CN110501356A - The method for supporting film to influence TEM sample image quality to eliminate carbon - Google Patents

The method for supporting film to influence TEM sample image quality to eliminate carbon Download PDF

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Publication number
CN110501356A
CN110501356A CN201910788056.0A CN201910788056A CN110501356A CN 110501356 A CN110501356 A CN 110501356A CN 201910788056 A CN201910788056 A CN 201910788056A CN 110501356 A CN110501356 A CN 110501356A
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CN
China
Prior art keywords
carbon
sample
film
tem
circular hole
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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.)
Pending
Application number
CN201910788056.0A
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Chinese (zh)
Inventor
陈柳
高金德
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Shanghai Huali Integrated Circuit Manufacturing Co Ltd
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Shanghai Huali Integrated Circuit Manufacturing Co Ltd
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Priority to CN201910788056.0A priority Critical patent/CN110501356A/en
Publication of CN110501356A publication Critical patent/CN110501356A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating 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
    • G01N23/02Investigating 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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating 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
    • G01N23/20Investigating 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
    • G01N23/20008Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
    • G01N23/2005Preparation of powder samples therefor
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/03Investigating materials by wave or particle radiation by transmission
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/05Investigating materials by wave or particle radiation by diffraction, scatter or reflection
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/10Different kinds of radiation or particles
    • G01N2223/102Different kinds of radiation or particles beta or electrons
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/60Specific applications or type of materials
    • G01N2223/61Specific applications or type of materials thin films, coatings

Abstract

The method that the invention discloses a kind of to support film to influence TEM sample image quality to eliminate carbon, the circular hole to form 4~6 μm of multiple diameters is processed to continuous carbon support film with FIB, and TEM sample is placed in the circular hole position, complete observing samples under subsequent TEM brightfield mode.The present invention effectively can differentiate and measure the thickness of nano-level thin-membrane, improve the sample preparation efficiency of TEM sample.

