CN105987836B - Tem sample and preparation method thereof - Google Patents
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Abstract
This application provides a kind of TEM samples and preparation method thereof.The preparation method includes：Step S1, the weight content by the mixing drop organic filler in the surface of sample to be prepared, mixed liquor for being dispersed with organic filler are 10~20%；Step S2 makes mixed liquor enter in sample to be prepared and obtains pretreatment TEM sample；And step S3, pretreatment TEM sample is handled using FIB boards, obtains TEM sample.Organic matter is dispersed into mixed liquor by the preparation method first, so that the concentration and surface tension of organic filler reduce, and then be conducive to diffusion of the mixed liquor into sample to be prepared, then by mixing drop in the surface of sample to be prepared, the displacement that the external force that directly coating is formed causes suspension structure is avoided；After obtaining pretreatment TEM sample, due to realizing substantive connection between suspension structure and matrix, when being handled using FIB boards, the damage to suspension structure will not be caused.
Description
Technical field
This application involves technical field of manufacturing semiconductors, in particular to a kind of TEM sample and preparation method thereof.
Background technology
With the development of semiconductor integrated circuit micrometer-nanometer processing technology and ultraprecise mechanical manufacturing technology, MEMS (micro-
Electro-mechanical systems) technology is also maked rapid progress, and there are many suspension structures in MEMS system
The presence of (floating structures), to realize certain mechanical functions.
Currently, transmission electron microscope (TEM) is increasingly used in by observing semiconductor device features to semiconductor
Device carries out failure analysis.Since the principle of TEM is that electronic diffraction penetrates sample imaging, TEM method sample preparations are wanted
It asks very high, usually requires that the thickness of sample no more than 0.1 micron.The semiconductor device structure grown on chip is stacking row
Row, when being located at the object construction of some semiconductor devices of bottom as TEM using on full wafer chip, it is necessary to which preparation includes
Object construction and the sample for meeting TEM sample thickness requirement.In the prior art, focused ion beam (FIB) board can be in full wafer
The regional area of chip completes the preparation of TEM sample, and process is that the sample of FIB boards is placed on using chip as sample levels
On platform, ion beam for being extracted from the liquid metal ion source of FIB boards (generally gallium Ga) is by acceleration, quality analysis, whole
The focused ion beam (I beam) with certain line and ion beam spot diameter is formed after the processing such as shape, focuses on sample surfaces
The regional area for bombarding chip, to carry out cutting and microfabrication preparation TEM sample to chip.
But the suspension structure in MEMS system brings bigger challenge to the preparation of TEM sample.For example it if to see
The stacks of thin films (film stack) for surveying top layer structure, according to conventional FIB methods come when preparing TEM sample, energetic ion
In beam cutting process, suspension structure can be caused suspension structure to be detached with matrix by larger injury, as depicted in figs. 1 and 2,
Final sample prepares failure.Therefore, it is necessary to upper layer suspension structure is tamped by fillers such as organic matters, but due to suspending
Structure closeness is larger, and intermediate gaps are smaller, and organic matter is difficult to overcome itself surface tension and be filled into below suspension structure；
In addition, the connection of suspension structure and lower section matrix is more fragile, external force when applying organic matter layer is easy so that suspension structure moves
Position, and then the result for making TEM measure is inaccurate.
Invention content
The application is intended to provide a kind of TEM sample and preparation method thereof, to solve that suspension structure exists in the prior art
TEM sample is difficult to the problem of preparing.
To achieve the goals above, according to the one side of the application, TEM sample preparation method, the preparation side are provided
Method includes：Step S1 will be dispersed with mixing drop organic filling in the surface of sample to be prepared, mixed liquor of organic filler
The weight content of object is 10~20%；Step S2 makes mixed liquor enter in sample to be prepared and obtains pretreatment TEM sample；And
Step S3 handles pretreatment TEM sample using FIB boards, obtains TEM sample.
Further, above-mentioned steps S1 includes that will mix drop in the surface of the close suspension structure of sample to be prepared.
Further, above-mentioned steps S1 uses dropper with the dropwise addition of the dripping quantity progress mixed liquor of 0.01~0.5ml/ drops.
Further, above-mentioned steps S1 further includes the preparation process of mixed liquor, and preparation process includes：By organic filler with
Dispersant is mixed, and pre-composition is formed；Pre-composition is ultrasonically treated, mixed liquor is obtained.
Further, the frequency of above-mentioned ultrasound is 20~40kHz, and the time of supersound process is 5~10min.
Further, above-mentioned dispersant is selected from acetone, ethyl alcohol, chloroform, dichloroethylene, tetrachloro-ethylene, ether and acetaldehyde group
At group in any one.
