CN108550512A - One kind being used for the multielectrode preparation method of example of transmission electron microscope bar - Google Patents
One kind being used for the multielectrode preparation method of example of transmission electron microscope bar Download PDFInfo
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- CN108550512A CN108550512A CN201810337495.5A CN201810337495A CN108550512A CN 108550512 A CN108550512 A CN 108550512A CN 201810337495 A CN201810337495 A CN 201810337495A CN 108550512 A CN108550512 A CN 108550512A
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- China
- Prior art keywords
- electrode
- preparation
- photoetching
- electron microscope
- transmission electron
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/02—Details
- H01J37/20—Means for supporting or positioning the objects or the material; Means for adjusting diaphragms or lenses associated with the support
-
- 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
- G01N23/22—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 measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
-
- 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
- G01N23/22—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 measuring secondary emission from the material
- G01N23/2204—Specimen supports therefor; Sample conveying means therefore
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
- H01J37/261—Details
Abstract
The invention discloses one kind be used for the multielectrode preparation method of example of transmission electron microscope bar, including electrode plate preparation and gamble piece preparation.Large electrode is obtained using photoetching, solution etches on silicon chip, electron beam lithography, ion beam etching, reactive ion etching, solution etches is reused and obtains four small electrodes.On sapphire gambling piece is obtained using photoetching, solution etches.The two is assembled to obtain a kind of for example of transmission electron microscope bar multi-electrode.Adjacent electrode spacing is between 25 microns to 55 microns.Break through the limitation that conventional electrical specimen holder only has two electrodes（It does not include probe）, provide a kind of preparation method of four electrodes.Some other means for needing to use multi-electrode measurement are implemented in transmission electron microscope.Electricity research of the Electronic Speculum in situ to Material Field is widened.
Description
Technical field
The present invention relates to nano ZnO in-situ test fields, more particularly to one kind being used for example of transmission electron microscope
The multielectrode production method of bar, specially mask etching multi-electrode, punching lead form combined platform.
Background technology
Higher and higher with the integrated level of circuit, during the continuous diminution of device feature size, many problems highlight
Out such as wire interconnection, Bimaterial in terface defect.These problems can cause the reduction of device lifetime even to be failed.Simultaneously
The working mechanism of some devices is also to be solved, such as the transformation mechanism of memory middle dielectric layer under the electric field.Therefore, people
Wish to further understand mechanism and reason that device works with failure, explores new material to improve the stability of device and integrate
Degree.The method of electrical response and military service behavior of the common research micro-nano device under electric field action has electrical characterization and structure at present
Characterization.The device current that electrical characterization for example monitors, which changes with time, is known that the service life of device, and monitoring capacitance with voltage becomes
Change can obtain defect distribution of device inside etc..But electrical characterization cannot intuitively see the change of device under voltage
Change, thus can not be from microcosmic upper parsing device mechanism and stability.Transmission electron microscope, which is one kind, can characterize material atom
The means of structure.With the development of technology, in situ TEM can apply electricity in traditional transmission electron microscope
, it is a kind of strong means of electrical response and military service behavior of the research micro-nano device under electric field action.But it uses at present
It is Two-port netwerk electrode in carrying the specimen holder in situ of micro-nano device sample, electricity is deposited at sample both ends based on focused ion beam technology
Pole measures.Even by the contact of probe also only there are three port, the measurement of other electrical datas, such as electricity cannot be satisfied
Conductance etc..And pressing for probe tip is easily damaged sample, therefore need significant care careful in operation.Therefore such as
What carries out multielectrode preparation and carries out electricity and the dynamic characterization of microstructure in the case where not damaging sample to be current
A problem.
Invention content
The purpose of the invention is to overcome the prior art to monitor nano-device atomic structure in situ to drill in electric field environment
The deficiency of change proposes a kind of for the multielectrode production method of example of transmission electron microscope bar.This method can provide four
Fixed electrode, is higher than traditional two fixed electrodes（It does not include traveling probe）.
