CN102235945B - Method for preparing amorphous film sample for transmission electron microscope research - Google Patents
Method for preparing amorphous film sample for transmission electron microscope research Download PDFInfo
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- CN102235945B CN102235945B CN 201010153603 CN201010153603A CN102235945B CN 102235945 B CN102235945 B CN 102235945B CN 201010153603 CN201010153603 CN 201010153603 CN 201010153603 A CN201010153603 A CN 201010153603A CN 102235945 B CN102235945 B CN 102235945B
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Abstract
The invention provides a method for preparing an amorphous film sample for transmission electron microscope research. The method is characterized by comprising the following steps: A, substrate cleaning; B, spin coating; C, material growing; and D, peeling, so that the amorphous film sample for transmission electron microscope experiments is obtained, wherein the substrate where the film material grows can be a glass slide, a silicon wafer, a quartz sheet or a gem plate. The method has a simple process and high yield, does not need mechanical, chemical, ion beam and other reduction technologies, and has the advantages of pollution prevention, low cost and strong operability; and the amorphous film prepared by the process can reduce occurrence of pseudomorph and rupture.
Description
Technical field
The present invention relates to a kind of preparation method of noncrystalline membrane, relate in particular to a kind of preparation method of the noncrystalline membrane sample for transmission electron microscope research.
Background technology
The micromechanism of photoelectric material determines the performances such as photoelectricity of material, and the microstructure of research material and area diffraction figure help the selection analysis of photoelectric material.The resolution of transmission electron microscope reaches 0.1～0.2nm, and enlargement factor reaches several ten thousand to 1,000,000 times, and the ultrastructure that energy viewing optics microscopically can't be seen clearly is the microstructural important means of research material.Use the tem study material, very thin sample need to be arranged as the object of observation, its principle of work is projecting on the film sample through the electron beam that accelerates and assemble, the ability that electron beam penetrates film sample depends on that the atomic weight of accelerating potential and film sample element is big or small, in general, accelerating potential is larger, and the atomic weight number of thin film composition is lower, the degree of depth that electron beam can penetrate is just larger, more can obtain effect clearly micro-image and area diffraction figure.In order to obtain effect clearly micro-image and area diffraction figure, the thickness requirement of the film sample of transmission electron microscope is in 5～200nm scope.
At present, film sample preparation method commonly used mainly contains the methods such as replica technique, the two sprays of electrolysis, ion milling, and wherein, replica technique just copies sample surface morphology, can not disclose material internal microstructure information; The two spray techniques of electrolysis are then easily introduced foreign impurity, inherent heterogeneous microstructure that can not objective ground reactive film material; The sample ions attenuate can attenuate occur in operating process inhomogeneous, even sample burst can occur, causes sample to be subject in various degree pollution, illusion, causes truly reflecting the micromechanism of sample, brings error to measurement result.For guaranteeing representative all features with true reflection institute analysis of material of film sample, the film sample that must guarantee to be used for transmission electron microscope is harmless, inclusion-free is introduced, and film sample thickness is below 200nm.
Summary of the invention
Prepare the deficiency that sample for use in transmitted electron microscope exists for solving existing method, the invention provides a kind of preparation method of the noncrystalline membrane sample for transmission electron microscope.
Noncrystalline membrane sample preparation methods for transmission electron microscope research provided by the invention, its technical scheme is:
A. substrate cleans, will be as the microslide of backing material, and in pure water, be placed on behind the scrub in the potassium bichromate solution with abluent and soaked 24 hours, clean with pure water rinsing again, be put in the Ultrasound Instrument with the ultrasonic processing of 30W 10 minutes, taking-up dries up with high pure nitrogen;
B. whirl coating gets rid of one deck organic gel equably with equal glue machine on the substrate of crossing through processing of step A in the gold-tinted darkroom, and all glue machine rotating speed is set to 5000～7700 rpms;
C. growth material adopts the method for magnetron sputtering at Grown noncrystalline membrane material, and the growthing process parameter of magnetron sputtering is: background vacuum pressure 2.0 * 10
-4～4.0 * 10
-4Pa, sputter gas are high-purity argon gas (Ar), and flow 20～150sccm, underlayer temperature are 10～500 ℃, and operating pressure is 0.8～1.5pa, sputtering power 5～300W, thin and thick 20～200nm;
D. peel off.The noncrystalline membrane that is grown on the substrate is put into acetone immersion 4 hours together with substrate, put into again ethanol and soak taking-up after 2 hours, treat that film surface ethanol is evaporated completely, obtain the noncrystalline membrane for the electron microscopic sample experiment.
