CN100360708C - Method for preparing film specimen in use for transmission electron microscope - Google Patents
Method for preparing film specimen in use for transmission electron microscope Download PDFInfo
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- CN100360708C CN100360708C CNB2004100205313A CN200410020531A CN100360708C CN 100360708 C CN100360708 C CN 100360708C CN B2004100205313 A CNB2004100205313 A CN B2004100205313A CN 200410020531 A CN200410020531 A CN 200410020531A CN 100360708 C CN100360708 C CN 100360708C
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- 238000000034 method Methods 0.000 title claims abstract description 21
- 230000005540 biological transmission Effects 0.000 title claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 72
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 27
- 239000000956 alloy Substances 0.000 claims abstract description 27
- 238000004544 sputter deposition Methods 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims description 19
- 239000002184 metal Substances 0.000 claims description 19
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 9
- 239000010936 titanium Substances 0.000 claims description 9
- 229910000640 Fe alloy Inorganic materials 0.000 claims description 8
- 239000007921 spray Substances 0.000 claims description 8
- 206010040844 Skin exfoliation Diseases 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 7
- 230000035618 desquamation Effects 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 7
- 238000000992 sputter etching Methods 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 238000007654 immersion Methods 0.000 claims description 6
- 239000000344 soap Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 229910052755 nonmetal Inorganic materials 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 2
- 229910000858 La alloy Inorganic materials 0.000 claims description 2
- 229910000861 Mg alloy Inorganic materials 0.000 claims description 2
- 229910001182 Mo alloy Inorganic materials 0.000 claims description 2
- 229910001093 Zr alloy Inorganic materials 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims description 2
- 238000007747 plating Methods 0.000 abstract description 7
- 150000002500 ions Chemical class 0.000 abstract 2
- 238000005507 spraying Methods 0.000 abstract 2
- 238000011946 reduction process Methods 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 240000007762 Ficus drupacea Species 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910021419 crystalline silicon Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
The present invention discloses a method for preparing a film sample for a transmission electron microscope. The method comprises the following specific steps: (1) a magnetically controlled sputtering method is used for plating a metallic film or an alloy film, an alloy target serves as a negative pole for magnetically controlled sputtering, a substrate serves as a positive pole, the vacuum degree of a back bottom is between 2.0 Pa and 8.0*10<-5> Pa, the gas atmosphere is an Ar atmosphere of which the vacuum degree is between 6.5 Pa and 7.5*10<-1> Pa, the current is between 0.5 A and 2 A, and the voltage is between 100 V and 300 V; (2) a circular sheet is punched from the metallic film or the alloy film; (3) the circular sheet is thinned with a double spraying method or ions to prepare a sample for observation with the electron microscope. The present invention adopts the magnetically controlled sputtering method, so the metallic film or the alloy film which is uniform, compact and easy to strip off can be obtained; the thickness of a plated film on the substrate is between 5 mu m and 9 mu m. Magnetically controlled sputter film plating can be directly combined with double spraying thinning or ion thinning to prepare the sample for the observation with the electron microscope. The present invention solves the problem that a film sample for the electron microscope is easy to pollute, break and lead in false images in the process of traditional machine thinning.
Description
Technical field
The invention belongs to the preparing electron microscopy specimen technical field, a kind of method for preparing Electronic Speculum with sample easily is provided especially.
Background technology
In order to study the microtexture of metal or alloy film, need the preparation electron microscopic sample to observe, be used for the sample of transmission electron microscope observation, owing to a little less than the penetrativity of electronics, require its thickness as thin as a wafer, be generally between 5～200nm.The general film that will observe that on metal substrate, plates earlier in traditional sample making course, and then metal substrate rubbing down to 50～below the 60 μ m, and then carry out the two spray of single face ionic fluid attenuate or single face attenuates, in this process, can cause sample to be subjected to pollution in various degree and in the mechanical reduction process, introduce easily illusion, influence final observing effect, can not observe the real structure of sample; In addition, the edge chamfer phenomenon appears in sample easily in the rubbing down process, when serious even can make that sample is cracked to be fallen, for also not having efficient ways to solve in these problem documents records.
