JPH08271453A - Observation method of superlattice cross-sectional structure of strain superlattice using transmission electron microscope - Google Patents

Observation method of superlattice cross-sectional structure of strain superlattice using transmission electron microscope

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Publication number
JPH08271453A
JPH08271453A JP9617395A JP9617395A JPH08271453A JP H08271453 A JPH08271453 A JP H08271453A JP 9617395 A JP9617395 A JP 9617395A JP 9617395 A JP9617395 A JP 9617395A JP H08271453 A JPH08271453 A JP H08271453A
Authority
JP
Japan
Prior art keywords
superlattice
observation
cross
image
crystal orientation
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.)
Pending
Application number
JP9617395A
Other languages
Japanese (ja)
Inventor
Fumiaki Hironaka
中 文 明 弘
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SAN BUNSEKI CENTER KK
Original Assignee
SAN BUNSEKI CENTER KK
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by SAN BUNSEKI CENTER KK filed Critical SAN BUNSEKI CENTER KK
Priority to JP9617395A priority Critical patent/JPH08271453A/en
Publication of JPH08271453A publication Critical patent/JPH08271453A/en
Pending legal-status Critical Current

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  • Sampling And Sample Adjustment (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

PURPOSE: To evaluate the superlattice cross-sectional structure of a strain superlattice by inclining the observation face of a dice-like observation piece in the [002] direction of Kikuchi image in (100) crystal orientation and observing a bright field image. CONSTITUTION: A sample has strain superlattice structure of Inx Ga1-x As-GaAs system, for example, and formed into a dice-like observation piece. The sample is observed by irradiating the observation piece, on the axis, with an electron beam in the (110) crystal orientation and then aligning the inclination to provide an observation plane accurately in the (100) crystal orientation using an inclination jig, e.g. a special biaxial inclination holder. Furthermore, the observation plane of the observation piece is inclined in the [002] direction of Kikuchi, image in (100) crystal orientation, i.e., the central point [00] of Kikuchi image is inclined in parallel with the superlattice to a specified position for eliminating participation of the isobaric interference wave thus observing a bright-field image. In other words, a clear bright-field image can be obtained by inclining the observation piece by a specified angle.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【発明の技術分野】本発明は、透過型電子顕微鏡装置に
よる歪超格子の超格子断面構造の観察方法に関するもの
である。
TECHNICAL FIELD The present invention relates to a method for observing a superlattice sectional structure of a strained superlattice by a transmission electron microscope apparatus.

【0002】[0002]

【発明の技術的背景】超格子デバイスなどの超格子構造
を有する結晶の超格子断面構造を観察する手段として、
従来から電子像の分解能が優れる透過型電子顕微鏡装置
が用いられている。この透過型電子顕微鏡装置を用いた
超格子の超格子断面構造の観察方法には、サイコロ形観
察片を用い等厚干渉波を捕捉した明視野像を観察するC
AT(Composition Analysis by Thickness Fringe)法
と、イオンエッチングまたは化学エッチング処理により
作製された断面薄膜片を観察片として断面構造を観察す
る方法とがある。このうち観察片として断面薄膜片を用
いる方法は、観察片の作製に長時間を要するため迅速に
超格子断面を観察、評価することができないという問題
がある。一方、CAT法は、観察片の作製が容易であり
迅速に超格子断面構造を評価できるため、広く採用され
ている。
BACKGROUND OF THE INVENTION As means for observing a superlattice cross-sectional structure of a crystal having a superlattice structure such as a superlattice device,
2. Description of the Related Art Transmission electron microscope apparatuses that have excellent electron image resolution have been used. As a method of observing the superlattice cross-section structure of the superlattice using this transmission electron microscope apparatus, a dice-shaped observation piece is used to observe a bright-field image capturing an equal-thickness interference wave.
There are an AT (Composition Analysis by Thickness Fringe) method and a method of observing a cross-section structure using a cross-section thin film piece produced by ion etching or chemical etching as an observation piece. Of these methods, the method of using a thin-film cross-section as an observation piece has a problem that it takes a long time to manufacture the observation piece, and thus the superlattice cross-section cannot be observed and evaluated rapidly. On the other hand, the CAT method is widely adopted because the observation piece is easy to manufacture and the superlattice sectional structure can be evaluated quickly.

