CN111521623B - Method for improving sample preparation success rate of powder sample transmission electron microscope in-situ heating chip - Google Patents
Method for improving sample preparation success rate of powder sample transmission electron microscope in-situ heating chip Download PDFInfo
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- CN111521623B CN111521623B CN202010349864.XA CN202010349864A CN111521623B CN 111521623 B CN111521623 B CN 111521623B CN 202010349864 A CN202010349864 A CN 202010349864A CN 111521623 B CN111521623 B CN 111521623B
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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
- G01N23/20—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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/2005—Preparation of powder samples therefor
Abstract
The invention discloses a method for improving the transmission of a powder sampleThe method for success rate of electron microscope in-situ heating chip sample preparation comprises the following steps of mixing Si 3 N 4 Placing the in-situ heating chip with the powder sample agglomerated on the film under an optical microscope to find Si 3 N 4 The hole and groove area of the film is covered, and then one end of the cotton fiber is slowly moved to the hole and groove area of the chip and is connected with Si by a micromanipulator under an optical microscope 3 N 4 Film contact; using a micromanipulator to apply cotton fibers to Si 3 N 4 The film is horizontally rubbed back and forth, so that agglomerated particles separated from the film can be automatically adsorbed on the fibers, and finally Si is adsorbed on the fibers 3 N 4 Removing the agglomerated nano powder in the film area; and adjusting the micro-manipulator to remove the cotton fibers contacted with the chip, thereby obtaining the reusable in-situ heating chip. The method of combining the micromanipulator with the optical microscope used by the invention can lead the aggregation to the Si 3 N 4 The powder sample of the film is removed rapidly and accurately, the operation is simple, and the Si content is reduced 3 N 4 The risk of damage of the film and the chip electrode effectively improves the operation success rate and saves time.
Description
Technical Field
The invention relates to the technical field of transmission electron microscope in-situ characterization, in particular to a method for improving the sample preparation success rate of a powder sample transmission electron microscope in-situ heating chip.
Background
The transmission electron microscope in-situ heating chip sample preparation method of the powder sample has the following difficulties: (1) If the amount of the nano-powder material dispersed in a solvent such as water or ethanol is too small, si is deposited 3 N 4 Less sample on the film, resulting in less sample particles available for observation; (2) If the amount of the nano-powder material dispersed in the solvent such as water or ethanol is too much, the nano-powder is easily aggregated in Si after the solution dropped to the groove area of the chip is volatilized 3 N 4 Thin film regions, ultimately rendering the transmitted electron beam blind for viewing; (3) If (1) occurs, it is necessary to place the film in transmissionTaking out the chip in the electron microscope, and then dripping the sample on the chip again, wherein in the process, if the times of bad titration are mastered, the nano powder in Si can be caused 3 N 4 The condition of agglomeration on the film; (4) It is difficult to judge the titration effect of the nano-powder even with an optical microscope during the dropping process, mainly because of the small size of the nano-powder.
At present, the method does not relate to removing agglomeration in an in-situ heating chip Si 3 N 4 Film area powder particle methods. Some conventional methods that we can imagine, such as soaking with ordinary ethanol or aqueous solution or adding magnetic stirring, are also difficult to remove the agglomerated nanopowder because the nanopowder is mixed with Si 3 N 4 The bonding force of the film is relatively strong van der waals force rather than ordinary physical contact. In addition, if the ultrasonic cleaning method is used, si having a thickness of several tens of nanometers is easily applied 3 N 4 The film shatters. Therefore, due to the difficulty in sample preparation, the sample preparation effect of the chip is not ideal, so that the expensive chip is directly discarded without being observed by a transmission electron microscope.
Disclosure of Invention
The invention aims to provide a method for improving the success rate of sample preparation of a powder sample transmission electron microscope in-situ heating chip, which solves the following technical problems: when the chip is heated in situ for preparing the sample by the transmission electron microscope of the powder sample, if a large amount of sample powder is agglomerated on Si 3 N 4 When the film cannot be observed under a transmission electron microscope, the polymer is agglomerated on Si by the method under the premise of not damaging the in-situ heating chip 3 N 4 The powder sample on the film is simply, quickly and effectively removed, and the reusable in-situ heating chip is obtained, so that the success rate of the transmission electron microscope in-situ heating chip sample preparation of the powder sample is improved.
