JPH09119907A - Method and device for measuring three-dimensional distribution of element concentration - Google Patents
Method and device for measuring three-dimensional distribution of element concentrationInfo
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- JPH09119907A JPH09119907A JP7275951A JP27595195A JPH09119907A JP H09119907 A JPH09119907 A JP H09119907A JP 7275951 A JP7275951 A JP 7275951A JP 27595195 A JP27595195 A JP 27595195A JP H09119907 A JPH09119907 A JP H09119907A
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- sample
- concentration distribution
- film thickness
- thickness direction
- electron beam
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、高い空間分解能を
有する元素濃度分布測定方法及び装置に関し、特に、分
析電子顕微鏡を用いて三次元（膜厚）方向の元素濃度分
布を測定する方法及び装置に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and apparatus for measuring element concentration distribution having high spatial resolution, and more particularly, a method and apparatus for measuring element concentration distribution in a three-dimensional (film thickness) direction using an analytical electron microscope. It is about.
【０００２】[0002]
【従来の技術】半導体素子中の元素濃度分布は素子の基
本特性を決め、また、半導体素子中に重金属などがある
と欠陥生成の原因となる。従って、半導体素子の歩留ま
り向上とも関連して、半導体素子中の元素濃度分布を精
密に測定することが求められている。2. Description of the Related Art The element concentration distribution in a semiconductor device determines the basic characteristics of the device, and the presence of heavy metals in the semiconductor device causes defects. Therefore, it is required to measure the element concentration distribution in the semiconductor element precisely in connection with the improvement of the yield of the semiconductor element.
【０００３】従来、膜の厚さ方向の元素濃度分布を測定
する手法として二次イオン質量分析法（Secondary Ion
Mass Spectroscopy、略してＳＩＭＳ）があるが、ＳＩ
ＭＳで用いられるプローブ径は約１μｍであり、０.５
μｍ以下の加工寸法で製造される半導体素子中の元素濃
度分布測定には適用できない。そこで、半導体素子中の
元素分析には、高い空間分解能を有する分析電子顕微鏡
−特性Ｘ線分析法（Energy Dipersive X-ray Spectrosc
opy、略してＥＤＸ）が用いられている。また、主とし
て軽元素の分析を行うには、分析電子顕微鏡−電子エネ
ルギ損失分光（Electron Energy Loss Spectroscopy、
略してＥＥＬＳ）法も用いられている。Conventionally, as a method for measuring the element concentration distribution in the thickness direction of the film, the secondary ion mass spectrometry (Secondary Ion) method is used.
Mass Spectroscopy, abbreviated SIMS), but SI
The probe diameter used in MS is about 1 μm and is 0.5
It cannot be applied to the measurement of element concentration distribution in a semiconductor device manufactured with a processing dimension of μm or less. Therefore, for elemental analysis in semiconductor devices, an energy dipersive X-ray spectroscopy method having a high spatial resolution is used.
opy, or EDX for short) is used. In addition, in order to analyze light elements mainly, analytical electron microscope-electron energy loss spectroscopy (Electron Energy Loss Spectroscopy,
The EELS method for short is also used.
【０００４】[0004]
【発明が解決しようとする課題】分析電子顕微鏡−ＥＤ
Ｘ法により半導体素子中の元素濃度分布を求める場合、
理論的には、平面薄膜試料を作成することによりｘ−ｙ
方向の分布が測定でき、断面薄膜試料を作成することに
よりｘ−ｚ、あるいはｙ−ｚ方向の分布が測定できる。Analytical Electron Microscope-ED
When obtaining the element concentration distribution in the semiconductor element by the X method,
Theoretically, by making a planar thin film sample, xy
The distribution in the direction can be measured, and the distribution in the xz or yz direction can be measured by preparing a cross-sectional thin film sample.
【０００５】分析電子顕微鏡のプローブ径は普通、１ｎ
ｍから１０ｎｍである。一方、薄膜試料の膜厚は、０.
