CN105136539A - Method for preparing TEM chip sample - Google Patents
Method for preparing TEM chip sample Download PDFInfo
- Publication number
- CN105136539A CN105136539A CN201510532705.2A CN201510532705A CN105136539A CN 105136539 A CN105136539 A CN 105136539A CN 201510532705 A CN201510532705 A CN 201510532705A CN 105136539 A CN105136539 A CN 105136539A
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- Prior art keywords
- metallic circuit
- chip
- sample
- chip sample
- prepare
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000010884 ion-beam technique Methods 0.000 claims abstract description 19
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000011248 coating agent Substances 0.000 claims description 22
- 238000000576 coating method Methods 0.000 claims description 22
- 238000005520 cutting process Methods 0.000 claims description 8
- 238000010894 electron beam technology Methods 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 230000001154 acute effect Effects 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 7
- 239000002184 metal Substances 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 6
- 230000005540 biological transmission Effects 0.000 description 10
- 230000008859 change Effects 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 3
- 229910001431 copper ion Inorganic materials 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005464 sample preparation method Methods 0.000 description 2
- 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
- 230000003321 amplification Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000005596 ionic collisions Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- -1 silver Chemical class 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides a method for preparing a TEM chip sample. The method includes the steps that a chip comprising a metal circuit is cut by a focused ion beam to form at least one surface exposing the metal circuit, and a carbon layer is deposited on the surface to cover the metal circuit. According to the method for preparing the TEM chip sample, the carbon layer is deposited on the surface exposing the metal circuit and used for protecting the metal circuit exposed out of the surface, in this way, the metal circuit will not make contact with outside air and is prevented from being oxidatively corroded by the outside air, even if the surface is covered with the carbon layer, sample observation in a TEM is not affected, and the success rate of sample preparation is increased.
Description
Technical field
The present invention relates to the field of transmission electron microscope observing chip sample, particularly a kind of method preparing TEM chip sample.
Background technology
Transmission electron microscope (TransmissionElectronMicroscope, be called for short TEM), be called for short transmission electron microscope, to on very thin sample the e-beam projection through accelerating and assemble, ion collision in electronics and sample and change direction, thus produce solid angle scattering, the size of scattering angle and the density of sample, thickness are relevant, therefore can form the different image of light and shade, image will show after amplification, focusing on image device (as video screen, film or photosensitive coupling component).Nowadays transmission electron microscope has very extensively and more and more important application in the every field comprising Integrated circuit analysis, and FIB (FocusedIonbeam, focused ion beam) the sample preparation TEM sample preparation means that to be then semiconductor applications main.
In current chip fabrication techniques, material for making metallic circuit adopts aluminium, nickel, copper etc., in order to improve the intensity of metallic circuit, also can be gold-plated on metallic circuit in subsequent technique, the metals such as silver, encapsulate a chip, often need through multiple working procedure, in this multiple working procedure, the metallic circuit formed and the other parts of chip often change because of the impact of environment, these changes may affect the reliability of chip, the metallic circuit even formed can produce fracture, cause whole chip failure, therefore the chip to these lost efficacy is needed to be analyzed, especially the failure conditions of observing metallic circuit in chip is needed.
At present when using transmission electron microscope observing to contain the chip of metallic circuit, if need the growing state observing metallic circuit, please refer to Fig. 1 and Fig. 2, be generally first by focused ion beam, chip 1 is cut out a sample strip 3 from centre, these sample strip 3 both sides have metallic circuit 2 to expose.In current chip fabrication techniques, metallic circuit 2 material of subsequent growth is generally copper, and copper exposure is easy to oxidized in atmosphere, moreover, copper ion very easily spreads, make the part around metallic circuit 2 cause variation to a certain degree, the both sides therefore causing sample strip 3 easily change original growth complexion, and observation is made a fault.
Therefore for above-mentioned defect, be necessary to improve above-mentioned TEM chip sample preparation method, improve sample preparation success ratio.