The technical scheme of the invention is as follows: a method for improving the success rate of sample preparation of a powder sample transmission electron microscope in-situ heating chip comprises the following steps:
(1) Selection of cotton fibers: selecting cotton fiber with the length of 5-20 mm;
(2) Obtaining a glass needle: arranging the capillary glass tube on a needle drawing instrument, and obtaining a conical glass needle point by adopting a gravity traction method for the capillary glass tube after the working temperature of the needle drawing instrument is set;
(3) Mutual adhesion of the glass needle tip and the cotton fiber: uniformly coating the adhesive on the glass needle point, and then mutually adhering the glass needle point and one end of the cotton fiber under an optical microscope;
(4) Fixing the glass needle with the micro-manipulator: fixing one end of the glass needle far away from the glass needle point on a micromanipulator, and enabling the needle point of the glass needle with cotton fibers to face downwards;
(5) Mixing Si 3 N 4 Placing the in-situ heating chip with the powder sample agglomerated on the film under an optical microscope to find Si 3 N 4 The hole and groove area of the film is then moved slowly to the hole and groove area of the chip by a micromanipulator under an optical microscope and then contacted with Si 3 N 4 Film contact;
(6) Using a micromanipulator to apply cotton fibers to Si 3 N 4 The film is horizontally rubbed back and forth, so that agglomerated particles separated from the film can be automatically adsorbed on the fibers, and finally Si is adsorbed on the fibers 3 N 4 Removing the agglomerated nano powder in the film area;
(7) And adjusting the micro-operator to remove the cotton fibers contacted with the chip to obtain the reusable in-situ heating chip.
Further, the length of the cotton fiber is 5-10 mm.
Further, the working temperature of the needle drawing instrument in the step (2) is set to be 580-650 ℃.
Further, the diameter of the glass needle tip in the step (2) is 15-25 μm.
Further, the length of the capillary glass tube in the step (2) is 8-15 mm, the outer diameter is 1-3 mm, and the inner diameter is 0.5-0.8 mm.
Further, the binder in the step (3) is polyvinylidene fluoride.
The beneficial effects of the invention are:
1、the method of combining the cotton fiber with the micromanipulator and the optical microscope can realize the in-situ heating of Si in the chip by the transmission electron microscope 3 N 4 Precise removal of different types of powder material agglomerated in thin film regions;
2. the applied sample preparation method is a simple physical removal process, does not need to adopt acid or alkali or organic solvent, and does not generate harmful pollutants in the whole operation process, so the method is green and environment-friendly;
3. the cotton fiber is driven to move by the conical glass needle tip, so that the position of the cotton fiber is easy to control;
4. the method of using a micromanipulator in combination with an optical microscope enables agglomeration in Si 3 N 4 The powder sample of the film is removed rapidly and accurately, the operation is simple, and the Si content is reduced 3 N 4 The risk of damage of the thin film and the chip electrode effectively improves the success rate of operation and saves time;
5. because the needle drawing instrument, the micromanipulator and the optical microscope are relatively conventional experimental instruments, experimental equipment is easy to obtain.
Drawings
FIG. 1 is a schematic flow chart of the method for improving the success rate of sample preparation of a powder sample transmission electron microscope in-situ heating chip according to the invention.
FIG. 2 shows that the sample powder in the MEMS chip is agglomerated to Si in a large amount 3 N 4 Optical microscopy topography on thin films.
FIG. 3 is an optical microscope topography of a MEMS chip processed using the present invention.
Reference numerals: 1-agglomerated sample powder, 2-Si 3 N 4 Film, 3-cotton fiber.
Detailed Description
The present invention will be further described with reference to the following examples and accompanying drawings, but the present invention is not limited to the scope of protection and application.
As shown in FIG. 1, the method for improving the success rate of the sample preparation of the powder sample transmission electron microscope in-situ heating chip comprises the following steps:
s1, selecting cotton fibers: selecting cotton fiber with the length of 5-10 mm;
s2, obtaining a glass needle: arranging the capillary glass tube on a needle drawing instrument, setting the working temperature of the needle drawing instrument to be 580-650 ℃, and obtaining a conical glass needle point by adopting a gravity traction method for the capillary glass tube; the diameter of the glass needle tip is 20 μm; the capillary glass tube used in the manufacturing process can adopt the specifications of 9mm in length, 1mm in outer diameter and 0.6mm in inner diameter;
s3, mutual adhesion of the glass needle tip and the cotton fiber: uniformly coating a bonding agent (such as polyvinylidene fluoride (PVDF)) on a glass needle point, and then mutually bonding one end of the cotton fiber with the glass needle point under an optical microscope;
s4, fixing the glass needle and the micro-manipulator: fixing one end of the glass needle far away from the glass needle point on a micromanipulator, and enabling the needle point of the glass needle with cotton fibers to face downwards;
s5, mixing Si 3 N 4 Placing the in-situ heating chip with the powder sample agglomerated on the film under an optical microscope to find Si 3 N 4 The hole and groove area of the film is covered, and then one end of the cotton fiber is slowly moved to the hole and groove area of the chip and is connected with Si by a micromanipulator under an optical microscope 3 N 4 The films are in contact.