【0003】しかしながら透過型電子顕微鏡装置を用い
CAT法により歪超格子の超格子断面を観察しようとす
ると、明視野像が歪み、超格子の断面膜厚が正確に計測
できないという問題がある。このため歪超格子の超格子
断面構造を観察する場合には、観察片の作製に長時間を
要する断面薄膜片を用いる方法を採用せざるを得なかっ
た。
However, when an attempt is made to observe the superlattice cross section of the strained superlattice by the CAT method using a transmission electron microscope apparatus, there is a problem that the bright field image is distorted and the cross-sectional film thickness of the superlattice cannot be measured accurately. For this reason, when observing the superlattice cross-section structure of the strained superlattice, a method of using a cross-section thin film piece that requires a long time for producing the observation piece has to be adopted.

【0004】[0004]

【発明の目的】本発明は、上記のような従来技術に鑑み
てなされたものであって、歪超格子の超格子断面構造
を、透過型電子顕微鏡装置により、正確にかつ迅速に評
価しうる超格子断面構造の観察方法を提供することを目
的としている。
SUMMARY OF THE INVENTION The present invention has been made in view of the above-mentioned prior art, and it is possible to accurately and quickly evaluate the superlattice cross-sectional structure of a strained superlattice with a transmission electron microscope apparatus. It is intended to provide a method for observing a superlattice cross-section structure.

【0005】[0005]

【発明の概要】本発明に係る透過型電子顕微鏡装置によ
る歪超格子の超格子断面構造の観察方法は、サイコロ型
観察片を用い、該観察片の観察面を(100)結晶方位
の菊池像の[002]方向に傾けて明視野像を観察する
ことを特徴としている。
SUMMARY OF THE INVENTION A method for observing a superlattice sectional structure of a strained superlattice by a transmission electron microscope apparatus according to the present invention uses a dice type observation piece, and the observation surface of the observation piece is a Kikuchi image of (100) crystal orientation. It is characterized in that the bright field image is observed by inclining in the [002] direction.

【0006】本発明によると、歪超格子の断面膜厚の測
定などの、超格子断面構造の観察を迅速にかつ正確にす
ることができる。
According to the present invention, the observation of the superlattice cross-section structure, such as the measurement of the cross-section film thickness of the strained superlattice, can be performed quickly and accurately.

【0007】[0007]

【発明の具体的説明】以下、本発明に係る透過型電子顕
微鏡装置による歪超格子の超格子断面構造の観察方法に
ついて具体的に説明する。
DETAILED DESCRIPTION OF THE INVENTION A method of observing a cross-sectional structure of a superlattice of a strained superlattice by a transmission electron microscope apparatus according to the present invention will be specifically described below.

【0008】本発明で用いられる透過型電子顕微鏡装置
は、電子線の加速電圧が200kV以上の透過型電子顕
微鏡装置である。本発明の方法に用いられる試料は、歪
をもった超格子構造を有する試料であり、たとえば、I
x Ga1-x As−GaAs系などの歪をもつ超格子構
造を有する試料が用いられる。このような試料は、CA
T法に用いられるものと同様のサイコロ型観察片に形成
して観察片とする。
The transmission electron microscope apparatus used in the present invention is a transmission electron microscope apparatus having an electron beam acceleration voltage of 200 kV or more. The sample used in the method of the present invention is a sample having a superlattice structure having a strain, for example, I
A sample having a strained superlattice structure such as n x Ga 1-x As-GaAs system is used. Such samples are
An observation piece is formed by forming a dice-type observation piece similar to that used in the T method.

【0009】本発明の歪超格子の超格子断面構造の観察
方法は、まずサイコロ型観察片の(110)結晶方位に
電子線を軸上照射し、次にこの観察片を特殊二軸傾斜ホ
ルダなどの傾斜冶具で、正確に(100)結晶方位の観
察面になるように傾斜のアライメントをとる。さらに、
この観察片の観察面を(100)結晶方位の菊池像の
[002]方向、すなわち超格子に対して平行方向に菊
池像の中心点[000]を、等圧干渉波の関与を除去で
きる特定位置に傾けて明視野像を観察する。
In the method of observing the superlattice cross-section structure of the strained superlattice of the present invention, first, the (110) crystal orientation of the dice type observation piece is irradiated with an electron beam on the axis, and then this observation piece is specially biaxially inclined holder. Using a tilting jig such as the above, the tilting is aligned so that the observation plane has the (100) crystal orientation accurately. further,
The observation point of this observation piece is specified by the center point [000] of the Kikuchi image in the [002] direction of the Kikuchi image in the (100) crystal orientation, that is, in the direction parallel to the superlattice. Tilt to the position and observe the bright field image.

