CN110133020A - A kind of in-situ preparation method of ultra-thin TEM sample and thus obtained ultra-thin TEM film - Google Patents
A kind of in-situ preparation method of ultra-thin TEM sample and thus obtained ultra-thin TEM film Download PDFInfo
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- CN110133020A CN110133020A CN201910339551.3A CN201910339551A CN110133020A CN 110133020 A CN110133020 A CN 110133020A CN 201910339551 A CN201910339551 A CN 201910339551A CN 110133020 A CN110133020 A CN 110133020A
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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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/40—Imaging
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/60—Specific applications or type of materials
- G01N2223/633—Specific applications or type of materials thickness, density, surface weight (unit area)
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/60—Specific applications or type of materials
- G01N2223/645—Specific applications or type of materials quality control
Abstract
The present invention relates to a kind of in-situ preparation methods of ultra-thin TEM sample, include the following steps: S1, carry out the position mark of defect with ion beam etching on the surface of raw sample；S2, reference position label carry out the thick of raw sample and are thinned, and obtain film sample；S3 carries out the fine of film sample and is thinned, obtains the ultra-thin TEM sample for being covered with carbon protective film.The present invention also provides the ultra-thin TEM films obtained according to above-mentioned in-situ preparation method, wherein the thickness of ultra-thin TEM film is less than 30nm.The in-situ preparation method of ultra-thin TEM sample according to the present invention, carbon protective layer therein do not influence transmitted electron image quality.Due to the supporting role of carbon protective layer, in film thinning process, the incidental bend fracture of ultra-thin sample and stripping problem are effectively prevented.
Description
Technical field
The present invention relates to the preparation of TEM sample, relate more specifically to a kind of ultra-thin TEM sample in-situ preparation method and
Thus obtained ultra-thin TEM film.
Background technique
Semiconductor failure analysis has vital effect in terms of the reliability for improving integrated circuit.With integrated level
Raising, the diminution of process, failure analysis faced difficulty also incrementally increase.Transmission electron microscope (TEM) conduct
A kind of very important tool can be used for detecting the features such as structure, pattern, the size of integrated circuit device, while can disclose material
Expect the relationship of microscopic structure and constituent.By the technology, precise positioning and deep characterization to defect are component failure
Basic reason provides strong support.
Present integrated circuit device minimum dimension is contracted to 10nm hereinafter, needing TEM technology in nanometer-Asia Ethylmercurichlorendimide grade scale
Under characteristic size characterization and failure analysis are carried out to device.Therefore, failure analysis must be equipped with corresponding advanced accurate TEM
Technology and TEM sample technology of preparing.A kind of method, that is, focused ion beam electron microscope of conventional effectively preparation TEM sample
(FIB).FIB technique can prepare the TEM sample of 50~100nm thickness.But when preparation TEM sample to 50nm thickness hereinafter,
It is easy to happen the bend fracture or bending breakaway of film sample.How thinner (especially 30nm or less) TEM sample is effectively prepared
Product realize quality, high resolution TEM imaging, are very important demand.
Summary of the invention
In order to solve the above-mentioned problems of the prior art, the present invention is intended to provide a kind of system in situ of ultra-thin TEM sample
Preparation Method and thus obtained ultra-thin TEM film.
The present invention provides a kind of in-situ preparation method of ultra-thin TEM sample, includes the following steps: S1, in the table of raw sample
The position mark of defect is carried out with ion beam etching in face；S2, reference position label carry out the thick of raw sample and are thinned, and obtain film
Sample；S3 carries out the fine of film sample and is thinned, obtains the ultra-thin TEM sample for being covered with carbon protective film.
The step S3 is specifically included: carried out first from the front of film sample it is thinned, until defect for the first time show
Come, next plates carbon protective film in the front；Then continue to be thinned from the back side of film sample, until defect is shown again,
Obtain ultra-thin TEM sample.
Carbon protective film is plated using electron beam in situ.