Realizing the specific technical solution of the object of the invention is：
A kind of preparation method for transmission electron microscope multi-electrode specimen holder, this method include step in detail below：
Step 1：The preparation of electrode plate
ⅰ）The silicon nitride that two-sided deposition thickness is 300~700 nanometers on silicon chip, as protective layer；
ⅱ）In a face splash-proofing sputtering metal of deposit matcoveredn silicon chip, which is known as front；
ⅲ）In positive spin coating photoresist, then photolithography patterning, etches the shape of electrode；
ⅳ）Use corresponding metal etch solution etches metal；
ⅴ）Wet method is removed photoresist, and large electrode is molded at this time；
ⅵ）Ion beam etching electrode is used in combination in the shape for carving four small electrodes using electron beam lithography on large electrode, small at this time
Electrode moulding, wherein on intermediate two shorter small electrodes with same process photoetching, etch electrode circular hole respectively；
ⅶ）Back side photoetching, alignment exposure, the distance that small electrode exposes can be determined according to the position of photoetching；
ⅷ）Reactive ion etching silicon nitride, until cutting through back side silicon nitride silicon；
ⅸ）Wet etching corrodes silicon.
ⅹ）Reactive ion etching keeps small electrode hanging from the positive silicon nitride of back-etching, exposure small electrode；It obtains described
Electrode plate.
Step 2：Gamble the preparation of piece
ⅰ）Select sapphire as gambling piece substrate, and in its surface splash-proofing sputtering metal；
ⅱ）It is carved graphically in the gambling piece substrate glazing of splash-proofing sputtering metal, draws four block length square-shaped electrode regions；
ⅲ）Use corresponding metal etch solution etches metal；
ⅳ）Photoetching, sapphire middle position etch a penetrating rectangle, are used for the assembling of electrode plate；
ⅴ）Photoetching, in step II）It is formed by four rectangular electrodes and etches four circular holes respectively for being led across metal
Line, four electrodes on connection electrode plate；The gambling piece is made；
Step 3：Assembling
ⅰ）Electrode plate is inserted into the penetrating rectangle that gambling piece center etches, plain conductor is used in combination to weld；Obtain described be used for
The multi-electrode of example of transmission electron microscope bar.
The splash-proofing sputtering metal is chrome gold or titanium/gold.
The metal etch solution is to remove golden liquid, remove chrome liquor or remove titanium liquid.
Beneficial effects of the present invention：Break through the limitation that conventional electrical specimen holder only has two electrodes（It does not include probe）, provide
A kind of preparation method of four electrodes.Allow some other means for needing to use multi-electrode measurement in transmission electron microscopy
Implement in mirror.Electricity research of the Electronic Speculum in situ to Material Field is widened.
Description of the drawings
Fig. 1 is multi-electrode electrode plate preparation technology flow chart；
Fig. 2 is gambling piece schematic diagram；
Fig. 3 is multi-electrode electrode plate schematic top plan view；
Fig. 4 is gambling piece and multi-electrode electrode plate assembling schematic diagram；
Fig. 5 is the optics picture of multi-electrode electrode plate.
In figure：1- silicon chips；2- silicon nitrides；3- metals；4- photoresists；5- electrode circular holes；The penetrating rectangles of 6-；7- gambles piece；
8- samples to be tested；9- electrode plates；10- gambles plate electrode circular hole.
Specific implementation mode
With reference to the accompanying drawings and embodiments, the present invention is described in further detail.Implement process, the item of the present invention
Part, experimental method etc. are among the general principles and common general knowledge in the art in addition to the following content specially referred to, the present invention
Content is not particularly limited.
Embodiment
Refering to fig. 1, the present invention includes：
1）The preparation of electrode plate
Step 1：In 1 two-sided deposit of silicon chip, 300 nanometers of silicon nitride 2, as protective layer.
Step 2：Chrome gold 3, chromium are sputtered in the one side of deposit matcoveredn silicon chip:5-10nm, gold：50-60nm, to distinguish
Step 1 is mentioned two-sided, and the face of step 2 sputtering is known as front.
Step 3：On the basis of step 2, conventional lithography process is used（Skin drying applies HMDS, gluing 4（Glue kind：
9920））, front baking, exposure, development（1 minute）, sweep counterdie（30 seconds）, solid glue（140 degrees Celsius, 1 minute））Front litho pattern
Change, etches the shape of electrode.