１μｍから０.２μｍであるため、測定領域は、長さ／
直径の比が１００以上のきわめて細長い円柱状であり、
基本的にこの長さ（膜厚）方向で元素濃度は一定である
と仮定している。しかし、実際の試料では、この長さ
（膜厚）方向に濃度分布があり、これが精密な元素濃度
分布測定の障害となっている。このことは、分析電子顕
微鏡−ＥＥＬＳ法においても全く同じである。膜厚方向
の元素濃度分布を計測する手段として、試料を傾斜させ
て分析を行い、最終的に膜厚方向の元素濃度分布を算出
する手法も提案されている。しかし、この方法は、ｘ−
ｙ平面上での位置精度が悪くなるだけでなく、試料傾斜
に伴ってｘ−ｙ平面上での測定位置が広がるとともに変
化し、結局、プローブ径に比べてｘ−ｙ平面上では広範
囲の領域で均一な濃度分布が要求されることになり、精
密な元素濃度分布測定から逸脱してしまう。The probe diameter of an analytical electron microscope is usually 1n.
m to 10 nm. On the other hand, the film thickness of the thin film sample is 0.
Since it is 1 μm to 0.2 μm, the measurement area is
It is a very elongated cylinder with a diameter ratio of 100 or more,
Basically, it is assumed that the element concentration is constant in this length (film thickness) direction. However, in an actual sample, there is a concentration distribution in this length (film thickness) direction, which is an obstacle to accurate element concentration distribution measurement. This is exactly the same in the analytical electron microscope-EELS method. As a means for measuring the element concentration distribution in the film thickness direction, a method of tilting a sample for analysis and finally calculating the element concentration distribution in the film thickness direction has also been proposed. However, this method
Not only the position accuracy on the y-plane deteriorates, but also the measurement position on the xy-plane expands and changes as the sample tilts, and as a result, a wider area on the xy-plane than the probe diameter. Therefore, a uniform concentration distribution is required, which deviates from precise element concentration distribution measurement.
【０００６】本発明は、分析電子顕微鏡による計測にお
いて、試料の平面方向で高い空間分解能を維持しなが
ら、膜厚方向の元素濃度分布を精密に評価することので
きる方法及び装置を提供することを目的とする。The present invention provides a method and apparatus capable of precisely evaluating the element concentration distribution in the film thickness direction while maintaining a high spatial resolution in the plane direction of a sample in the measurement by an analytical electron microscope. To aim.
【０００７】[0007]
【課題を解決するための手段】本発明では、分析電子顕
微鏡におけるＥＤＸとＥＥＬＳの信号を演算することで
膜厚方向の元素濃度分布を求める。ＥＥＬＳの信号の代
わりに、複数のＥＤＸ信号を用いることも可能である。
単一のＥＤＸ検出器を用いた場合でも、ＥＤＸの検出角
を走査して計測したり、形状が非対称である試料を電子
線照射軸の回りに回転することで、試料による遮蔽状態
を変えて複数回計測することで膜厚方向の元素濃度分布
測定が可能となる。In the present invention, the element concentration distribution in the film thickness direction is obtained by calculating the signals of EDX and EELS in an analytical electron microscope. It is also possible to use a plurality of EDX signals instead of the EELS signals.
Even when a single EDX detector is used, the detection angle of the EDX can be scanned and measured, or the sample with an asymmetrical shape can be rotated around the electron beam irradiation axis to change the shielding state of the sample. By measuring a plurality of times, it is possible to measure the element concentration distribution in the film thickness direction.