【0010】このように観察片を特定の角度に傾けるこ
とにより等厚干渉波の関与を除いた鮮明な明視野像を得
ることができる。
By thus tilting the observation piece at a specific angle, it is possible to obtain a clear bright-field image without the contribution of the equal-thickness interference wave.

【0011】[0011]

【発明の効果】本発明は、歪超格子の超格子断面構造
を、透過型電子顕微鏡装置により、正確にかつ迅速に評
価することができる。
According to the present invention, the superlattice cross-section structure of the strained superlattice can be accurately and quickly evaluated by the transmission electron microscope apparatus.

【0012】[0012]

【実施例】以下、実施例に基づいて本発明をさらに具体
的に説明するが、本発明はこれら実施例に限定されるも
のではない。
The present invention will be described in more detail based on the following examples, but the invention is not intended to be limited to these examples.

【0013】[0013]

【実施例1】MOCVD法によりGaAs基板上に成長
形成させたIn0.15Ga0.85As層とGaAs層との多
層構造を有する歪超格子試料からサイコロ型観察片を作
製した。この観察片を用い、透過電子顕微鏡装置(日本
電子(株)製、JEM2000FX)により以下のよう
にして超格子断面構造の観察をした。
Example 1 A dice-type observation piece was prepared from a strained superlattice sample having a multilayer structure of an In 0.15 Ga 0.85 As layer and a GaAs layer grown and formed on a GaAs substrate by the MOCVD method. Using this observation piece, the superlattice cross-section structure was observed with a transmission electron microscope apparatus (JEM2000FX, manufactured by JEOL Ltd.) as follows.

【0014】まず、サイコロ型観察片の(110)結晶
方位に電子線を軸上照射し、次に観察片を傾斜冶具(試
料ホルダ)で、正確に(100)結晶方位の観察面にな
るように傾斜のアライメントをとった。さらに、観察片
を(100)結晶方位の菊池像の[002]方向に傾け
て明視野像により超格子断面構造を観察した。得られた
超格子断面像の電子顕微鏡写真を図1に示す。
First, the (110) crystal orientation of the dice type observation piece is irradiated with an electron beam on the axis, and then the observation piece is accurately tilted to the observation plane of the (100) crystal orientation by a tilting jig (sample holder). Aligned to the slope. Furthermore, the observation piece was tilted in the [002] direction of the Kikuchi image in the (100) crystal orientation, and the superlattice cross-sectional structure was observed by a bright-field image. An electron micrograph of the obtained superlattice cross-sectional image is shown in FIG.

【0015】観察条件を以下に示す。 加速条件:200kV 試料ホルダ:特殊2軸傾斜ホルダ 集束レンズ絞り径:50μmφ 対物レンズ絞り径:20μmφThe observation conditions are shown below. Acceleration condition: 200 kV Sample holder: Special biaxial tilt holder Focusing lens diaphragm diameter: 50 μmφ Objective lens diaphragm diameter: 20 μmφ

【0016】[0016]

【比較例1】実施例1において、観察片を(100)結
晶方位の菊池像の[020]方向に傾けて超格子断面を
観察した以外は、実施例1と同様にして超格子断面を観
察した。得られた超格子断面像の電子顕微鏡写真を図2
に示す。
Comparative Example 1 A superlattice cross section was observed in the same manner as in Example 1 except that the observation piece was tilted in the [020] direction of the Kikuchi image of the (100) crystal orientation and the superlattice cross section was observed. did. An electron micrograph of the obtained superlattice cross-sectional image is shown in FIG.
Shown in

【0017】[0017]

【比較例2】実施例1において、観察片を(100)結
晶方位の菊池像の[022]方向に傾けて超格子断面を
観察した以外は、実施例1と同様にして超格子断面を観
察した。得られた超格子断面像の電子顕微鏡写真を図3
に示す。
Comparative Example 2 A superlattice cross section was observed in the same manner as in Example 1 except that the observation piece was tilted in the [022] direction of the Kikuchi image of the (100) crystal orientation in Example 1 and the superlattice cross section was observed. did. Fig. 3 shows an electron micrograph of the obtained superlattice cross-sectional image.
Shown in

【0018】[0018]

【比較例3】実施例1において用いたものと同様の観察
片を用い、CAT法により超格子断面を観察した。得ら
れた超格子断面像の電子顕微鏡写真を図4に示す。
COMPARATIVE EXAMPLE 3 The same observation piece as that used in Example 1 was used to observe the cross section of the superlattice by the CAT method. An electron micrograph of the obtained superlattice cross-sectional image is shown in FIG.