Further, above-mentioned organic filler is the soluble matter and lyotrope of dispersant.
Further, above-mentioned steps S2 includes carrying out vacuumize process to the sample to be prepared that surface has mixed liquor to obtain
Pre-process TEM sample.
Further, the negative pressure that vacuumize process is formed in above-mentioned steps S2 is 100~150torr.
Further, the draw vacuum duration of above-mentioned steps S2 is 10~20min.
According to the another aspect of the application, a kind of TEM sample is provided, changes TEM sample and is prepared using above-mentioned preparation method
It forms.
Using the technical solution of the application, organic matter is dispersed into mixed liquor first so that the concentration of organic filler and
Surface tension reduces, and then is conducive to diffusion of the mixed liquor into sample to be prepared, then will mix drop in sample to be prepared
Surface, the displacement of suspension structure is caused so as to avoid the external force that direct coating is formed；Obtain pretreatment TEM sample it
Afterwards, due to realizing substantive connection between suspension structure and matrix, when being handled using FIB boards, using this
The common treatment conditions in field can avoid causing the damage to suspension structure.
Description of the drawings
The accompanying drawings which form a part of this application are used for providing further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation do not constitute the improper restriction to the application for explaining the application.In the accompanying drawings：
Fig. 1 shows a kind of E-beam testing result figures of the suspension structure of MEMS in the prior art；
Fig. 2 shows TEM testing results of the MEMS with suspension structure shown in Fig. 1 using the FIB TEM samples prepared
Figure；
Fig. 3 shows the flow diagram of preparation method provided by the present application；
Fig. 4-shows the E-beam testing result figures of the TEM sample of embodiment 1；And
Fig. 5 shows the E-beam testing result figures of the TEM sample of comparative example 1.
Specific implementation mode
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific implementation mode, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
Be also intended to include plural form, additionally, it should be understood that, when in the present specification using belong to "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or combination thereof.
For ease of description, herein can with use space relative terms, as " ... on ", " in ... top ",
" ... upper surface ", " above " etc., for describing such as a device shown in the figure or feature and other devices or spy
The spatial relation of sign.It should be understood that spatially relative term is intended to comprising the orientation in addition to device described in figure
Except different direction in use or operation.For example, if the device in attached drawing is squeezed, it is described as " in other devices
It will be positioned as " under other devices or construction after part or construction top " or the device of " on other devices or construction "
Side " or " under other devices or construction ".Thus, exemplary term " ... top " may include " ... top " and
" in ... lower section " two kinds of orientation.The device can also other different modes positioning (be rotated by 90 ° or be in other orientation), and
And respective explanations are made to the opposite description in space used herein above.
Now, the illustrative embodiments according to the application are more fully described with reference to the accompanying drawings.However, these are exemplary
Embodiment can be implemented by many different forms, and should not be construed to be limited solely to embodiment party set forth herein
Formula.It should be understood that thesing embodiments are provided so that disclosure herein is thoroughly and complete, and these are shown
The design of example property embodiment is fully conveyed to those of ordinary skill in the art, in the accompanying drawings, for the sake of clarity, expands layer
With the thickness in region, and make that identical device is presented with like reference characters, thus description of them will be omitted.
As background technology is introduced, the suspension structure closeness in existing MEMS system is larger, and intermediate gaps are smaller,
Organic matter is difficult to overcome itself surface tension and be filled into below suspension structure；In addition, the company of suspension structure and lower section matrix
Connecing that comparison is fragile, external force when applying organic matter layer is easy so that suspension structure displacement, and then the result for making TEM measure is inaccurate,
In order to solve the problems, such as mentioned above due to there are caused by suspension structure, present applicant proposes a kind of TEM sample preparation method,
Wherein Fig. 3 shows the flow diagram of the preparation method, which includes：Step S1 will be dispersed with organic filler
Mixing drop in the surface of sample to be prepared；Step S2 makes mixed liquor enter in sample to be prepared, obtains pretreatment TEM samples
Product；And step S3, pretreatment TEM sample is handled using FIB boards, obtains TEM sample.