【０００８】ＥＥＬＳ検出器と単一のＥＤＸ検出器を用
いた場合には、電子エネルギー損失スペクトル強度から
試料の膜厚方向の平均元素濃度を求めることができ、特
性Ｘ線信号と電子エネルギー損失スペクトル信号との差
から試料膜厚方向の元素濃度分布の濃度勾配を求めるこ
とができる。複数のＥＤＸ検出器を用いたり、単一のＥ
ＤＸ検出器でもその検出角度を走査して多くの計測値を
得ると、それらの計測値を演算することにより、試料膜
厚方向の元素濃度分布を２次以上の多項式で近似するこ
とができる。When the EELS detector and the single EDX detector are used, the average element concentration in the film thickness direction of the sample can be obtained from the electron energy loss spectrum intensity, and the characteristic X-ray signal and the electron energy loss spectrum can be obtained. The concentration gradient of the element concentration distribution in the sample film thickness direction can be obtained from the difference from the signal. Use multiple EDX detectors or use a single E
Even if the DX detector scans the detected angle to obtain many measured values, the element concentration distribution in the sample film thickness direction can be approximated by a polynomial of quadratic or higher order by calculating these measured values.
【０００９】また、本発明による三次元元素濃度分布測
定装置は、電子線発生手段と、電子線発生手段により発
生した電子線を試料に照射する手段と、試料から発生し
た特性Ｘ線を検出する第１の検出器と、試料を透過した
電子線の電子エネルギー損失スペクトルを検出する第２
の検出器と、第１の検出器及び第２の検出器の出力を演
算して試料の膜厚方向の元素分布を求める演算手段とを
含むことを特徴とする。Further, the three-dimensional element concentration distribution measuring device according to the present invention detects the characteristic X-rays generated from the sample, the electron beam generating means, the means for irradiating the sample with the electron beam generated by the electron beam generating means. A first detector and a second detector for detecting an electron energy loss spectrum of an electron beam transmitted through a sample
And a calculating means for calculating outputs of the first detector and the second detector to obtain an element distribution in the film thickness direction of the sample.
【００１０】以下、図面を参照して、より詳細に説明す
る。図１は、計測領域からの信号をＥＤＸとＥＥＬＳで
取り込む分析電子顕微鏡の模式図である。電子銃６から
放出された電子線４は収束レンズ７によって試料１上に
収束される。このとき電子線照射によって試料１から発
せられた特性Ｘ線５はＥＤＸ検出器２によって検出され
る。一方、試料１を透過した電子線は、対物レンズ８及
び投射レンズ９によって像１０として結像され、スリッ
ト１１の後方に配置されたＥＥＬＳ検出器３は試料計測
領域を透過した電子線をエネルギー分析して電子のエネ
ルギー損失スペクトルを求める。ＥＤＸ検出器２の出力
信号とＥＥＬＳ検出器３の出力信号は、演算装置１２に
入力されて演算される。Hereinafter, a more detailed description will be given with reference to the drawings. FIG. 1 is a schematic diagram of an analytical electron microscope that captures signals from a measurement region by EDX and EELS. The electron beam 4 emitted from the electron gun 6 is converged on the sample 1 by the converging lens 7. At this time, the characteristic X-rays 5 emitted from the sample 1 by the electron beam irradiation are detected by the EDX detector 2. On the other hand, the electron beam transmitted through the sample 1 is imaged as an image 10 by the objective lens 8 and the projection lens 9, and the EELS detector 3 arranged behind the slit 11 analyzes the energy of the electron beam transmitted through the sample measurement region. Then, the energy loss spectrum of the electron is obtained. The output signal of the EDX detector 2 and the output signal of the EELS detector 3 are input to the arithmetic unit 12 and arithmetically operated.