Summary of the invention
The objective of the invention is to: provide a kind of Electronic Speculum for preparing easily with the method for film sample, solved Electronic Speculum with film sample in traditional mechanical reduction process, polluted easily, the problem of broken and introducing illusion.
Technical scheme of the present invention is:
A kind of preparation method of used in transmission electron microscope film sample, carry out as follows:
1) utilize magnetically controlled sputter method to produce metallic membrane or alloy film, magnetron sputtering is a negative pole with the metal or alloy target, and substrate is anodal, and concrete steps and processing parameter are as follows:
A) vacuum chamber is vacuumized, make back of the body end vacuum tightness reach 2.0 * 10
-5～8.0 * 10
-5Pa;
B) feed Ar gas to vacuum chamber, making plated film atmosphere is Ar atmosphere, and vacuum degree control is 6.5 * 10 during with plated film
-1～7.5 * 10
-1Between the Pa scope;
C) sputtering voltage is 100～300V, and target current is 0.5～2A;
D) pre-sputter sputter coating on substrate again after 2～5 minutes, 60～90 minutes plated film time, the thickness that makes film on the substrate is between 5～9 μ m;
2) on described substrate, directly take off utilize magnetically controlled sputter method plate the metal or alloy film, go out the disk that diameter is 3mm then;
3) described disk is carried out two spray attenuates or ion milling and make the sample that electron microscopic observation is used.
Before the described step a), after substrate deoiled through acetone, alcohol ultrasonic cleaning respectively, be placed in the suds, soak 1～5 minute time, take out air-dryly then, make its surface scribble one deck soap film uniformly.
Described step 2) adopts: will plate good film and make the automatic and substrate desquamation of film, and use then towards model machine and make the disk that diameter is 3mm with distilled water immersion.
Described substrate adopts molybdenum, stainless steel, copper or the nickel substrate in the metal substrate; Perhaps adopt glass or monocrystalline substrate in the nonmetal substrate.
Described target matter is one of titanium or titanium alloy, iron and iron alloy, copper and copper alloy and zirconium alloy, molybdenum alloy, lanthanum alloy, magnesium alloy.
Beneficial effect of the present invention is as follows:
1, the present invention adopts method sputter coating on substrate of magnetron sputtering, the target utilization height, sedimentation rate is fast, working temperature is low, the temperature rise of substrate is low, damage little, by optimizing the magnetron sputtering technique parameter, can obtain evenly, fine and close metal or alloy film, and strong adhesion between the film of existing magnetron sputtering technique plating and the substrate, the present invention proposes on the thought basis that overcomes the strong bonding force of film and substrate, the thickness of institute's plated film is between 5～9 μ m on the substrate, can directly magnetron sputtering plating be combined with two spray attenuates or ion milling and make the sample that electron microscopic observation is used, solve Electronic Speculum and in traditional mechanical reduction process, polluted easily with film sample, the problem of fragmentation and introducing illusion.
2, the present invention is used on metal or nonmetal (glass, silicon single crystal etc.) substrate and is coated with metal and alloy films thereof such as aluminium, copper, iron, chromium, nickel, titanium, applied range.
3, the present invention adopts metal substrate and nonmetal substrate, and metal substrate is as substrates such as molybdenum, stainless steel, copper or nickel; Nonmetal substrate adopts method sputter coating on substrate of magnetron sputtering as substrates such as glass, silicon single crystal, can directly take off utilize magnetically controlled sputter method plate the metal or alloy film, also can make film automatically and substrate desquamation with distilled water immersion.
4, the present invention is placed on clean substrate in the suds before carrying out magnetron sputtering, soaks 1～5 minute time, takes out air-dryly then, makes its surface scribble one deck soap film uniformly, is beneficial to film and substrate desquamation.
