CN104422604B - A kind of electron microscopic sample preparation method - Google Patents
A kind of electron microscopic sample preparation method Download PDFInfo
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- CN104422604B CN104422604B CN201310365495.3A CN201310365495A CN104422604B CN 104422604 B CN104422604 B CN 104422604B CN 201310365495 A CN201310365495 A CN 201310365495A CN 104422604 B CN104422604 B CN 104422604B
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Abstract
The invention discloses a kind of electron microscopic sample preparation method, including:Offer includes the wafer in region to be sampled, and cutting, which is taken out, on the wafer includes the study in region to be sampled, and the region to be sampled includes geodesic structure to be checked and detecting pad;Protection glue-line is formed on the study surface;In the protection film surface formation positioning hole, the positioning hole is located above the detecting pad, to determine the position for detecting structure and detecting pad;The study is prepared into the suitable electron microscopic sample of thickness using FIB.The present invention can ensure that the structure of the electron microscopic sample comprising low k materials is not deformed upon in preparation process, accurately obtain the real shape characteristic of low k materials in small size processing procedure, meanwhile, success rate prepared by operating efficiency and electron microscopic sample is the method increase, cost is saved.
Description
Technical field
The present invention relates to semiconductor fabrication and material analysis field, more particularly to a kind of electron microscopic sample preparation method.
Background technology
The today continued to develop in electronic technology, with constantly advancing for Moore's Law, semiconductor industry is in order to improve
The performance and speed of integrated circuit, more and more, less and less transistor is integrated in the chips.With this miniaturization
The distance between different layer conductors also reduce therewith in trend, chip.Silica as insulating barrier between wire is due to thickness
The continuous diminution of degree causes selfcapacity to increase.Interference signal is transmitted in the accumulation of this electric charge, reduces the reliability of circuit, and
And the further raising of limit frequency.In order to solve this problem, semiconductor industry will apply advanced low-k materials or low-k
Material(K is less than SiO2=3.9)Instead of traditional silicon dioxide insulator material.The application of such a material, can reduce integrated circuit
Leakage current, the capacity effect between reduction wire, reduction integrated circuit is the problems such as generate heat.Because air has extremely low dielectric
Constant(k=1), so dielectric constant can also greatly be reduced by adding air bubble in the dielectric.
Semiconductor devices using such low-k material manufactures is carrying out TEM(Transmission electron microscope, transmission
electron microscope)Problems can be brought during the preparation of sample.Preparation TEM sample common at present has two kinds of sides
Formula:One kind is that, plus Ion Milling preparation TEM samples, this method requires a great deal of time by Polish grindings
Hand lapping and the shortcoming of positioning in distress, it is impossible to the position of structure needed for accurately confirming, influence operating efficiency;It is another to be
The method that TEM sample is prepared using FIB, there is fast speed, high yield rate, accurate positioning.FIB equipment has E- simultaneously
beam(Electron beam)And I-beam(Ion beam)System, generally first will be to be sampled before I-beam carries out cutting sample
Region carries out deposition protective layer using E-beam, to ensure that the geodesic structure to be checked for sampling region is not destroyed by follow-up ion beam.
And for low-k materials, problem will be produced when E-beam carries out deposition protective layer.Due to electronics penetration capacity very
By force, the position of general 1 μm of sample surfaces can be penetrated, and the irradiation of electron beam can assemble substantial amounts of heat.So, insulating barrier
Low-k materials are very yielding in the case where the electron beam for preparing sample is acted on, and sample band detection structure in preparation process is lost original
Some patterns, impact analysis result.
So that geodesic structure to be checked is common double damask structure as an example, referring to figs. 1A to Figure 1B, there is provided be formed with partly to lead
The substrate 101 of body transistor(Transistor is not shown), dual damascene openings are etched in the dielectric layer 102 of low-k materials
After 103, when before follow-up deposited metal step or only depositing one layer of adhesion layer, in order to determine whether the structure etched meets
It is required that, usually a tem analysis can be carried out in this step in production, as shown in figure 1, now double big before electron microscopic sample is prepared into
The height of Ma Shige openings 103 is THK1;In sample preparation after E-beam deposition protective layers as shown in Figure 1B, double big horses
The gross distortion of opening 103 of scholar's leather structure, is no longer presented vertical shape, and now the height of dual damascene openings 103 is THK2.