【００１１】ＥＥＬＳに関しては、試料１を透過する電
子線は、試料中の各元素で固有のエネルギー損失を生じ
てＥＥＬＳ検出器３に入り、電子のエネルギー損失量と
その強度から元素の種類と濃度が算出できる。この場
合、透過電子線はほぼ全量が検出器に入るため、試料の
膜厚方向の元素濃度分布には無関係に、各元素は平均濃
度が検出される。一方、ＥＤＸ測定では、試料１を透過
する電子線は、試料中の各元素に固有の特性Ｘ線を放出
させ、このＸ線のエネルギーと強度を検出して、元素の
種類と濃度を算出する。このとき、特性Ｘ線５は試料１
から等方的に放出されるが、ＥＤＸ検出器２に取り込ま
れるのはその一部である。そして、試料の膜厚方向に元
素濃度分布があると、試料自身の遮蔽効果により信号強
度に変化が生じる。Regarding EELS, an electron beam passing through the sample 1 causes an energy loss specific to each element in the sample and enters the EELS detector 3, and the type and concentration of the element are determined based on the energy loss amount of the electron and its intensity. Can be calculated. In this case, almost all of the transmitted electron beam enters the detector, so that the average concentration of each element is detected regardless of the element concentration distribution in the film thickness direction of the sample. On the other hand, in the EDX measurement, the electron beam passing through the sample 1 emits a characteristic X-ray unique to each element in the sample, the energy and intensity of this X-ray are detected, and the type and concentration of the element are calculated. . At this time, the characteristic X-ray 5 is the sample 1
It is isotropically emitted from the EDX detector, but only a part thereof is taken into the EDX detector 2. When the element concentration distribution exists in the film thickness direction of the sample, the signal intensity changes due to the shielding effect of the sample itself.
【００１２】すなわち、図２に示すように、ある元素が
膜試料１の上部領域に存在すると、放出されたＸ線５ａ
はＥＤＸ検出器２の立体角にほぼ等しい割合で取り込ま
れる。しかし、その元素が膜の下部領域にあると、放出
されたＸ線５ｂは膜試料１自体で吸収されるため、ＥＤ
Ｘ検出器２の立体角に比べて低い割合でしか取り込まれ
ない。That is, as shown in FIG. 2, when a certain element exists in the upper region of the film sample 1, the emitted X-ray 5a is emitted.
Are taken in at a rate substantially equal to the solid angle of the EDX detector 2. However, when the element is in the lower region of the film, the emitted X-rays 5b are absorbed by the film sample 1 itself, so that the ED
It is taken in only at a low rate compared to the solid angle of the X detector 2.
【００１３】このことから、平均の元素濃度を与えるＥ
ＥＬＳ信号と、膜厚方向の元素濃度分布に依存するＥＤ
Ｘ信号を組合せて演算装置１２で演算することにより、
試料の膜厚方向の元素濃度分布を算出することが可能と
なる。なお、従来、分析電子顕微鏡に備付けられたＥＤ
ＸとＥＥＬＳとを用いて、分析結果の確認をした例はあ
る（日本電子顕微鏡学会第５１回学術講演会予稿集、
ｐ．３３，１９９５年５月）。しかし、両者の信号の差
を演算することにより、新たな情報を得ようとした試み
はこれまでにない。From this fact, E which gives the average elemental concentration is obtained.
ED that depends on ELS signal and element concentration distribution in the film thickness direction
By combining the X signals and calculating by the calculation device 12,
It is possible to calculate the element concentration distribution in the film thickness direction of the sample. In addition, the ED conventionally provided in the analytical electron microscope.
There is an example in which the analysis result was confirmed using X and EELS (Proceedings of the 51st Scientific Lecture Meeting of the Electron Microscope Society of Japan,
p. 33, May 1995). However, there has been no attempt to obtain new information by calculating the difference between the two signals.