As the microslide of backing material growing film material, can also use silicon chip, piezoid or jewel sheet to substitute, wherein, adopt the silicon chip of epitaxy-ready not need before use to carry out any processing; Adopt the same microslide of pre-treatment method of piezoid and jewel sheet.
The invention has the beneficial effects as follows: the inventive method technique is simple, yield rate is higher, need not introduce the thinning techniques such as machinery, chemistry, ion beam, have advantages of be difficult for polluting, cost is low, workable; Can reduce the generation of illusion, fracture phenomena with the noncrystalline membrane of this technique preparation.
Description of drawings
Fig. 1 is the micro-image of the transmission electron microscope of amorphous MCT film sample;
Fig. 2 is the area diffraction figure of the transmission electron microscope of amorphous MCT film sample.
Specific embodiments
Below in conjunction with accompanying drawing, the present invention is described in further detail.
Embodiment one:
The present embodiment is take preparation used in transmission electron microscope amorphous mercury cadmium telluride thin film sample as example, its concrete steps are as follows: select clean smooth No. 7101 smooth microslides as substrate, in pure water, clean the greasy dirt of slide surface with abluent, put into again in the potassium bichromate solution and to soak the metal that removed slide surface in 24 hours and attach thing, then totally put into again in the pure water ultrasonic with pure water rinsing, ultrasonic power 30w is set, ultrasonic 10 minutes, the high pure nitrogen of usefulness 99.999% blows off the moisture of slide surface after finishing, then in the gold-tinted darkroom, get rid of equably last layer photoresist (positive glue AZ9260) with equal glue machine, about thickness 6 μ m (all glue machine rotating speed be set to 7700 rpms), deliver to magazine after finishing and keep 10 ℃ of substrate constant temperature in the magnetron sputtering apparatus, background vacuum pressure 2.0 * 10
-4～4.0 * 10
-4Pa, sputter gas are 99.999% high-purity argon gas, flow 150sccm, and operating pressure is 1.1pa, and sputtering power is 10W, and target is selected Hg
1-xCd
xTe (x=0.22 in the present embodiment), growth amorphous MCT membraneous material, the Material growth time is 5 minutes, the thickness of growth is 150～180nm, after growth finishes, material is put into acetone together with substrate soaked 4 hours, put into again ethanol and soaked 2 hours, take out natural drying after, obtain diameter and be about the smooth amorphous MCT film sample of 3mm and be used for electron microscope experiment.
Embodiment two:
The present embodiment is take preparation used in transmission electron microscope amorphous silicon membrane sample as example, its concrete steps are as follows: select clean smooth No. 7101 smooth microslides as substrate, in pure water, clean the greasy dirt of slide surface with abluent, put into again in the potassium bichromate solution and to soak the metal that removed slide surface in 24 hours and attach thing, then totally put into again in the pure water ultrasonic with pure water rinsing, ultrasonic power 30w is set, ultrasonic 10 minutes, the high pure nitrogen of usefulness 99.999% blows off the moisture of slide surface after finishing, then in the gold-tinted darkroom, get rid of equably last layer photoresist (positive glue AZ9260) with equal glue machine, about thickness 6 μ m (all glue machine rotating speed be set to 7700 rpms), deliver to magazine after finishing and keep 250 ℃ of substrate constant temperature in the magnetron sputtering apparatus, background vacuum pressure 2.0 * 10
-4～4.0 * 10
-4Pa, sputter gas are 99.999% high-purity argon gas, flow 150sccm, and operating pressure is 1.5pa, sputtering power is that 200W, target are selected monocrystalline silicon, the amorphous silicon thin-film materials of growing with this understanding.The Material growth time is 6 minutes, and the thickness of growth is 150～180nm, after growth finishes, material is put into acetone together with substrate to be soaked 4 hours, put into again ethanol and soaked 2 hours, takes out natural drying after, obtain diameter and be about the smooth amorphous silicon membrane sample of 3mm for electron microscope experiment.