【0019】[0019]

【参考例1】実施例1と同様のIn0.15Ga0.85As層
とGaAs層との多層構造を有する歪超格子試料からイ
オンエッチング処理によって断面薄膜片を作製し、実施
例1で用いたものと同様の透過型電子顕微鏡装置で観察
した。得られた超格子断面像の電子顕微鏡写真を図5に
示す。
Reference Example 1 A cross-section thin film piece was produced by ion etching from a strained superlattice sample having a multilayer structure of In 0.15 Ga 0.85 As layer and GaAs layer similar to that of Example 1, and was used in Example 1. It was observed with the same transmission electron microscope apparatus. The electron micrograph of the obtained superlattice cross-sectional image is shown in FIG.

【0020】実施例1および参考例1から、本発明の方
法によると断面薄膜片を観察する方法と同様に超格子の
断面膜厚が正確に計測できることがわかる。
It can be seen from Example 1 and Reference Example 1 that the cross-sectional film thickness of the superlattice can be accurately measured by the method of the present invention as in the method of observing the cross-sectional thin film piece.

【図面の簡単な説明】[Brief description of drawings]

【図1】 本発明の方法により観察した歪超格子の超格
子断面を示す図(電子顕微鏡写真)である。
FIG. 1 is a diagram (electron micrograph) showing a superlattice cross section of a strained superlattice observed by a method of the present invention.

【図2】 観察片の(100)結晶方位の菊池像の[0
20]方向の明視野像を示す図(電子顕微鏡写真)であ
る。
[Fig. 2] Fig. 2 shows a [100] crystallographic orientation of the observed piece of [0
FIG. 20 is a diagram (electron micrograph) showing a bright-field image in the [20] direction.

【図3】 観察片の(100)結晶方位の菊池像の[0
22]方向の明視野像を示す図(電子顕微鏡写真)であ
る。
FIG. 3 shows a [100] crystal orientation of the observed piece [0
FIG. 22 is a diagram (electron micrograph) showing a bright-field image in the [22] direction.

【図4】 従来の方法によりCAT法で観察した歪超格
子の超格子断面を示す図(電子顕微鏡写真)である。
FIG. 4 is a diagram (electron micrograph) showing a superlattice cross section of a strained superlattice observed by a CAT method by a conventional method.

【図5】 イオンエッチング法により作製した薄膜化観
察片を用いて観察した歪超格子の超格子断面を示す図
(電子顕微鏡写真)である。
FIG. 5 is a diagram (electron micrograph) showing a superlattice cross section of a strained superlattice observed using a thin film observation piece produced by an ion etching method.

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】 透過型電子顕微鏡装置による歪超格子の
超格子断面構造の観察方法において、 サイコロ型観察片を用い、該観察片の観察面を(10
0)結晶方位の菊池像の[002]方向に傾けて明視野
像を観察することを特徴とする透過型電子顕微鏡装置に
よる歪超格子の超格子断面構造の観察方法。
1. A method of observing a superlattice sectional structure of a strained superlattice by a transmission electron microscope apparatus, wherein a dice type observation piece is used, and an observation surface of the observation piece is (10)
0) A method for observing a superlattice cross-sectional structure of a strained superlattice by a transmission electron microscope apparatus, which comprises observing a bright field image by inclining in a [002] direction of a Kikuchi image in a crystal orientation.
JP9617395A 1995-03-29 1995-03-29 Observation method of superlattice cross-sectional structure of strain superlattice using transmission electron microscope Pending JPH08271453A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP9617395A JPH08271453A (en) 1995-03-29 1995-03-29 Observation method of superlattice cross-sectional structure of strain superlattice using transmission electron microscope

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP9617395A JPH08271453A (en) 1995-03-29 1995-03-29 Observation method of superlattice cross-sectional structure of strain superlattice using transmission electron microscope

Publications (1)

Publication Number Publication Date
JPH08271453A true JPH08271453A (en) 1996-10-18

Family

ID=14157941

Family Applications (1)

Application Number Title Priority Date Filing Date
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Country Status (1)

Country Link
JP (1) JPH08271453A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004093263A (en) * 2002-08-30 2004-03-25 Fujitsu Ltd Method of evaluating lattice strain in crystal material

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004093263A (en) * 2002-08-30 2004-03-25 Fujitsu Ltd Method of evaluating lattice strain in crystal material

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