Step 4：Using going golden liquid to etch gold, etches 20 seconds, place into chrome liquor, etch 30 seconds.
Step 5：It is put into acetone soak to remove photoresist for 15 minutes, large electrode is molded at this time.
Step 6：The shape for carving four small electrodes using electron beam lithography on large electrode is used in combination ion beam etching electric
Pole, at this time small electrode be molded, on intermediate two shorter small electrodes with same process photoetching, etching electrode circular hole 5 respectively.
Step 7：Back side photoetching（Glue kind 9920）, it is directed at exposure, can determine what small electrode exposed according to the position of photoetching
Distance.
Step 8：Reactive ion etching silicon nitride, until cutting through back side silicon nitride silicon.
Step 9：Use a concentration of 33% potassium hydroxide solution corrosion of wet etching 5 hours silicon at 80 degrees celsius.
Step 10：Reactive ion etching keeps small electrode hanging, obtains from the positive silicon nitride of back-etching, exposure small electrode
The electrode plate 9.
2）Gamble the preparation of piece
Step 1：It is 0.3 millimeter of 2 cun of sapphires as substrate to select thickness, slice be made a length of 4 millimeters, width be 2.4 millimeters
Cuboid, and its surface sputter chrome gold.
Step 2：Photolithography patterning on the basis of step 1 draws 1.4 millimeters of four block length, wide 1 millimeter of rectangle electricity
Polar region domain, horizontally adjacent 0.2 millimeter of four rectangles are vertically adjacent to 0.4 millimeter, as shown in Figure 2.
Step 3：Using go golden liquid and go chrome liquor etch Jin Hege.
Step 4：Photoetching, sapphire middle position etch a penetrating rectangle 6, are used for the assembling of electrode plate 9, such as
Shown in Fig. 2.
Step 5：Photoetching etches the circular hole 10 of four 0.4 millimeter of diameters respectively on being formed by four rectangular electrodes
For passing through plain conductor, four electrodes on connection electrode plate 9, as shown in Figure 2.
3）Assembling
Step 1：By electrode plate 9（As shown in Figure 3）It is inserted into 7 center of gambling piece to etch in the penetrating rectangle 6 come, metal is used in combination
Conducting wire connection electrode：Longer electrode is connected in respectively on two electrodes above gambling piece 7 on electrode plate 9, shorter on electrode plate 9
Two electrodes metal wire passes through the circular hole 5 on two noncontinuous electrodes to be connected with two electrodes below gambling piece, as shown in Figure 4.
Fig. 5 is the optical photograph of made electrode plate 9, and adjacent electrode spacing is between 25 microns to 55 microns.
Probe can be used to carry out required operation simultaneously during sample test.
Claims (3)
1. a kind of preparation method for transmission electron microscope multi-electrode specimen holder, which is characterized in that this method includes following
Specific steps：
Step 1：The preparation of electrode plate
ⅰ）The silicon nitride that two-sided deposition thickness is 300~700 nanometers on silicon chip, as protective layer；
ⅱ）In a face splash-proofing sputtering metal of deposit matcoveredn silicon chip, which is known as front；
ⅲ）In positive spin coating photoresist, then photolithography patterning, etches the shape of electrode；
ⅳ）Use corresponding metal etch solution etches metal；
ⅴ）Wet method is removed photoresist, and large electrode is molded at this time；
ⅵ）Ion beam etching electrode is used in combination in the shape for carving four small electrodes using electron beam lithography on large electrode, small at this time
Electrode moulding；Wherein, on two small electrodes with same process photoetching, respectively etch electrode circular hole；
ⅶ）Back side photoetching, alignment exposure, the distance exposed according to the location determination small electrode of photoetching；
ⅷ）Reactive ion etching silicon nitride, until cutting through back side silicon nitride silicon；
ⅸ）Wet etching corrodes silicon；
ⅹ）Reactive ion etching keeps small electrode hanging from the positive silicon nitride of back-etching, exposure small electrode；The electrode is made
Plate；
Step 2：Gamble the preparation of piece
ⅰ）Select sapphire as gambling piece substrate, and in its surface splash-proofing sputtering metal；
ⅱ）It is carved graphically in the gambling piece substrate glazing of splash-proofing sputtering metal, draws four block length square-shaped electrode regions；
ⅲ）Use corresponding metal etch solution etches metal；
ⅳ）Photoetching, sapphire middle position etch a penetrating rectangle；
ⅴ）Photoetching, in step II）It is formed by four rectangular electrodes and etches four circular holes respectively；The gambling piece is made；
Step 3：Assembling
ⅰ）Electrode plate is inserted into the penetrating rectangle that gambling piece center etches, plain conductor is used in combination to weld；Obtain described be used for
The multi-electrode of example of transmission electron microscope bar.