The step S3 is specifically included: by film sample, integrally interception is come out from raw sample, is moved and is pasted into probe
On TEM sample platform in situ, carries out the fine of film sample and be thinned.
The step S2 is specifically included: cross-sectional sample cutting is carried out, until close to fault location, then cut from the back side,
It is again adjacent to fault location, obtains film sample.
Film sample with a thickness of 500nm.
The present invention also provides the ultra-thin TEM films obtained according to above-mentioned in-situ preparation method, wherein ultra-thin TEM film
Thickness be less than 30nm.Preferably, ultra-thin TEM film with a thickness of 10nm.
The thickness of carbon protective film is less than 50nm.
The in-situ preparation method of ultra-thin TEM sample according to the present invention, using FIB in-situ thinning technology, when defect shows
After out, one layer of C film protective layer is covered in blemish surface, then continues to be thinned from the film sample back side again, until from the back side
Defect is shown again.Last TEM sample is the film sample for being covered with carbon protective layer, and carbon protective layer therein does not influence to transmit
Electronic imaging quality.Due to the supporting role of carbon protective layer, in film thinning process, effectively prevents ultra-thin sample and be easy hair
Raw bend fracture and stripping problem.Particularly, the present invention for existing device feature size (10nm or less) characterization problem with
And corresponding device failure analysis demand, the TEM film sample of 10nm thickness is realized, is provided for high-resolution TEM phenetic analysis
High quality sample.Moreover, preparation method according to the present invention is not necessarily to any other ancillary equipment such as particular sample platform, existing
Have and carried out instrumental function exploitation in equipment and promoted, effectively controls cost.
Detailed description of the invention
Fig. 1 is the process signal of the in-situ preparation method of ultra-thin TEM sample according to a preferred embodiment of the present invention
Figure；
Fig. 2 is the observation schematic diagram of ultra-thin TEM sample according to a preferred embodiment of the present invention.
Specific embodiment
With reference to the accompanying drawing, presently preferred embodiments of the present invention is provided, and is described in detail.
The in-situ preparation method of ultra-thin TEM sample according to a preferred embodiment of the present invention is included in raw sample first
The position mark 12 of defect 11 is carried out with ion beam etching in 1 surface, as shown in figure 1 a) shown in.
Next the in-situ preparation method of ultra-thin TEM sample according to a preferred embodiment of the present invention includes referring to position
Tagging 12 carries out the thick of raw sample 1 and is thinned, i.e., cross-sectional sample is cut, until cut at defect 11, then from the back side,
It is again adjacent at defect 11, the film sample 2 that thickness of sample d is about 500nm at this time, b as shown in figure 1) shown in.
Next the in-situ preparation method of ultra-thin TEM sample according to a preferred embodiment of the present invention includes by film
Sample 2 is whole to be intercepted out, is moved and is pasted on TEM sample platform 3 in situ with probe, c as shown in figure 1) shown in.
Next the in-situ preparation method of ultra-thin TEM sample according to a preferred embodiment of the present invention includes that progress is thin
The fine of membrane sample 2 is thinned.Thinned, d as shown in figure 1 is carried out from the front 21 of film sample 2 first) shown in, until defect 11
Display for the first time, e as shown in figure 1) shown in；Next the carbon for being plated one layer of 50nm thickness in situ using electron beam in the front is protected
Cuticula 4, f as shown in figure 1) shown in；Then continue to be thinned from the back side of film sample 2, until showing defect 11 again, such as scheme
G in 1) shown in, the preparation of ultra-thin TEM sample 5 is completed at this time.
Final TEM sample 5 is the ultra-thin sample 51 for being covered with carbon protective film 4, and the thickness of ultra-thin sample 51 is only 10nm.Its
In, carbon protective film 4 conductive can be suitable for FIB sample making course and be penetrated by electron beam, and transmission TEM electron beam is not stopped to be worn
Saturating ultra-thin sample 51 is suitable for TEM characterization observation, as shown in Figure 2.In this way, passing through the supporting role of carbon protective film 4, avoid
The curling and rupture of ultra-thin sample 51.In fact, the thickness of the carbon protective film 4 can be adjusted according to practical sample preparation, with not
It is preferred more than 50nm.