Because the dielectric layer of low-k materials there occurs serious deformation, height THK2 now can be far smaller than the structure on chip
Actual height THK1, so that impact analysis result.
The content of the invention
The present invention provides a kind of electron microscopic sample preparation method, to prevent the structure comprising low-k materials from preparing sample
During deform, impact analysis result.
In order to solve the above technical problems, the present invention provides a kind of electron microscopic sample preparation method, including:Offer includes to be sampled
The wafer in region, cutting, which is taken out, on the wafer includes the study in region to be sampled, and the region to be sampled includes to be detected
Structure and detecting pad;Protection glue-line is formed on the study surface;In the protection film surface formation positioning hole, the positioning
Hole position is above the detecting pad, to determine the position for detecting structure and detecting pad;The study is prepared into thickness using FIB
Suitable electron microscopic sample.
Optionally, the method for the formation protection glue-line is:
Protection glue is uniformly smeared on study surface, then study is placed on warm table and heated, to solidify Protection glue shape
Into protection glue-line.
Optionally, the method for uniformly smearing Protection glue on study surface is:
In study surface smear Protection glue, there is provided the second study that another surface smear has Protection glue;
Study and the second study are scribbled to the one side laminating of Protection glue, extrudes and makes study and the second study relative motion,
Until observing that color fringe occurs in study Protection glue surface.
Optionally, the Protection glue is that epoxy resin and curing agent are mixed.
Optionally, the Protection glue is 100% epoxy resin by purity and purity is 100% curing agent using volume ratio as 1:1
~20:1 is formulated.
Optionally, the epoxy resin is bisphenol A-type, bmminated bisphenol-A type, the one or more of phenol aldehyde type;The solidification
Agent is tetrabydrophthalic anhydride.
Optionally, described that study is placed on to the process heated on warm table, temperature is 300 DEG C, the duration is 15~
20min。
Optionally, the opening of the positioning hole is the square that the length of side is 10~20 μm.
As a result of above technical scheme, compared with prior art, the present invention has advantages below:
The electron microscopic sample preparation method that the present invention is provided can ensure that prepared by the structure of the electron microscopic sample comprising low-k materials
During do not deform upon, accurately obtain the real shape characteristic of low-k materials in small size processing procedure, it is thus possible to obtain more
Accurate detection data, meanwhile, success rate prepared by operating efficiency and electron microscopic sample is the method increase, cost is saved.
Brief description of the drawings
Figure 1A and Figure 1B is the signal that geodesic structure to be checked is deformed upon before and after preparing of existing electron microscopic sample preparation method
Figure;
The flow chart for the electron microscopic sample preparation method that Fig. 2 is provided by the embodiment of the present invention;
Each step corresponding construction of the electron microscopic sample preparation method that Fig. 3 A to Fig. 3 E are provided by the embodiment of the present invention shows
It is intended to.
Embodiment
According to background technology, during electron microscopic sample is prepared using FIB, the structure of low-k materials easily occurs
Deformation loses original pattern, impact analysis result.
Fig. 2 is refer to, the flow chart of its electron microscopic sample preparation method provided by the embodiment of the present invention, with reference to the Fig. 2,
This method comprises the following steps:
Step S210 is there is provided the wafer for including region to be sampled, and cutting, which is taken out, on the wafer includes region to be sampled
Study, the region to be sampled include geodesic structure to be checked and detecting pad;
Step S220, forms protection glue-line on the study surface;
Step S230, in the protection film surface formation positioning hole, the positioning hole is located above the detecting pad, with
It is determined that the position of detection structure and detecting pad;
Step S240, the suitable electron microscopic sample of thickness is prepared into using FIB by the study.