Organic matter is filled into sample to be prepared using above-mentioned preparation method, organic matter is dispersed into mixed liquor first, is made
The concentration and surface tension for obtaining organic filler reduce, and then are conducive to diffusion of the mixed liquor into sample to be prepared, then will
Drop is mixed in the surface of sample to be prepared, the displacement of suspension structure is caused so as to avoid the external force that direct coating is formed；
After obtaining pretreatment TEM sample, due to realizing substantive connection between suspension structure and matrix, using FIB machines
When platform is handled, it can avoid causing the damage to suspension structure using treatment conditions commonly used in the art.Wherein, the application
The surface tension of organic filler can be reduced as much as possible using dispersion dilution agent organic filler, and content of organics is got over
More, the surface tension of mixed liquor is bigger, thus in mixed liquor organic filler content it is more fewer better；But organic filler
Content is fewer, and the time that mixed liquor fills sample to be prepared longer can cause collateral damage to sample, by applicant to available
It is studied in the organic matter dosage of the application, it is determined that the weight content of organic filler is 10%~20% in mixed liquor.
When drop will be mixed in the surface of sample to be prepared, in order to make suspension knot of the mixed liquor to sample to be prepared as early as possible
It is permeated in structure, the step S1 of preferably above-mentioned preparation method includes that will mix drop in the table of the close suspension structure of sample to be prepared
Face.
In addition, when drop will be mixed in the surface of sample to be prepared, the pressure dripped is avoided droplets to sample to be prepared
Suspension structure caused by accidental injury, the step S1 of preferably above-mentioned preparation method uses dropper with the drop of 0.01~0.5ml/ drops
Dosage carries out the dropwise addition of mixed liquor.
It is excellent in order to make organic matter sufficiently uniformly be scattered in mixed liquor in a kind of preferred embodiment of the application
Choose state preparation method step S1 further include mixed liquor preparation process, preparation process includes：By organic filler and dispersion
Agent is mixed, and pre-composition is formed；Pre-composition is ultrasonically treated, mixed liquor is obtained.The use of ultrasound can make organic fill out
It is fully dispersed in dispersant to fill object.It is preferred that frequency ultrasonic in above-mentioned ultrasonic procedure is 20~40kHz, the time of supersound process
For 5~10min.
The main function for forming the dispersant of above-mentioned mixed liquor is for diluting organic filler, while in order to avoid excessive
Dispersant retain in sample, it is preferred to use dispersant of the volatile solvents as the application, such as acetone, ethyl alcohol, chlorine
Imitative, dichloroethylene, tetrachloro-ethylene, ether and acetaldehyde.
The organic filler that can be used for the application is soluble soluble matter and lyotrope in above-mentioned dispersant, wherein above-mentioned
Soluble matter and lyotrope are identical as the definition of the soluble matter of this field and lyotrope, and details are not described herein, for example use polyethylene
Alcohol formal is soluble in acetone, chloroform, dichloroethylene, tetrachloro-ethylene, using polyvinyl butyral as organic filler
As organic filler, it is soluble in ethyl alcohol.
The application mixed liquor can rely on gravity or osmosis to enter sample to be prepared, in order to accelerate the entrance of mixed liquor
The speed of sample to be prepared, the step S2 of preferably above-mentioned preparation method include being carried out to the sample to be prepared that surface has mixed liquor
Vacuumize process obtains pretreatment TEM sample, accelerates the speed that mixed liquor enters sample to be prepared using the negative pressure to be formed is vacuumized
Degree, and be conducive to the volatilization of dispersant in mixed liquor.
In carrying out above-mentioned vacuum, to be formed by negative pressure excessive in order to avoid vacuumizing, and suspension structure is caused to become
Shape, the negative pressure that vacuumize process is formed in preferably above-mentioned steps S2 are 100~150torr.It is verified by inventor's test of many times
It gives, organic filler can realize suspension structure and matrix into the lower section of suspension structure after persistently vacuumizing 10~20min
Substantive connection.
In another preferred embodiment of the application, a kind of TEM sample is provided, the TEM sample is using above-mentioned
Preparation method be prepared.Prepared TEM sample realizes substantive connection, Neng Goushi between suspension structure and matrix
Now to the accurate detection of sample top layer structure.
Below with reference to embodiment and comparative example, the advantageous effect that further illustrates the present invention.
Embodiment 1
Polyvinyl formal is mixed with acetone, and use frequency for the supersound process 8min of 40kHz after, implemented
The mixed liquor that the polyvinyl formal weight content of example 1 is 15%；Use dropper with the dropwise addition of 0.2ml/ drops the mixed liquor
Then the sample to be prepared is placed in vacuum system on the surface of sample to be prepared and carries out vacuumize process by amount drop, utilize
Vacuum system forms the negative pressure of 120torr, and continues 15min, obtains pretreatment TEM sample；The pretreatment TEM sample is placed in
It is handled in FIB boards, selects the ion beam voltage of 30kv to cut, be observed under the electron beam of 5kv.Obtain embodiment 1
TEM sample.