5, the present invention adopts pre-sputter to carry out plated film after 2～5 minutes, because the easy oxidation of alloys target can be removed the zone of oxidation on the alloys target by pre-sputter, carries out plated film then, can obtain clean metal or alloy film, and its purity is higher.
Description of drawings
Fig. 1 a is the TiZrYAl alloy film photo that obtains with the glass substrate sputter.
Fig. 1 b is the TiZrYAl alloy film photo that obtains for the substrate sputter with Mo.
Fig. 1 c is the transmission electron microscope photo of TiZrYAl alloy film.
Fig. 2 a is to be the Fe alloy film photo that the substrate sputter obtains with monocrystalline silicon piece Si.
Fig. 2 b is the transmission electron microscope photo of Fe alloy film.
Fig. 3 a is the pure Ti film photo that obtains for the substrate sputter with the stainless steel substrates.
Fig. 3 b is the transmission electron microscope photo of pure Ti film.
Embodiment
The present invention adopts following method and technology, success prepare the Electronic Speculum film sample.
1) utilize magnetically controlled sputter method to prepare the metal or alloy film, magnetron sputtering is negative pole with the alloys target, and substrate is anodal, and concrete steps and processing parameter are as follows:
A) vacuum chamber is vacuumized, make back of the body end vacuum tightness reach 2.0 * 10
-1～8.0 * 10
-5Pa;
B) feed Ar gas to vacuum chamber, making plated film atmosphere is Ar atmosphere, and vacuum degree control is 6.5 * 10 during with plated film
-1～7.5 * 10
-1Between the Pa scope;
C) sputtering voltage is 100～300V, and target current is 0.5～2A;
D) pre-sputter sputter coating on substrate again after 2～5 minutes, 60～90 minutes plated film time, the thickness that makes plated film on the substrate is between 5～9 μ m;
2) on described substrate, directly take off utilize magnetically controlled sputter method plate the metal or alloy film, go out the disk that diameter is 3mm then;
3) described disk is carried out two spray attenuates or ion milling and obtain the sample that electron microscopic observation is used.
Embodiment 1
Specimen preparation: sheet glass and Mo sheet after deoiling through acetone, alcohol ultrasonic cleaning respectively are placed in the suds as substrate, soaked 2 minutes, take out air-dryly then, make its surface scribble one deck soap film uniformly; Being negative pole with the TiZrYAl alloys target then, is positive pole with glass substrate and Mo substrate respectively, adopts following processing parameter preparation on magnetron sputtering coater: be evacuated to the back of the body end vacuum tightness during sputter earlier and reach 6.0 * 10
-5About Pa, feed purity then and be 99.99% Ar gas, the vacuum tightness when making plated film maintains 7.0 * 10
-1About Pa, electric current 1A, voltage 160V, pre-sputter sputter coating on substrate again after 5 minutes, 90 minutes plated film time, thickness is about 9 μ m, Fig. 1 a and Fig. 1 b are respectively the glass substrate that obtains after the sputter and the Ti alloy film photo of Mo, can see that film peels off phenomenon with substrate.
The film that plating is good makes the automatic and substrate desquamation of Ti alloy film with distilled water immersion, use then towards model machine and make the disk that diameter is 3mm, carry out two spray attenuates or ion milling again and produce electron microscopic sample, shown in Fig. 1 c, the present invention's success observed Ti alloy film TEM (transmission electron microscope) photo, the gained Electronic Speculum is clean, even, fine and close with film sample, solved Electronic Speculum with film sample in traditional mechanical reduction process, polluted easily, broken and introduce the problem of illusion.