The electron microscopic sample preparation method of the present invention is described in more detail below in conjunction with diagrammatic cross-section, wherein table
Show the preferred embodiments of the present invention, it should be appreciated that those skilled in the art can change invention described herein, and still
Realize the advantageous effects of the present invention.
As shown in Figure 3A, and with reference to step S210, first there is provided the wafer 201 including region to be sampled, in the wafer
Cutting, which is taken out, on 201 includes the study 202 in region to be sampled, and the region to be sampled includes geodesic structure to be checked and detecting pad.This
The length of side of taking-up study is elected as in 1cm-3cm, the present embodiment and diagram in embodiment includes dual damascene with geodesic structure to be checked
Exemplified by opening.
As shown in Fig. 3 B to 3C, and step S220 is combined, then, protection glue-line is formed on the surface of study 202.Specifically
, Protection glue 204 is uniformly smeared on study surface, then study 202 is placed on warm table and heated, to solidify Protection glue shape
Into protection glue-line.
The preferably uniform mode for smearing Protection glue 204, first in the surface smear Protection glue 204 of study 202, there is provided another table
Face is coated with the second study 203 of Protection glue;The study 203 of study 202 and second is scribbled to the one side laminating of Protection glue, extruding is simultaneously
Make the relative motion of 202 and second study of study 203, until observing that color fringe occurs in the Protection glue surface of study 202.Using this
Method smear Protection glue the surface of study 202 can both applied Protection glue 204 is sufficiently thin, follow-up sample preparation matter is not influenceed
Protection glue 204, can be fully filled opening and the cavity on study 202 by amount again, protect geodesic structure to be checked in follow-up system
It is not destroyed in standby.
The Protection glue 204 is that epoxy resin and curing agent are mixed, preferably, the epoxy resin be bisphenol A-type,
The one or more of bmminated bisphenol-A type, phenol aldehyde type;The curing agent can be a variety of solidifications including tetrabydrophthalic anhydride
Agent.Preferably, the Protection glue is 100% epoxy resin by purity and purity is 100% curing agent using volume ratio as 1:1~20:1
It is formulated.
Progress be heating and curing temperature can for room temperature to 300 DEG C, the heat time can arrive according to temperature difference for 5min
60min.Preferably, temperature elects 300 DEG C as, the duration is 15~20min, can so obtain the preferable Protection glue of quality
Layer.
As shown in Fig. 3 D to 3E, and step S230 is combined, then in the protection film surface formation positioning hole 213, institute
State positioning hole 213 and be located at the top of detecting pad 211, to determine the position of geodesic structure to be checked and detecting pad 211.The present embodiment
In, geodesic structure to be checked is located at two detecting pad intermediate regions.The determination of the position of positioning hole 213 can be completed by light microscope,
This is due to that protection glue-line main component is organic matter, and FIB boards secondary electron can not be through protection glue-line imaging, thus utilizes
The translucency of glue-line is protected to be positioned.In the present embodiment, the determination of position of positioning hole is by laser marking machine (Laser
Marker) board is positioned, and positioning hole is then formed above detecting pad.Preferably, the positioning hole opening shape is that the length of side is
10~20 μm of square, this size range both can guarantee that is pin-pointed to desired position in follow-up FIB preparations, again
The excessive situation for causing Protection glue to be splashed of opening size is avoided to occur.
As shown in Figure 3 D, and with reference to step S240, the study is prepared into the suitable electron microscopic sample of thickness using FIB.
Specifically, on the protection glue-line in region to be sampled deposits tungsten(W)Protective layer, then treats sampling region using ion beam and carries out
Cutting and thinned, formation electron microscopic sample.Then picking up system can be utilized(Pick Up System)By the Electronic Speculum sample prepared
Product take out from study surface, are placed on the copper mesh used in shooting, and carry out the follow-up TEM to electron microscopic sample and shoot, obtain required figure
Piece, carries out the steps such as data analysis.Thus obtained data are the actual size and pattern of geodesic structure to be checked.