Embodiment 2
Polyvinyl formal is mixed with acetone, and use frequency for the supersound process 10min of 20kHz after, obtain reality
Apply the mixed liquor that the polyvinyl formal weight content of example 2 is 10%；Use dropper with the drop of 0.5ml/ drops the mixed liquor
Dosage is dripped on the surface of sample to be prepared, and then the sample to be prepared is placed in vacuum system and carries out vacuumize process, profit
The negative pressure of 150torr is formed with vacuum system, and continues 10min, obtains pretreatment TEM sample；The pretreatment TEM sample is set
It is handled in FIB boards, obtains the TEM sample of embodiment 2.
Embodiment 3
Polyvinyl formal is mixed with acetone, and use frequency for the supersound process 8min of 40kHz after, implemented
The mixed liquor that the polyvinyl formal weight content of example 3 is 10%；Use dropper with the dropwise addition of 0.1ml/ drops the mixed liquor
Then the sample to be prepared is placed in vacuum system on the surface of sample to be prepared and carries out vacuumize process by amount drop, utilize
Vacuum system forms the negative pressure of 100torr, and continues 20min, obtains pretreatment TEM sample；The pretreatment TEM sample is placed in
It is handled in FIB boards, obtains the TEM sample of embodiment 3.
Embodiment 4
Polyvinyl butyral is mixed with ethyl alcohol, and use frequency for the supersound process 8min of 40kHz after, implemented
The mixed liquor that 4 polyvinyl formal weight content of example is 15%；Use dropper with the dripping quantity of 0.6ml/ drops the mixed liquor
It drips on the surface of sample to be prepared, then the sample to be prepared is placed in vacuum system and carries out vacuumize process, using true
Empty set unites to form the negative pressure of 120torr, and continues 15min, obtains pretreatment TEM sample；The pretreatment TEM sample is placed in
It is handled in FIB boards, obtains the TEM sample of embodiment 4.
Embodiment 5
Polyvinyl formal is mixed with chloroform, and use frequency for the supersound process 8min of 40Hz after, implemented
The mixed liquor that the polyvinyl formal weight content of example 5 is 20%；Use dropper with the dropwise addition of 0.01ml/ drops the mixed liquor
Then the sample to be prepared is placed in vacuum system on the surface of sample to be prepared and carries out vacuumize process by amount drop, utilize
Vacuum system forms the negative pressure of 120torr, and continues 15min, obtains pretreatment TEM sample；The pretreatment TEM sample is placed in
It is handled in FIB boards, obtains the TEM sample of embodiment 5.
Comparative example 1
Polyvinyl formal is mixed with acetone, and use frequency for the supersound process 15min of 40kHz after, obtain pair
The mixed liquor that the polyvinyl formal weight content of ratio 1 is 30%；Use dropper with the drop of 0.2ml/ drops the mixed liquor
Dosage is dripped on the surface of sample to be prepared, and then the sample to be prepared is placed in vacuum system and carries out vacuumize process, profit
The negative pressure of 200torr is formed with vacuum system, and continues 5min, obtains pretreatment TEM sample；The pretreatment TEM sample is set
It is handled in FIB boards, obtains the TEM sample of comparative example 1.
Comparative example 2
Polyvinyl butyral is mixed with ethyl alcohol, and use frequency for the supersound process 8min of 40kHz after, compared
The mixed liquor that the polyvinyl formal weight content of example 2 is 5%；Use dropper with the dripping quantity of 0.5ml/ drops the mixed liquor
It drips on the surface of sample to be prepared, then the sample to be prepared is placed in vacuum system and carries out vacuumize process, using true
Empty set unites to form the negative pressure of 50torr, and continues 30min, obtains pretreatment TEM sample；The pretreatment TEM sample is placed in FIB
It is handled in board, obtains the TEM sample of comparative example 2.
Comparative example 3
The surface that polyvinyl formal is coated in sample to be prepared same as Example 1 obtains pretreatment TEM samples
Product；The pretreatment TEM sample is placed in FIB boards and is handled, the TEM sample of comparative example 1 is obtained.
TEM is carried out under the same conditions to the TEM sample of embodiment 1 to 5 and comparative example 1 to 3 to detect to obtain accordingly
TEM schemes, and carries out E-beam (electron beam) detections under the same conditions and obtain corresponding E-beam testing result figures, wherein scheming
4 show that the E-beam testing result figures of embodiment 1, Fig. 5 show the E-beam testing result figures of comparative example 3.