S6, using a micromanipulator to make the cotton fiber in Si 3 N 4 The film is horizontally rubbed back and forth, and then the friction force acts on Si 3 N 4 The force of the cotton fibers on the film is very small, so that agglomerated particles adhered to the film are separated from the film while the film and the annular electrode on the film are not damaged; in addition, the cotton fiber has electrostatic force, and the agglomerated particles separated from the film in the process can be automatically adsorbed to the fiber, and finally Si is adsorbed to the fiber 3 N 4 And removing the agglomerated nano powder in the film area.
And S7, adjusting the micro-operator to remove the cotton fibers in contact with the chip, so as to obtain the reusable in-situ heating chip.
The invention adopts a method of combining a micromanipulator and an optical microscope, and can accurately control the cotton fiber to be just matched with Si 3 N 4 The contact height position of the nanometer film horizontally moves back and forth, and the phenomenon that the glass needle tip is contacted with the nanometer film to damage the film and the electrode in the operation process is well avoided.
The advantages of the present invention are illustrated below in connection with comparative experiments.
As shown in FIG. 2, during the preparation of MEMS chip samples, there was a lot of agglomerated powder samples 1 to Si if mishandled 3 N 4 In the region of the film 3, the transmission electron beam eventually fails to pass through these agglomerated powder sample regions and cannot be observed by transmission electron microscopy;
as shown in figure 3, the method for improving the success rate of the in-situ heating chip sample preparation of the powder sample by the transmission electron microscope of the invention combines the cotton fiber 2 with the glass needle, the optical microscope and the micromanipulator without damaging Si 3 N 4 On the premise of the thin film 3, the tip of the cotton fiber 1 is controlled to move back and forth in the agglomerated powder sample area and finally agglomerated on Si under the precise action of the cotton fiber 2 3 N 4 The powder sample in the area of the membrane 3 is removed very well. The processed MEMS chip can be reused for preparing powder samples, and the utilization rate is high.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or simple substitutions which are not thought of by the inventive labor should be covered within the scope of the present invention.
Claims (5)
1. A method for improving the success rate of the in-situ heating chip sample preparation of a powder sample is characterized by comprising the following steps:
(1) Selection of cotton fibers: selecting cotton fiber with the length of 5-20 mm;
(2) Obtaining a glass needle: arranging the capillary glass tube on a needle drawing instrument, and obtaining a conical glass needle point by adopting a gravity traction method for the capillary glass tube after setting the working temperature of the needle drawing instrument;
(3) Mutual adhesion of the glass needle tip and the cotton fiber: uniformly coating the adhesive on the glass needle point, and then mutually adhering the glass needle point and one end of the cotton fiber under an optical microscope;
(4) Fixing the glass needle with the micro-manipulator: fixing one end of the glass needle far away from the glass needle point on a micromanipulator, and enabling the needle point of the glass needle with cotton fibers to face downwards;
(5) Mixing Si 3 N 4 Placing the in-situ heating chip with the powder sample agglomerated on the film under an optical microscope to find Si 3 N 4 The hole and groove area of the film is covered, and then one end of the cotton fiber is slowly moved to the hole and groove area of the chip and is connected with Si by a micromanipulator under an optical microscope 3 N 4 Film contact;
(6) Using a micromanipulator to apply cotton fibers to Si 3 N 4 The film is rubbed horizontally back and forth, so that agglomerated particles separated from the film can be automatically adsorbed on the fibers, and finally Si is adsorbed on the fibers 3 N 4 Removing the agglomerated nano powder in the film area;
(7) Adjusting a micro-operator to remove the cotton fibers contacted with the chip to obtain a reusable in-situ heating chip;
the binder in the step (3) is polyvinylidene fluoride.
2. The method for improving the success rate of the powder sample transmission electron microscope in-situ heating chip sample preparation according to claim 1, which is characterized in that: the length of the cotton fiber is 5-10 mm.
3. The method for improving the success rate of the powder sample preparation by the transmission electron microscope in-situ heating chip according to claim 1, which is characterized in that: the working temperature of the needle drawing instrument in the step (2) is set to be 580-650 ℃.
4. The method for improving the success rate of the sample preparation of the powder sample transmission electron microscope in-situ heating chip according to claim 1 or 3, which is characterized in that: the diameter of the glass needle point in the step (2) is 15-25 μm.