【００１４】図３（ａ），（ｂ）は、Ｓｉ中のＷ元素濃
度分布が膜厚方向で異なる場合のＥＤＸ検出効率の差を
示す。図中、実線はＳｉ中の実際のＷ元素濃度を表し、
破線は実線で示されるような元素濃度勾配がある試料か
ら発せられるＸ線をＥＤＸ検出器で検出するとき、膜厚
方向各位置のＷ元素から発せられたＸ線がＥＤＸ検出器
の総カウント数に対して寄与する寄与度を表す。図の横
軸は、図２の配置で膜試料１の底面から測った膜厚方向
の距離ｚ（μｍ）を表し、縦軸の左の目盛りはＷ元素の
濃度を、右の目盛りはＥＤＸ検出器のカウント数に対す
る寄与度を任意尺度で表す。FIGS. 3A and 3B show the difference in EDX detection efficiency when the W element concentration distribution in Si differs in the film thickness direction. In the figure, the solid line represents the actual W element concentration in Si,
The broken line indicates the total number of counts of the EDX detector when the X-rays emitted from the W element at each position in the film thickness direction are detected when the X-rays emitted from the sample having the element concentration gradient as shown by the solid line are detected by the EDX detector. Represents the degree of contribution to. The horizontal axis of the figure represents the distance z (μm) in the film thickness direction measured from the bottom surface of the film sample 1 in the arrangement of FIG. 2, the left scale on the vertical axis is the concentration of W element, and the right scale is the EDX detection. The contribution to the number of vessels is represented by an arbitrary scale.
【００１５】図３（ａ）はＷ元素が試料の膜厚方向に直
線的な濃度勾配をもって上部領域に多く存在する場合を
表し、図３（ｂ）はＷ元素が試料の膜厚方向に直線的な
濃度勾配をもって逆に下部領域に多く存在する場合を表
す。なお、ＥＤＸ検出器の総カウント数は、図中の破線
の下側領域を積分したものに相当する。Ｗ元素が膜の上
部領域に多く存在する図３（ａ）の場合に比べ、図３
（ｂ）のようにＷ元素が膜の下部領域に多く存在するほ
ど、Ｗ元素から放出される８.４ｅＶのＸ線が膜を構成
しているＳｉ元素によって吸収、散乱される割合が増加
し、検出効率は低下する。従って、ＥＥＬＳとＥＤＸ各
々１台からの信号を用いると、膜厚方向に直線（一次
式）で近似した元素濃度分布が得られることになる。す
なわち、ＥＤＸ信号から算出した見かけ上の元素濃度
と、ＥＥＬＳ信号による元素濃度が等しい場合、この元
素濃度は膜厚方向で一様である。しかし、ＥＤＸ信号に
よる見かけ上の元素濃度がＥＥＬＳ信号による元素濃度
よりも小（大）のとき、この元素濃度は膜厚方向に下部
から上部に向かって減少（増加）している。言いかえれ
ば、ＥＥＬＳの信号は濃度直線の切片（厚さ方向中央部
での濃度）を与え、ＥＥＬＳとＥＤＸの信号強度の差は
濃度直線の傾きを与える。FIG. 3A shows a case where a large amount of W element is present in the upper region with a linear concentration gradient in the film thickness direction of the sample, and FIG. 3B shows that W element is linear in the film thickness direction of the sample. On the contrary, a large concentration gradient is present in the lower region. The total count number of the EDX detector corresponds to the integral of the lower area of the broken line in the figure. As compared with the case of FIG. 3A in which a large amount of W element is present in the upper region of the film, FIG.
As shown in (b), the more W element is present in the lower region of the film, the more the 8.4 eV X-rays emitted from the W element are absorbed and scattered by the Si element constituting the film. , The detection efficiency decreases. Therefore, if signals from one EELS and one EDX are used, an element concentration distribution approximated by a straight line (linear equation) in the film thickness direction can be obtained. That is, when the apparent element concentration calculated from the EDX signal is equal to the element concentration obtained from the EELS signal, the element concentration is uniform in the film thickness direction. However, when the apparent element concentration by the EDX signal is smaller (larger) than the element concentration by the EELS signal, this element concentration decreases (increases) from the lower portion to the upper portion in the film thickness direction. In other words, the EELS signal gives the intercept of the concentration straight line (the concentration at the central portion in the thickness direction), and the difference between the signal intensities of EELS and EDX gives the slope of the concentration straight line.