Description

The method for supporting film to influence TEM sample image quality to eliminate carbon
Technical field
The present invention relates to the failure analysis fields of semiconductor chip manufacturing, more particularly to one kind to eliminate carbon branch Hold the method that film influences ultra-thin TEM (transmission electron microscope) sample image quality.
Background technique
In semiconductor integrated circuit manufacture, processing procedure is smaller and smaller at present, needs to be carried out with FIB (focused ion beam) Demand of the sample preparation in turn with TEM observation is also more and more.For some lesser processing procedures, especially 28/14 nanometer and with Under, the demand for needing to observe different ultra-thin medium thickness degree (generally Nano grade) is more and more common.
There are two types of the method for preparing TEM sample with FIB now is usual:
One is conventional TEM method for making sample, i.e., are directly prepared into about 80 nanometers of thickness of TEM sample with FIB, then use glass Thin slice TEM sample is extracted to get up to be placed on continuously distributed carbon support film from silicon chip surface by Electrostatic Absorption and be carried out by glass needle tubing TEM observation.The advantages of this method is: sample preparation speed fast (about 45 minutes or so) can comparatively fast obtain TEM result;Disadvantage Be: when sample preparation obtains it is blocked up when just can not carry out reprocessing be prepared for.In addition, the carbon due to about 30 nanometers of thickness supports film In the presence of will affect the clarity of image, cause the film thickness of Nano grade can not accurate measurement.
Another method is the sample that about 500 ran of thickness is first made with FIB, then indoor with FIB chamber is located at Extraction sample mode system in sample extraction to pectination copper ring, will finally carry out finishing and be made about 40 in FIB board in situ The considerable sample of the TEM of nanometer thickness.This method do not have carbon support film stop, can with some nanoscale thickness of accurate measurement, Image clearly.But its sample preparation time, speed was slower relatively long (about 2-3 hours or so).
Film thickness employed in the advanced process of 14nm is typically all (the generally 1~2nm) of Nano grade at present, The TEM observation effect obtained using conventional sample preparation means has been unable to satisfy analysis gradually and required.It is past during actual observation Toward because film thickness can not accurately measuring and need to prepare sample using extracting sample mode in relatively time consuming laborious FIB board Product, the time of such method of preparing sample are twice or more of conventional method of preparing sample;Although and conventional method of preparing sample in time compared with To save, but sample is placed on carbon and supports on film, when TEM is observed, the carbon branch with certain thickness (generally 20~30nm) Hold film will image quality to sample and constituent analysis affect, cause film contrast to be deteriorated, the interface between different films It is less susceptible to differentiate, and then influences thickness measuring, additional carbon signal also can bring interference to the constituent analysis of film.
Summary of the invention
The technical problem to be solved in the present invention is to provide one kind to support film to influence TEM sample image quality to eliminate carbon Method, effectively can differentiate and measure the thickness of nano-level thin-membrane, improve the sample preparation efficiency of TEM sample.
In order to solve the above technical problems, the side of the invention for supporting film to influence TEM sample image quality to eliminate carbon Method adopts the following technical scheme that realization:
The circular hole to form 4~6 μm of multiple diameters is processed to continuous carbon support film with FIB, and in the circular hole TEM sample is placed in position, completes observing samples under subsequent TEM brightfield mode.
Using method of the invention by the transformation to continuously distributed carbon support film, carbon can be effectively eliminated and support film pair Picture quality brought by TEM sample observation and the interference in terms of elemental analysis;Achievable less conventional TEM system of taking time Sample loading mode goes to prepare sample, and its TEM observation effect can be observed with more other method of preparing sample of taking time TEM obtained Effect compares favourably, so as to effectively differentiate and measure the thickness of nano-level thin-membrane, due to there is no carbon that film is supported to stop, acquisition Image clearly, film level can be differentiated clearly, and interface is obvious, convenient for measuring.
Detailed description of the invention
Present invention will now be described in further detail with reference to the accompanying drawings and specific embodiments:
Fig. 1 is the method schematic diagram for supporting film to influence TEM sample image quality to eliminate carbon.
Specific embodiment
The method for supporting film to influence ultra-thin (nanoscale) TEM sample image quality to eliminate carbon, it is intended to eliminate Carbon formwork film to the TEM sample carried thereon when TEM is observed to interference brought by image image quality and elemental analysis, Ideal TEM sample observation effect is obtained with time-consuming less conventional FIB method of preparing sample to realize, it is final to realize The resolution of heterogeneity nano-level thin-membrane and thickness accurate measurement in 28nm/14nm processing procedure, while being also beneficial to improve TEM sample Sample preparation efficiency.
The method for supporting film to influence TEM sample image quality to eliminate carbon, in the following embodiments, specifically Implementation it is as follows:
Step 1: supporting film to reprocess in existing carbon using FIB, film is supported to pass through OM (optical microscopy) flatness in carbon It is placed in FIB, reduces the scope after confirmation, support film quality with E-Beam (electron beam) confirmation carbon again, find dreamboat area Domain.
Step 2: switching under I-Beam (ion beam) window, in the dreamboat region, continuous carbon is supported Film (52 °) under high angle carefully repairs carbon using I-Beam 90pA electric current and supports film, gets 4~6 μm of circular holes, makes mesh The blocking that mark region does not have carbon to support film.It can once support to process multiple similar circular holes on film in carbon, to reach same Carbon supports the purpose that multiple TEM samples are placed on film.
Step 3: supporting film to remove in the carbon in circular hole, by the sample normally cut, (i.e. conventional method for making sample is cut Sample) sample is placed into using electrostatic using the glass electrostatic needle tubing of sample extraction system instrument before the round hole accomplished fluently Hole area realizes that sample area avoids carbon and supports film.
Complete observing samples under subsequent TEM brightfield mode.The TEM sample being arranged so that is put into transmission electron microscope Middle observation, the available image with the equal quality using the TEM sample for extracting the preparation of sample method for making sample in FIB board are imitated Fruit, to realize the observation requirements of each layer nanometer grade thickness film while saving the sample preparation time.
As shown in connection with fig. 1, top half is using the observation area 3 before the present invention in figure, and electron beam penetrates carbon when TEM is observed Support film 2 and sample 1, the thickness entirely observed is including the thickness that carbon supports film 2.Lower half portion is after applying the present invention in figure Observation area 4, TEM observe when electron beam only penetrate sample 1, do not include carbon support film 2.
Above by specific embodiment, invention is explained in detail, but these are not constituted to of the invention Limitation.Without departing from the principles of the present invention, those skilled in the art can also make many modification and improvement, these It should be regarded as protection scope of the present invention.

Claims (5)

1. a kind of method for supporting film to influence TEM sample image quality to eliminate carbon, which is characterized in that with FIB to continuous Carbon support film to process the circular hole to form 4~6 μm of multiple diameters, and place TEM sample in the circular hole position.
2. the method as described in claim 1, it is characterised in that: the method for supporting film processing to carbon is that carbon is supported to film warp It is placed in FIB, reduces the scope after crossing the confirmation of OM flatness, support film quality with electron beam confirmation carbon again, find dreamboat Region.
3. the method as described in claim 1, it is characterised in that: the method for forming multiple 4~6 μm of diameter of circular holes It is under ion beam window, in the dreamboat region, to support film to use ion beam under high angle in continuous carbon 90pA electric current processes carbon and supports film, gets multiple 4~6 μm of circular holes, makes to support in the circular hole of target area without carbon The blocking of film.
4. method as claimed in claim 3, it is characterised in that: the high angle is 52 °.
5. the method as described in claim 1, it is characterised in that: the method for placing TEM sample in the circular hole position It is to support film to remove in the carbon in circular hole, the sample normally cut is used to the glass electrostatic of sample extraction system instrument The circular hole area that needle tubing is accomplished fluently before sample is placed into using electrostatic.
CN201910788056.0A 2019-08-26 2019-08-26 The method for supporting film to influence TEM sample image quality to eliminate carbon Pending CN110501356A (en)

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Publication number Priority date Publication date Assignee Title
CN111896571A (en) * 2020-07-27 2020-11-06 上海华力集成电路制造有限公司 Method for correcting imaging direction of TEM sample

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Application publication date: 20191126