Embodiment 2
Difference from Example 1 is:
Specimen preparation: the single crystalline Si sheet after deoiling through acetone, alcohol ultrasonic cleaning is placed in the suds as substrate, soaked 4 minutes, take out air-dryly then, make its surface scribble one deck soap film uniformly; (alloy designations is: FeZrSiMn) being negative pole, is positive pole with the single crystalline Si sheet, adopts following processing parameter on magnetron sputtering coater, is evacuated to the back of the body end vacuum tightness during sputter earlier and reaches 3.0 * 10 with the Fe alloys target then
-5About Pa, feed purity then and be 99.99% Ar gas, the vacuum tightness when making plated film maintains 6.5 * 10
-1About Pa, electric current 1A, voltage 200V, pre-sputter sputter coating on substrate again after 2 minutes, 60 minutes plated film time, thickness is about 5 μ m.Fig. 2 a is the Fe alloy film photo of the silicon substrate that obtains after the sputter, can see that film peels off phenomenon with substrate.
The film that plating is good makes the automatic and substrate desquamation of Fe alloy film with distilled water immersion, use then towards model machine and make the disk that diameter is 3mm, carry out two spray attenuates or ion milling again and produce electron microscopic sample, shown in Fig. 2 b, the observed Fe alloy film TEM photo of the present invention's success, the gained Electronic Speculum is clean, even, fine and close with film sample, solved Electronic Speculum with film sample in traditional mechanical reduction process, polluted easily, broken and introduce the problem of illusion.
Embodiment 3
Difference from Example 1 is:
Specimen preparation: the stainless steel after deoiling through acetone, alcohol ultrasonic cleaning respectively is placed in the suds as substrate, soaked 4 minutes, take out air-dryly then, make its surface scribble one deck soap film uniformly; Being negative pole with Ti (purity is 99.9%) target then, is anodal with the stainless steel substrates, adopts following processing parameter on magnetron sputtering coater, is evacuated to the back of the body end vacuum tightness during sputter earlier and reaches 8.0 * 10
-5About Pa, feed purity then and be 99.99% Ar gas, the vacuum tightness when making plated film maintains 6.8 * 10
-1About Pa, electric current 1A, voltage 180V, pre-sputter sputter coating on substrate again after 3 minutes, 80 minutes plated film time, thickness is about 8 μ m.Fig. 3 a is the Ti film photo of the stainless steel substrates substrate that obtains after the sputter, can see that film peels off phenomenon with substrate.
The film that plating is good makes the automatic and substrate desquamation of Ti film with distilled water immersion, use then towards model machine and make the disk that diameter is 3mm, carry out two spray attenuates or ion milling again and produce electron microscopic sample, shown in Fig. 3 b, the observed pure Ti film TEM photo of the present invention's success, the gained Electronic Speculum is clean, even, fine and close with film sample, solved Electronic Speculum with film sample in traditional mechanical reduction process, polluted easily, broken and introduce the problem of illusion.
In addition, metal substrate has also adopted substrates such as Cu, Ni, and the alloys target material has also adopted alloys such as Zr, Mo, La, Mg, all reaches the object of the invention, and obtains effect preferably.
Claims (4)
1, a kind of preparation method of used in transmission electron microscope film sample is characterized in that:
1) utilize magnetically controlled sputter method to produce metallic membrane or alloy film, magnetron sputtering is a negative pole with the metal or alloy target, substrate is anodal, after process acetone, alcohol ultrasonic cleaning are deoiled respectively with substrate, be placed in the suds, soak 1～5 minute time, take out air-dry then, make its surface scribble one deck soap film uniformly, concrete steps and processing parameter are as follows:
A) vacuum chamber is vacuumized, make back of the body end vacuum tightness reach 2.0 * 10
-5～8.0 * 10
-5Pa;
B) feed Ar gas to vacuum chamber, making plated film atmosphere is Ar atmosphere, and vacuum degree control is 6.5 * 10 during with plated film
-1～7.5 * 10
-1Between the Pa scope;
C) sputtering voltage is 100～300V, and target current is 0.5～2A;
D) pre-sputter sputter coating on substrate again after 2～5 minutes, 60～90 minutes plated film time, the thickness that makes film on the substrate is between 5～9 μ m;
2) on described substrate, directly take off utilize magnetically controlled sputter method plate the metal or alloy film, go out the disk that diameter is 3mm then;
3) described disk is carried out two spray attenuates or ion milling and make the sample that electron microscopic observation is used.