The electron microscopic sample preparation method that the present invention is provided can ensure that prepared by the structure of the electron microscopic sample comprising low-k materials
During do not deform upon, accurately obtain the real shape characteristic of low-k materials in small size processing procedure, it is thus possible to obtain more
Accurate detection data, meanwhile, success rate prepared by operating efficiency and electron microscopic sample is the method increase, cost is saved.
Although the present invention is disclosed as above with preferred embodiment, the present invention is not limited to this.Any art technology
Personnel, without departing from the spirit and scope of the present invention, can make various changes or modifications, therefore protection scope of the present invention should
It is defined when by claim limited range.
Claims (6)
1. a kind of electron microscopic sample preparation method, including:
Offer includes the wafer in region to be sampled, and cutting, which is taken out, on the wafer includes the study in region to be sampled, described to treat
Sampling region includes geodesic structure to be checked and detecting pad;
Protection glue-line is formed on the study surface;
In the protection film surface formation positioning hole, the positioning hole is located above the detecting pad, to determine to detect structure
With the position of detecting pad;
The study is prepared into the suitable electron microscopic sample of thickness using FIB;
Wherein, the method for the formation protection glue-line is:
In study surface smear Protection glue, there is provided the second study that another surface smear has Protection glue;
Study and the second study are scribbled to the one side laminating of Protection glue, extrudes and makes study and the second study relative motion, until
It was observed that there is color fringe in study Protection glue surface;
Study is placed on warm table and heated, to solidify Protection glue formation protection glue-line.
2. electron microscopic sample preparation method as claimed in claim 1, it is characterised in that the Protection glue is epoxy resin and solidification
Agent is mixed.
3. electron microscopic sample preparation method as claimed in claim 2, it is characterised in that the Protection glue is 100% ring by purity
Oxygen tree fat and purity are 100% curing agent using volume ratio as 1:1~20:1 is formulated.
4. electron microscopic sample preparation method as claimed in claim 2, it is characterised in that the epoxy resin is bisphenol A-type, bromination
The one or more of bisphenol A-type, phenol aldehyde type;The curing agent is tetrabydrophthalic anhydride.
5. electron microscopic sample preparation method as claimed in claim 2, it is characterised in that described study is placed on warm table adds
The process of heat, temperature is 300 DEG C, and the duration is 15~20min.
6. electron microscopic sample preparation method as claimed in claim 1, it is characterised in that the opening of the positioning hole is that the length of side is 10
~20 μm of square.
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CN104422604B true CN104422604B (en) | 2017-09-26 |
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CN106556721A (en) * | 2015-09-29 | 2017-04-05 | 中芯国际集成电路制造(上海)有限公司 | Test sample and preparation method thereof |
CN105806679A (en) * | 2016-05-17 | 2016-07-27 | 上海华力微电子有限公司 | Preparation method for TEM sample |
CN113189370A (en) * | 2021-05-28 | 2021-07-30 | 上海华力微电子有限公司 | Preparation method of TEM sample |
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KR100636029B1 (en) * | 2004-09-10 | 2006-10-18 | 삼성전자주식회사 | Method for forming specimen protecting layer and method for manufacturing transmission electron microscope of specimen for analyzing using the same |
JP4048210B2 (en) * | 2005-12-16 | 2008-02-20 | 株式会社日立製作所 | Sample preparation method |
KR100744267B1 (en) * | 2005-12-28 | 2007-07-30 | 동부일렉트로닉스 주식회사 | specimen manufacturing method for Transmission Electron Microscope |
CN102384867B (en) * | 2010-09-02 | 2014-03-12 | 中芯国际集成电路制造(上海)有限公司 | Method for preparing failure analysis sample |
CN102420151B (en) * | 2011-04-29 | 2013-12-04 | 上海华力微电子有限公司 | Detection method used for characterizing damage of low-dielectric material |
CN103000578A (en) * | 2012-11-28 | 2013-03-27 | 上海华力微电子有限公司 | Method for representing critical size after through-hole etching |
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