Prior art illustrates: 1-chip, 2-metallic circuit, 3-sample strip;
The present invention illustrates: 10-chip, 11-first surface, 12-second surface, 13-the 3rd surface, 14-the 4th surface, 20-metallic circuit, 30-focused ion beam, 40-electron beam, 50-C
10h
8gas, 60-sample strip, 70-carbon-coating, 80-redundance, 90-chip sample sheet.
Summary of the invention
The invention provides a kind of method preparing TEM chip sample; for the problems referred to above; after cutting out the surface of exposing metallic circuit; deposited carbon layer on a surface; protect metallic circuit so not by outside air oxidation corrosion; in transmission electron microscope, carbon-coating does not also affect observation simultaneously, therefore improves the success ratio of sample preparation.
For achieving the above object, the invention provides a kind of method preparing TEM chip sample, chip containing metallic circuit is formed at least one surface of exposing described metallic circuit under focused ion beam cutting, at described surface deposition carbon-coating, described metallic circuit is covered by carbon-coating.
As preferably, comprise the following steps:
Step one: the described chip containing metallic circuit is provided;
Step 2: use described focused ion beam to cut the described chip containing metallic circuit, makes the described chip containing metallic circuit form surface described at least one, described metallic circuit is exposed on described surface;
Step 3: will the reagent for the formation of carbon-coating be loaded in the device being used for launching described focused ion beam, and the described surface emitting electron beam in step 2 and described reagent are bombarded, deposited carbon layer on said surface;
Step 4: remove described containing part untreated on the chip of metallic circuit cutting, make chip sample sheet.
As preferably, in step 2, form four described surfaces.
As preferably, be C for the formation of the reagent of carbon-coating in step 3
10h
8gas.
As preferably, the time of bombarding in step 3 is 20 seconds ~ 30 seconds.
As preferably, be that electron gun is launched for launching the device of described focused ion beam in step 3, the strength of current that described electron gun is launched is 11nA.
As preferably, formed by the transmit direction of the electron beam in described electron gun and described surface, acute angle is 52 °.
As preferably, deposited carbon layer carries out under vacuum on said surface.
As preferably, the carbon layers having thicknesses deposited on said surface is 10nm ~ 50nm.
As preferably, the material of described metallic circuit is copper.
Compared with prior art, the invention has the beneficial effects as follows: the invention provides a kind of method preparing TEM chip sample, chip containing metallic circuit is formed at least one surface of exposing described metallic circuit under focused ion beam cutting, at described surface deposition carbon-coating, described metallic circuit is covered by carbon-coating.Chip sample preparation method provided by the invention makes exposing the surface deposition carbon-coating of metallic circuit; utilize carbon-coating to the metallic circuit protecting surface to expose; metallic circuit is made to contact outside air like this; thus prevent by outside air oxidation corrosion; even if cover carbon-coating on the surface simultaneously; do not affect the observation of sample in transmission electron microscope, therefore improve the success ratio of sample preparation yet.
Accompanying drawing explanation
Fig. 1 is untreated chip sample cut-open view in prior art;
Fig. 2 is the sample strip cut-open view formed after using focused ion beam to cut in prior art;
Fig. 3 is the cut-open view after chips sample of the present invention uses focused ion beam cutting;
Fig. 4 is the cut-open view at chip sample side deposited carbon layer in the present invention;
Fig. 5 is the cut-open view of the sample strip formed after cutting unprocessed portion in the present invention;
Fig. 6 is the process flow diagram that the present invention prepares the method for TEM chip sample.
Embodiment
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, are described in detail the specific embodiment of the present invention below in conjunction with accompanying drawing.