【００１６】さらに、ＥＤＸ検出器を試料面に対して異
なった角度で２台設置すると、２つの膜厚方向情報が得
られるため、膜厚方向の元素濃度分布を二次曲線で近似
することが可能になる。同様に、図４に示すように、Ｅ
ＤＸ検出器を試料面に対する角度で走査して多数の信号
を取り込むと、図５に示すように、膜厚方向に多次曲線
で近似した元素濃度分布曲線が得られる。Furthermore, if two EDX detectors are installed at different angles with respect to the sample surface, two pieces of information in the film thickness direction can be obtained, so that the element concentration distribution in the film thickness direction can be approximated by a quadratic curve. It will be possible. Similarly, as shown in FIG.
When a DX detector is scanned at an angle with respect to the sample surface and a large number of signals are taken in, an element concentration distribution curve approximated by a multi-order curve in the film thickness direction is obtained, as shown in FIG.
【００１７】検出器の数を増やすかわりに、試料形状を
工夫する方法もある。すなわち、収束イオンビーム（Fo
cused Ion Beam、略してＦＩＢ）を用いて、図６に示す
ように膜厚がステップ状に変化している形状に試料を加
工すれば（あるいは、膜厚方向にステップ状に加工され
た試料部位を利用してもよい）、固定した取り込み角を
持つ単一のＥＤＸ検出器とＥＥＬＳを使用しても、試料
をｘ−ｙ面上で例えば１８０°回転して２回信号を取り
込むことにより、膜厚方向に二次曲線で近似した元素濃
度分布を得ることが可能である。There is also a method of devising the sample shape instead of increasing the number of detectors. That is, the focused ion beam (Fo
If the sample is processed into a shape in which the film thickness changes stepwise as shown in FIG. 6 using cused ion beam (FIB for short) (or the sample portion processed stepwise in the film thickness direction) , And using a single EDX detector with a fixed acquisition angle and EELS, by rotating the sample, for example 180 ° in the xy plane, to acquire the signal twice, It is possible to obtain an element concentration distribution that is approximated by a quadratic curve in the film thickness direction.
【００１８】本発明の原理を一般化して説明する。膜厚
がｔである試料の膜厚方向（ｚ方向）の元素濃度分布を
ｆ(ｚ)、試料面に対して角度θで設置されたＥＤＸ検出
器による検出信号をＣEDX(θ)、試料中の膜厚方向位置
ｚから放出されたＸ線がＸ線発生点とＥＤＸ検出器の間
に介在する試料で吸収、散乱を受けることを考慮した検
出効率をｇ(θ,ｚ)とすると、以下の関係が成立する。The principle of the present invention will be generalized and explained. The element concentration distribution in the film thickness direction (z direction) of the sample having the film thickness t is f (z), the detection signal by the EDX detector installed at an angle θ with respect to the sample surface is C EDX (θ), the sample Letting g (θ, z) be the detection efficiency considering that the X-ray emitted from the position z in the film thickness direction is absorbed and scattered by the sample interposed between the X-ray generation point and the EDX detector, The following relationship holds.
【００１９】ＣEDX(θ)＝∫ｆ(ｚ)ｇ(θ,ｚ)ｄｚ ここでｇ(θ,ｚ)は、試料による既知のＸ線減衰係数、
試料の形状、試料とＥＤＸ検出器の位置関係から求める
ことができ、典型的には図９のようになる。図９は膜厚
方向の距離ｚを横軸とし、膜厚が０.１μｍのとき試料
表面から発せられたＸ線を検出するときの検出効率を１
としたＥＤＸ検出器の検出効率を縦軸として、検出角度
が３０°の時の検出効率曲線ｇ(３０°,ｚ)と検出角度
が６０°の時の検出効率曲線ｇ(６０°,ｚ)を示したも
のである。C EDX (θ) = ∫f (z) g (θ, z) dz where g (θ, z) is the known X-ray attenuation coefficient of the sample,
It can be determined from the shape of the sample and the positional relationship between the sample and the EDX detector, and is typically as shown in FIG. In FIG. 9, the distance z in the film thickness direction is taken as the horizontal axis, and the detection efficiency when detecting X-rays emitted from the sample surface when the film thickness is 0.1 μm is 1
The detection efficiency curve g (30 °, z) when the detection angle is 30 ° and the detection efficiency curve g (60 °, z) when the detection angle is 60 ° are shown with the detection efficiency of the EDX detector as the vertical axis. Is shown.