2. according to the method described in claim 1, it is characterized in that, the splash-proofing sputtering metal is chrome gold or titanium/gold.
3. according to the method described in claim 1, it is characterized in that, the metal etch solution is to remove golden liquid, remove chrome liquor or go
Titanium liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810337495.5A CN108550512A (en) | 2018-04-16 | 2018-04-16 | One kind being used for the multielectrode preparation method of example of transmission electron microscope bar |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810337495.5A CN108550512A (en) | 2018-04-16 | 2018-04-16 | One kind being used for the multielectrode preparation method of example of transmission electron microscope bar |
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| Publication Number | Publication Date |
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| CN108550512A true CN108550512A (en) | 2018-09-18 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201810337495.5A Pending CN108550512A (en) | 2018-04-16 | 2018-04-16 | One kind being used for the multielectrode preparation method of example of transmission electron microscope bar |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006015167A2 (en) * | 2004-07-28 | 2006-02-09 | The Board Of Trustees Of The University Of Illinois | Tem mems device holder and method of fabrication |
| CN101275895A (en) * | 2008-01-04 | 2008-10-01 | 中国科学院物理研究所 | Sample platform system for in-situ measuring Na electronic device property in transmission electron microscope |
| CN102983049A (en) * | 2012-11-22 | 2013-03-20 | 北京大学 | Transmission electron microscope sample bearing device |
| CN103411982A (en) * | 2013-07-05 | 2013-11-27 | 东南大学 | Transmission electron microscope (TEM) sample stage for measuring solid-liquid phase interface electrochemical reaction in situ |
| CN103531424A (en) * | 2013-10-14 | 2014-01-22 | 东南大学 | Transmission electron microscope sample table of in-situ measurement nanometer device |
| CN103928279A (en) * | 2013-01-15 | 2014-07-16 | Fei公司 | Sample carrier for an electron microscope |
| US20170003243A1 (en) * | 2015-07-01 | 2017-01-05 | Honda Motor Co., Ltd. | Analytical cell and method of producing the same |
-
2018
- 2018-04-16 CN CN201810337495.5A patent/CN108550512A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006015167A2 (en) * | 2004-07-28 | 2006-02-09 | The Board Of Trustees Of The University Of Illinois | Tem mems device holder and method of fabrication |
| CN101275895A (en) * | 2008-01-04 | 2008-10-01 | 中国科学院物理研究所 | Sample platform system for in-situ measuring Na electronic device property in transmission electron microscope |
| CN102983049A (en) * | 2012-11-22 | 2013-03-20 | 北京大学 | Transmission electron microscope sample bearing device |
| CN102983049B (en) * | 2012-11-22 | 2015-07-29 | 北京大学 | Sample for use in transmitted electron microscope bogey |
| CN103928279A (en) * | 2013-01-15 | 2014-07-16 | Fei公司 | Sample carrier for an electron microscope |
| CN103411982A (en) * | 2013-07-05 | 2013-11-27 | 东南大学 | Transmission electron microscope (TEM) sample stage for measuring solid-liquid phase interface electrochemical reaction in situ |
| CN103531424A (en) * | 2013-10-14 | 2014-01-22 | 东南大学 | Transmission electron microscope sample table of in-situ measurement nanometer device |
| US20170003243A1 (en) * | 2015-07-01 | 2017-01-05 | Honda Motor Co., Ltd. | Analytical cell and method of producing the same |
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Application publication date: 20180918 |
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