Organic matter has been filled into each position below suspension structure in Fig. 4 it can be seen from the comparison of Fig. 4 and Fig. 5, real
The substantive connection for having showed suspension structure and matrix, to restrained effectively the ion beam pair of FIB in TEM sample preparation process
The injury of sample, and the suspension structure in Fig. 5 and matrix stripping, illustrate in TEM sample preparation process, the ion beam pair of FIB
Sample causes injury, and same problem occur in comparative example 1 and comparative example 3.In addition, the test result phase of embodiment 1 to 5
Seemingly, it is significantly better than that the filling effect of the organic matter of comparative example 1 to 3.
It can be seen from the above description that the application the above embodiments realize following technique effect：
Organic matter is dispersed into mixed liquor so that the concentration and surface tension of organic filler reduce, and then are conducive to mix
Diffusion of the liquid into sample to be prepared is closed, then by mixing drop in the surface of sample to be prepared, so as to avoid directly coating
The external force of formation causes the displacement of suspension structure；After obtaining pretreatment TEM sample, due to real between suspension structure and matrix
Substantive connection is showed, therefore, when being handled using FIB boards, can avoid using treatment conditions commonly used in the art
Cause the damage to suspension structure.
The foregoing is merely the preferred embodiments of the application, are not intended to limit this application, for the skill of this field
For art personnel, the application can have various modifications and variations.Within the spirit and principles of this application, any made by repair
Change, equivalent replacement, improvement etc., should be included within the protection domain of the application.
Claims (9)
1. a kind of TEM sample preparation method, which is characterized in that the preparation method includes：
Step S1 has by the mixing drop for being dispersed with organic filler in the surface of sample to be prepared described in the mixed liquor
The weight content of machine filler is 10~20%；
Step S2 makes the mixed liquor enter in the sample to be prepared and obtains pretreatment TEM sample；And
Step S3 handles the pretreatment TEM sample using FIB boards, obtains the TEM sample,
The mixed liquor is selected from acetone, ethyl alcohol, chloroform, dichloro using organic filler, the dispersant described in dispersion dilution agent
Ethylene, tetrachloro-ethylene, ether and acetaldehyde composition group in any one, the organic filler be the dispersant it is solvable
Object and lyotrope.
2. preparation method according to claim 1, which is characterized in that the step S1 includes by the mixing drop in described
The surface of the close suspension structure of sample to be prepared.
3. preparation method according to claim 1, which is characterized in that the step S1 uses dropper with 0.01~0.5ml/ drops
Dripping quantity carry out the dropwise addition of the mixed liquor.
4. preparation method according to claim 1, which is characterized in that the step S1 further includes the preparation of the mixed liquor
Journey, the preparation process include：
The organic filler is mixed with the dispersant, forms pre-composition；
The pre-composition is ultrasonically treated, the mixed liquor is obtained.
5. preparation method according to claim 4, which is characterized in that the frequency of the ultrasound is 20~40kHz, the ultrasound
The time of processing is 5~10min.
6. preparation method according to claim 1, which is characterized in that the step S2 includes having the mixed liquor to surface
The sample to be prepared carry out vacuumize process and obtain the pretreatment TEM sample.
7. preparation method according to claim 6, which is characterized in that the negative pressure of vacuumize process formation is in the step S2
100~150torr.
8. preparation method according to claim 6, which is characterized in that the draw vacuum duration of the step S2 be 10~
20min。
9. a kind of TEM sample, which is characterized in that the TEM sample is using any one of claim 1 to 8 preparation method
It is prepared.
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| CN201510086443.1A CN105987836B (en) | 2015-02-17 | 2015-02-17 | Tem sample and preparation method thereof |
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|---|---|---|---|---|
| US6194720B1 (en) * | 1998-06-24 | 2001-02-27 | Micron Technology, Inc. | Preparation of transmission electron microscope samples |
| CN102530831A (en) * | 2010-12-27 | 2012-07-04 | 上海丽恒光微电子科技有限公司 | Manufacture method for MEMS (Micro-electromechanical Systems) device |
| CN103543044A (en) * | 2012-07-17 | 2014-01-29 | 无锡华润上华半导体有限公司 | Preparation method for section shape analyzing sample of MEMS (micro electro mechanical systems) device |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005326211A (en) * | 2004-05-13 | 2005-11-24 | Bridgestone Corp | Sample preparation method |
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2015
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6194720B1 (en) * | 1998-06-24 | 2001-02-27 | Micron Technology, Inc. | Preparation of transmission electron microscope samples |
| CN102530831A (en) * | 2010-12-27 | 2012-07-04 | 上海丽恒光微电子科技有限公司 | Manufacture method for MEMS (Micro-electromechanical Systems) device |
| CN103543044A (en) * | 2012-07-17 | 2014-01-29 | 无锡华润上华半导体有限公司 | Preparation method for section shape analyzing sample of MEMS (micro electro mechanical systems) device |
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| Title |
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