Above-described, only presently preferred embodiments of the present invention, the range being not intended to limit the invention, of the invention is upper
Stating embodiment can also make a variety of changes.Made by i.e. all claims applied according to the present invention and description
Simply, equivalent changes and modifications fall within the claims of the invention patent.The not detailed description of the present invention is
Routine techniques content.
Claims (8)
1. a kind of in-situ preparation method of ultra-thin TEM sample, which comprises the steps of:
S1 carries out the position mark of defect with ion beam etching on the surface of raw sample；
S2, reference position label carry out the thick of raw sample and are thinned, and obtain film sample；
S3 carries out the fine of film sample and is thinned, obtains the ultra-thin TEM sample for being covered with carbon protective film.
2. in-situ preparation method according to claim 1, which is characterized in that the step S3 is specifically included: first from thin
The front of membrane sample carry out it is thinned, until defect for the first time display, next the front plating carbon protective film；Then from thin
The back side of membrane sample continues to be thinned, until showing defect again, obtains ultra-thin TEM sample.
3. in-situ preparation method according to claim 2, which is characterized in that plate carbon protective film in situ using electron beam.
4. in-situ preparation method according to claim 1, which is characterized in that the step S3 is specifically included: by film sample
Integrally interception comes out product from raw sample, is moved and is pasted on TEM sample platform in situ with probe, carries out finely subtracting for film sample
It is thin.
5. in-situ preparation method according to claim 1, which is characterized in that the step S2 is specifically included: carrying out section
Sample cutting, until close to fault location, then cut from the back side, it is again adjacent to fault location, obtains film sample.
6. in-situ preparation method according to claim 1, which is characterized in that film sample with a thickness of 500nm.
7. the ultra-thin TEM film that in-situ preparation method according to claim 1 to 6 obtains, which is characterized in that
The thickness of ultra-thin TEM film is less than 30nm.
8. ultra-thin TEM film according to claim 7, which is characterized in that the thickness of carbon protective film is less than 50nm.
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| CN201910339551.3A CN110133020A (en) | 2019-04-25 | 2019-04-25 | A kind of in-situ preparation method of ultra-thin TEM sample and thus obtained ultra-thin TEM film |
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| CN201910339551.3A CN110133020A (en) | 2019-04-25 | 2019-04-25 | A kind of in-situ preparation method of ultra-thin TEM sample and thus obtained ultra-thin TEM film |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111208319A (en) * | 2020-01-19 | 2020-05-29 | 中国科学院上海微系统与信息技术研究所 | Preparation method for accurately positioning and preparing fin field effect transistor needle point sample |
| CN111220820A (en) * | 2020-01-19 | 2020-06-02 | 中国科学院上海微系统与信息技术研究所 | Preparation method of atomic probe tip sample for accurately positioning fin field effect transistor |
| CN111366428A (en) * | 2020-03-03 | 2020-07-03 | 上海华力集成电路制造有限公司 | Method for preparing TEM sample by FIB back cut |
| CN111380877A (en) * | 2020-03-30 | 2020-07-07 | 上海华力集成电路制造有限公司 | Preparation method of front-layer defect transmission sample |
| CN114324412A (en) * | 2021-11-16 | 2022-04-12 | 上海华力集成电路制造有限公司 | TEM sample preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111208319A (en) * | 2020-01-19 | 2020-05-29 | 中国科学院上海微系统与信息技术研究所 | Preparation method for accurately positioning and preparing fin field effect transistor needle point sample |
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| CN111366428B (en) * | 2020-03-03 | 2023-06-09 | 上海华力集成电路制造有限公司 | Method for preparing TEM sample by FIB (fiber reinforced plastic) inverted cutting |
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| CN114324412A (en) * | 2021-11-16 | 2022-04-12 | 上海华力集成电路制造有限公司 | TEM sample preparation method |
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Application publication date: 20190816 |