Claims (2)
1. one kind is used for the noncrystalline membrane sample preparation methods that transmission electron microscope is studied, and it is characterized in that realizing by following steps:
A. substrate cleans, will be as the microslide of backing material, and in pure water, be placed on behind the scrub in the potassium bichromate solution with abluent and soaked 24 hours, clean with pure water rinsing again, be put in the Ultrasound Instrument with the ultrasonic processing of 30W 10 minutes, taking-up dries up with high pure nitrogen;
B. whirl coating gets rid of one deck organic gel equably with equal glue machine on the substrate of crossing through processing of step A in the gold-tinted darkroom, and all glue machine rotating speed is set to 5000～7700 rpms;
C. growth material adopts the method for magnetron sputtering at Grown noncrystalline membrane material, and the growthing process parameter of magnetron sputtering is: background vacuum pressure 2.0 * 10
-4～4.0 * 10
-4Pa, sputter gas are high-purity argon gas, and flow 20～150sccm, underlayer temperature T are 10～50 ℃, and operating pressure is 0.8～1.5pa, sputtering power 5～300W, thin and thick 20～200nm;
D. peel off, the noncrystalline membrane that is grown on the substrate is put into acetone immersion 4 hours together with substrate, put into again ethanol and soak taking-up after 2 hours, treat that film surface ethanol is evaporated completely, obtain the noncrystalline membrane for the electron microscopic sample experiment.
2. according to noncrystalline membrane sample preparation methods claimed in claim 1, it is characterized in that with silicon chip, piezoid or jewel sheet as backing material.
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| CN106908290B (en) * | 2017-02-16 | 2019-10-11 | 中国科学院合肥物质科学研究院 | The preparation method of holography observation transmission electron microscope sample |
| CN107167485B (en) * | 2017-04-14 | 2019-09-17 | 广西大学 | A kind of preparation method of the power-up transmission electron microscope cross-sectional sample in situ of hetero-junction thin-film |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1402594A (en) * | 2002-09-20 | 2003-03-12 | 西安理工大学 | Process of mfg. electrothermal SnO2:F film heating pipe by ultrasonic spray |
| CN1641067A (en) * | 2004-01-09 | 2005-07-20 | 中国科学院金属研究所 | Method for preparing film sample for transmission electron microscope |
| CN1696334A (en) * | 2004-05-12 | 2005-11-16 | 中国科学院金属研究所 | Method for preparing film specimen in use for transmission electron microscope |
| CN101216386A (en) * | 2007-12-26 | 2008-07-09 | 厦门大学 | Thin film material transmission electron microscope sample preparation method |
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| US7276561B2 (en) * | 2003-08-28 | 2007-10-02 | Japan Atomic Energy Research Institute | Processes for producing nano-space controlled polymer ion-exchange membranes |
| US7348570B2 (en) * | 2005-12-14 | 2008-03-25 | University Of Washington | Unsupported, electron transparent films and related methods |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1402594A (en) * | 2002-09-20 | 2003-03-12 | 西安理工大学 | Process of mfg. electrothermal SnO2:F film heating pipe by ultrasonic spray |
| CN1641067A (en) * | 2004-01-09 | 2005-07-20 | 中国科学院金属研究所 | Method for preparing film sample for transmission electron microscope |
| CN1696334A (en) * | 2004-05-12 | 2005-11-16 | 中国科学院金属研究所 | Method for preparing film specimen in use for transmission electron microscope |
| CN101216386A (en) * | 2007-12-26 | 2008-07-09 | 厦门大学 | Thin film material transmission electron microscope sample preparation method |
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