2, according to the preparation method of the described used in transmission electron microscope film sample of claim 1, it is characterized in that: described step 2) adopt: will plate good film and make the automatic and substrate desquamation of film, and use then towards model machine and make the disk that diameter is 3mm with distilled water immersion.
3, according to the preparation method of the described used in transmission electron microscope film sample of claim 1, it is characterized in that: described substrate adopts molybdenum, stainless steel, copper or the nickel substrate in the metal substrate; Perhaps adopt glass or monocrystalline substrate in the nonmetal substrate.
4, according to the preparation method of the described used in transmission electron microscope film sample of claim 1, it is characterized in that: described target matter is one of titanium or titanium alloy, iron and iron alloy, copper and copper alloy and zirconium alloy, molybdenum alloy, lanthanum alloy, magnesium alloy.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100205313A CN100360708C (en) | 2004-05-12 | 2004-05-12 | Method for preparing film specimen in use for transmission electron microscope |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100205313A CN100360708C (en) | 2004-05-12 | 2004-05-12 | Method for preparing film specimen in use for transmission electron microscope |
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| Publication Number | Publication Date |
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| CN1696334A CN1696334A (en) | 2005-11-16 |
| CN100360708C true CN100360708C (en) | 2008-01-09 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101581637B (en) * | 2009-06-19 | 2011-08-17 | 武汉钢铁(集团)公司 | Method for preparing electron microscope film sample with silicon steel sheet coating |
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| CN100390524C (en) * | 2006-05-26 | 2008-05-28 | 北京科技大学 | Method for preparing film sample for use in transmitted electron microscope |
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| CN102235945B (en) * | 2010-04-23 | 2013-02-20 | 昆明物理研究所 | Method for preparing amorphous film sample for transmission electron microscope research |
| JP5951223B2 (en) * | 2011-11-02 | 2016-07-13 | 株式会社日立ハイテクノロジーズ | Electron microscopy, electron microscope and observation specimen preparation device |
| CN105675364B (en) * | 2016-01-15 | 2018-03-23 | 中国地质科学院矿产资源研究所 | Preparation method of zircon mineral particle transmission sample |
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| CN109001240B (en) * | 2018-08-17 | 2021-04-13 | 胜科纳米（苏州）有限公司 | Method for preparing non-conductive material sample |
| CN113083979B (en) * | 2021-03-26 | 2023-02-28 | 中国工程物理研究院上海激光等离子体研究所 | Preparation method of self-supporting thin film target component for strong laser loading physical experiment |
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|---|---|---|---|---|
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| JPH04164225A (en) * | 1990-10-29 | 1992-06-09 | Sumitomo Metal Mining Co Ltd | Method of forming sample to be observed by transmission type electron microscope |
| JP2002122524A (en) * | 2000-10-13 | 2002-04-26 | Sumitomo Metal Mining Co Ltd | Method of making sample for transmission electron microscope |
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- 2004-05-12 CN CNB2004100205313A patent/CN100360708C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS62185143A (en) * | 1986-02-10 | 1987-08-13 | Matsushita Electric Ind Co Ltd | Preparation of sample for transmission electron microscope |
| JPH04164225A (en) * | 1990-10-29 | 1992-06-09 | Sumitomo Metal Mining Co Ltd | Method of forming sample to be observed by transmission type electron microscope |
| JP2002122524A (en) * | 2000-10-13 | 2002-04-26 | Sumitomo Metal Mining Co Ltd | Method of making sample for transmission electron microscope |
| CN1464294A (en) * | 2002-06-07 | 2003-12-31 | 清华大学 | Process of transmission electron microscope specimen preparation for easy damp-affecting denaturization crystal thin film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101581637B (en) * | 2009-06-19 | 2011-08-17 | 武汉钢铁(集团)公司 | Method for preparing electron microscope film sample with silicon steel sheet coating |
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| CN1696334A (en) | 2005-11-16 |
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