 40 minutes, therefore should using
Before method, a whole morning generally can be only done the test of 4-5 sample, and 6- can then be increased to by testing quantity after adopting this method
10.Compared with multidigit sample stage, the method for the present invention is almost zero cost, is suitable for various conventional sample platforms and multidigit sample
Platform, without equipment purchase and restructuring cost；Double functions of inclining of double sample stages that incline more are remained simultaneously, thus the scope of application is more
Extensively.For this purpose, complete itself work on the basis of, spy the method is arranged, to can for go together real work into
Row reference and utilization.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (6)
1. it is a kind of based on transmission electron microscope common sample platform simultaneously load two samples method, which is characterized in that it is described based on
The method that transmission electron microscope common sample platform loads two samples simultaneously, specifically includes the following steps:
Step 1: according to the different characteristics of pre-detection material, suitable TEM is selected to support film support grid, and routinely powder sample
Preparation method by powder sample be scattered in support support grid on it is to be measured；
Step 2: the support grid for having prepared sample is cut in half with blade, and to two samples of well cutting, is recorded as respectively
1#,2#；
Step 3: utilize homemade TEM sample transfer tool, respectively by two samples of 1#, 2# be transferred to sample stage left and right or
Upper and lower two sides, and record corresponding position；
Step 4: being put into TEM for sample stage, is tested after vacuum reaches test request.
2. the method for being loaded two samples simultaneously based on transmission electron microscope common sample platform as described in claim 1, feature are existed
In, in the step 1, film support grid diameter 3mm.
3. the method for being loaded two samples simultaneously based on transmission electron microscope common sample platform as described in claim 1, feature are existed
In in the step 1, powder sample is nano particle, nano wire, nanometer sheet etc..
4. the method for being loaded two samples simultaneously based on transmission electron microscope common sample platform as described in claim 1, feature are existed
In, prevented plowing from the step 2, in cutting process support grid support film.
5. the method for being loaded two samples simultaneously based on transmission electron microscope common sample platform as described in claim 1, feature are existed
In to two samples of well cutting, being recorded as 1#, 2# respectively in the step 2.
6. the method for being loaded two samples simultaneously based on transmission electron microscope common sample platform as described in claim 1, feature are existed
In when test, according to the position of 1#, 2# actual load, finding corresponding region in the step 4；In this way, completing a sample
The test of another sample can be directly carried out after the test of product.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112113811A (en) * | 2020-08-28 | 2020-12-22 | 中国科学院金属研究所 | Preparation method of special sample for three-dimensional nano X-ray microscope |
| CN113189123A (en) * | 2021-04-30 | 2021-07-30 | 东南大学 | Observation micro-area positioning method based on internal standard substance microarray |
| CN113192816A (en) * | 2021-04-26 | 2021-07-30 | 中国科学院物理研究所 | Electron microscope carrier net, preparation method thereof and microscope product |
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| CN113189123B (en) * | 2021-04-30 | 2023-01-31 | 东南大学 | Observation micro-area positioning method based on internal standard substance microarray |
| CN113484545A (en) * | 2021-07-19 | 2021-10-08 | 中科合成油技术有限公司 | Transmission electron microscope multi-sample grid, matched sample preparation table thereof, preparation method and use method |
| WO2023087474A1 (en) * | 2021-11-19 | 2023-05-25 | 深圳晶泰科技有限公司 | Preparation device and method for powder sample |
| CN117804872A (en) * | 2024-02-28 | 2024-04-02 | 广州智达实验室科技有限公司 | Electronic microscope sample preparation system and control method |
| CN117804872B (en) * | 2024-02-28 | 2024-05-28 | 广州智达实验室科技有限公司 | Electronic microscope sample preparation system and control method |
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