5. The method for improving the success rate of the powder sample preparation by the transmission electron microscope in-situ heating chip according to claim 1, which is characterized in that: the length of the capillary glass tube in the step (2) is 8-15 mm, the outer diameter is 1-3 mm, and the inner diameter is 0.5-0.8 mm.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06275190A (en) * | 1993-03-18 | 1994-09-30 | Nikon Corp | Manufacture of cantilever, and scanning type probe microscope provided with the same |
| WO2007011076A1 (en) * | 2005-07-15 | 2007-01-25 | Korea Institute Of Machinery And Materials | Attaching method of nano materials using langmuir-blodgett |
| CN109827820A (en) * | 2019-03-07 | 2019-05-31 | 中国工程物理研究院材料研究所 | A kind of in situ TEM sample preparation methods based on heating chip |
Family Cites Families (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6582983B1 (en) * | 2002-07-12 | 2003-06-24 | Keteca Singapore Singapore | Method and wafer for maintaining ultra clean bonding pads on a wafer |
| EP1754049A2 (en) * | 2004-06-08 | 2007-02-21 | Omniprobe, Inc. | Method for manipulating microscopic particles and analyzing the composition thereof |
| CN101835557B (en) * | 2007-10-24 | 2015-01-07 | 同和电子科技有限公司 | Silver microparticle-containing composition, process for production of the composition, process for production of the silver microparticle, and paste containing the silver microparticle |
| CN101538370B (en) * | 2008-03-20 | 2011-07-27 | 中国石油大学(北京) | Polymeric composite in-situ growth nano-particle molecular film and preparation method thereof |
| CN102531015A (en) * | 2011-05-26 | 2012-07-04 | 中国科学院福建物质结构研究所 | Method for preparing porous aluminum oxide superfine powder |
| US8969827B2 (en) * | 2012-07-09 | 2015-03-03 | Materials Analysis Technology (Us) Corp. | Specimen preparation for transmission electron microscopy |
| JP6246089B2 (en) * | 2014-07-17 | 2017-12-13 | 富士フイルム株式会社 | Display device with conductive film and touch panel |
| CN104990840A (en) * | 2015-06-05 | 2015-10-21 | 中国海洋大学 | Method for observing morphology of ultrafine powder sample by using scanning electron microscope |
| CN107505174B (en) * | 2017-07-12 | 2019-11-12 | 广西大学 | A kind of method for making sample of the transmission electron microscope In Situ Heating chip of nano material |
| 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 |
| CN108169266B (en) * | 2017-11-09 | 2020-11-24 | 广东科技学院 | Preparation method of scanning electron microscope sample of micron-sized ionic crystal powder |
| CN108426905A (en) * | 2018-02-02 | 2018-08-21 | 东华大学 | A kind of simple and easy method of nanometer powder dispersion electron microscopyc sample preparation |
| CN108381379B (en) * | 2018-04-13 | 2019-05-24 | 中国电子科技集团公司第四十六研究所 | The polishing method that aluminum-nitride single crystal piece electrobrightening and chemically mechanical polishing combine |
| CN108744990B (en) * | 2018-06-01 | 2020-08-07 | 徐州医科大学 | Silver nanoparticle modified titanium dioxide nanofiber membrane material and preparation method and application thereof |
| CN108554663A (en) * | 2018-06-27 | 2018-09-21 | 湖北金稽山机械科技有限公司 | A kind of thickening powder body material molding machine |
| CN109235038A (en) * | 2018-08-31 | 2019-01-18 | 高昕文 | A kind of preparation method of antibacterial facial mask fabric |
| CN109239113B (en) * | 2018-09-30 | 2019-06-14 | 中国科学院地质与地球物理研究所 | The transmission electron microscope sample preparation method of the Armco magnetic iron protein nano particle of bio-mimetic syntheses |
| CN110068962A (en) * | 2019-06-17 | 2019-07-30 | 京东方科技集团股份有限公司 | Display base plate and its friction orientation method, preparation method |
| CN110231355B (en) * | 2019-06-17 | 2020-08-25 | 西安交通大学 | Method for preparing micron-sized metal powder transmission electron microscope film sample |
-
2020
- 2020-04-28 CN CN202010349864.XA patent/CN111521623B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06275190A (en) * | 1993-03-18 | 1994-09-30 | Nikon Corp | Manufacture of cantilever, and scanning type probe microscope provided with the same |
| WO2007011076A1 (en) * | 2005-07-15 | 2007-01-25 | Korea Institute Of Machinery And Materials | Attaching method of nano materials using langmuir-blodgett |
| CN109827820A (en) * | 2019-03-07 | 2019-05-31 | 中国工程物理研究院材料研究所 | A kind of in situ TEM sample preparation methods based on heating chip |
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