Embodiment one
Please refer to Fig. 6, and composition graphs 3 to Fig. 5, for achieving the above object, the invention provides one and preparing TEM chip sample method, comprising the following steps:
Step one: the chip 10 containing metallic circuit 20 is provided;
Step 2: please refer to Fig. 3, focused ion beam 30 is used to cut the chip 10 containing metallic circuit 20, preferably, the ion gun strength of current being used for transmitting focusing ion beam 30 is adjusted to 100pA ~ 7000pA, focused ion beam 30 is used to cut out two grooves at chip 10 center section, expose the sample strip 60 that intermediate demand carries out observing, the inwall of described two grooves forms first surface 11 successively, second surface 12, 3rd surface 13, 4th surface 14, these four surfaces are parallel to each other, at second surface 12, 3rd surface 13 all there is metallic circuit 20 to expose, usually, the material of these metallic circuits 20 is copper, place easy oxidized corrosion in atmosphere.
Step 3: please refer to Fig. 4, also there is electron gun at the device (not shown) at the ion gun place for transmitting focusing ion beam 30, used in electron gun is in divergent bundle 40, close ion gun, open electron gun, under vacuum, aligning second surface 12 and the 3rd surperficial 13 divergent bundles 40 bombard, the acute angle theta that electron gun and second surface 12 are formed is 52 °, the transmitter current intensity of electron beam 40 is set to 11nA, be furnished with gas injection system in the system at simultaneously electron gun place, this gas injection system discharges C to second surface 12 and the 3rd surperficial 13
10h
8gas 50, this gas molecular link under the scanning of electron beam 40 is bombarded being positioned at second surface 12 and the 3rd surface 13 ruptures, define carbon dust, drop on second surface 12 and the 3rd surface 13, be deposited as carbon-coating 70 gradually, after electron beam 40 launches 20 seconds ~ 30 seconds, close electron gun and gas injection system, stop the deposition of carbon-coating 70, the thickness of the carbon-coating 70 now obtained is 10nm ~ 50nm, make metallic circuit 20 to contact outside air like this, thus prevent metallic circuit 20 by outside air oxidation corrosion.In addition, on second surface 12 and the 3rd surface 13 due to the stop of carbon layer on surface 70, can alleviate copper ion in metallic circuit 20 to neighbouring diffusion, it is rotten that the part that therefore can slow down near metallic circuit 20 occurs due to copper ion diffusion.
Step 4: please refer to Fig. 5, cuts removal by redundance 80, makes chip sample sheet 90.
The chip sample sheet 90 made is put into transmission electron microscope observe, because transmission electron microscope is when observing sample, the pattern of sample penetrates sample to obtain for the incident beam observing sample by launching, and incident beam can penetrate carbon-coating 70 equally, , sample topography is presented, and due to the carbon atom ordinal number in carbon-coating 70 less, therefore the impact (as scattering etc.) for incident beam is very little, make the pattern of the chip sample sheet 90 presented and the consistent appearance not having to present during carbon-coating 70, therefore the carbon-coating 70 be positioned on second surface 12 and the 3rd surface 13 does not affect the observation of transmission electron microscope.
Obviously, those skilled in the art can carry out various change and modification to invention and not depart from the spirit and scope of the present invention.If these amendments of the present invention and modification belong within the scope of the claims in the present invention and equivalent technologies thereof, then the present invention is also intended to comprise these change and modification.
Claims (10)
1. prepare a method for TEM chip sample, it is characterized in that, the chip containing metallic circuit is formed at least one surface of exposing described metallic circuit under focused ion beam cutting, at described surface deposition carbon-coating, described metallic circuit is covered by carbon-coating.
2. prepare the method for TEM chip sample as claimed in claim 1, it is characterized in that, comprise the following steps:
Step one: the described chip containing metallic circuit is provided;
Step 2: use described focused ion beam to cut the described chip containing metallic circuit, makes the described chip containing metallic circuit form surface described at least one, described metallic circuit is exposed on described surface;
Step 3: will the reagent for the formation of carbon-coating be loaded in the device being used for launching described focused ion beam, and the described surface emitting electron beam in step 2 and described reagent are bombarded, deposited carbon layer on said surface;
Step 4: remove described containing part untreated on the chip of metallic circuit cutting, make chip sample sheet.
3. prepare the method for TEM chip sample as claimed in claim 2, it is characterized in that, in step 2, form four described surfaces.
4. preparing as claimed in claim 2 the method for TEM chip sample, it is characterized in that, is C for the formation of the reagent of carbon-coating in step 3
10h
8gas.
5. prepare the method for TEM chip sample as claimed in claim 2, it is characterized in that, the time of bombarding in step 3 is 20 seconds ~ 30 seconds.
6. prepare as claimed in claim 2 the method for TEM chip sample, it is characterized in that, be electron gun for launching the device of described focused ion beam in step 3, the strength of current of described electron gun transmitting is 11nA.
7. prepare as claimed in claim 6 the method for TEM chip sample, it is characterized in that, formed by the transmit direction of the electron beam in described electron gun and described surface, acute angle is 52 °.
8. prepare the method for TEM chip sample as claimed in claim 1 or 2, it is characterized in that, deposited carbon layer carries out under vacuum on said surface.
9. prepare the method for TEM chip sample as claimed in claim 1 or 2, it is characterized in that, the carbon layers having thicknesses deposited on said surface is 10nm ~ 50nm.
10. prepare the method for TEM chip sample as claimed in claim 1 or 2, it is characterized in that, the material of described metallic circuit is copper.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510532705.2A CN105136539B (en) | 2015-08-26 | 2015-08-26 | A method of preparing TEM chip sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510532705.2A CN105136539B (en) | 2015-08-26 | 2015-08-26 | A method of preparing TEM chip sample |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105136539A true CN105136539A (en) | 2015-12-09 |
| CN105136539B CN105136539B (en) | 2019-05-03 |
Family
ID=54721969
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510532705.2A Active CN105136539B (en) | 2015-08-26 | 2015-08-26 | A method of preparing TEM chip sample |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109001018A (en) * | 2018-07-09 | 2018-12-14 | 华慧芯科技（天津）有限公司 | A kind of transmission sample preparation of oxidizable material and two-dimensional material reinforcement means |
| CN110133020A (en) * | 2019-04-25 | 2019-08-16 | 中国科学院上海微系统与信息技术研究所 | A kind of in-situ preparation method of ultra-thin TEM sample and the ultra-thin TEM film obtained therefrom |
| CN113504393A (en) * | 2021-07-07 | 2021-10-15 | 大连理工大学 | Preparation method of environmental atmosphere electron microscope in-situ heating and in-situ electrifying sample |
| CN113834831A (en) * | 2020-06-08 | 2021-12-24 | 宸鸿科技(厦门)有限公司 | Method for preparing transmission electron microscope sample |
| CN114062083A (en) * | 2021-11-22 | 2022-02-18 | 华东师范大学 | Preparation method of wire bonding interface transmission electron microscope sample and method for observing the evolution process of intermetallic compounds |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109001018A (en) * | 2018-07-09 | 2018-12-14 | 华慧芯科技（天津）有限公司 | A kind of transmission sample preparation of oxidizable material and two-dimensional material reinforcement means |
| CN110133020A (en) * | 2019-04-25 | 2019-08-16 | 中国科学院上海微系统与信息技术研究所 | A kind of in-situ preparation method of ultra-thin TEM sample and the ultra-thin TEM film obtained therefrom |
| CN113834831A (en) * | 2020-06-08 | 2021-12-24 | 宸鸿科技(厦门)有限公司 | Method for preparing transmission electron microscope sample |
| CN113834831B (en) * | 2020-06-08 | 2023-07-21 | 全德科技(厦门)有限公司 | Method for preparing transmission electron microscope sample |
| CN113504393A (en) * | 2021-07-07 | 2021-10-15 | 大连理工大学 | Preparation method of environmental atmosphere electron microscope in-situ heating and in-situ electrifying sample |
| CN114062083A (en) * | 2021-11-22 | 2022-02-18 | 华东师范大学 | Preparation method of wire bonding interface transmission electron microscope sample and method for observing the evolution process of intermetallic compounds |
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| CN105136539B (en) | 2019-05-03 |
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