【００２０】いま、元素濃度分布ｆ(ｚ)を次のｎ次の多
項式で近似する。 ｆ(ｚ)＝ａ0＋ａ1ｚ＋ａ2ｚ2＋…＋ａnｚn ＥＥＬＳ信号ＣEELSはｆ(ｚ)の平均値を表し、Ａを比例
係数として次式が成立する。 ＣEELS＝Ａ∫ｆ(ｚ)ｄｚ／ｔ 試料面に対して角度θ1，θ2，…，θnで設置したＥＤ
Ｘ検出器の検出信号ＣE DX(θ1)，ＣEDX(θ2)，…，Ｃ
EDX(θn)を検出すると、（ｎ＋１）個の未知数ａ0，
ａ1，ａ2，…，ａnに対してＥＥＬＳ信号ＣEELSと合わ
せて（ｎ＋１）個の関係式が得られるため、連立方程式
を解いて係数ａ0，ａ1，ａ2，…，ａnの値を決定するこ
と、すなわち膜厚方向の元素濃度分布ｆ(ｚ)を求めるこ
とができる。Now, the element concentration distribution f (z) is approximated by the following n-th order polynomial. f (z) = a 0 + a 1 z + a 2 z 2 + ... + a n z n The EELS signal C EELS represents the average value of f (z), and the following equation is established with A as a proportional coefficient. C EELS = A∫f (z) dz / t ED installed at angles θ 1 , θ 2 , ..., θ n with respect to the sample surface
Detection signals of the X detector C E DX (θ 1 ), C EDX (θ 2 ), ..., C
When EDX (θ n ) is detected, (n + 1) unknowns a 0 ,
a 1, a 2, ..., in conjunction with EELS signals C EELS against a n (n + 1) for the number of relational expressions can be obtained, the coefficient by solving the simultaneous equations a 0, a 1, a 2 , ..., a It is possible to determine the value of n , that is, to obtain the element concentration distribution f (z) in the film thickness direction.
【００２１】ＥＥＬＳ検出器を用いない場合であって
も、ＥＤＸ検出器の検出角度を変えた検出信号をもう一
つ増やすことにより、同様にして（ｎ＋１）個の連立方
程式を解いて係数ａ0，ａ1，ａ2，…，ａnを求めること
が可能である。Even when the EELS detector is not used, another detection signal obtained by changing the detection angle of the EDX detector is increased to solve (n + 1) simultaneous equations and solve the coefficient a 0. , a 1, a 2, ... , it is possible to determine the a n.
【００２２】[0022]
【発明の実施の形態】以下、本発明の実施例について説
明する。ただし、以下に記載した数値や数式はあくまで
も説明の便宜のためのものであり、これによって本発明
が限定されるものではない。第１の実施例について説明
する。試料は半導体シリコン素子のコンタクト部であ
り、合金Ａｌ−Ｃｕ−Ｓｉとシリコンの間には、アルミ
ニウムとシリコンとの反応を避けるために、バリアメタ
ルと呼ばれるタングステンが使われている。ＦＩＢを用
いてＴＥＭ用断面試料を作成した。膜厚は約０.１μｍ
である。Embodiments of the present invention will be described below. However, the numerical values and mathematical formulas described below are for convenience of description only, and the present invention is not limited thereby. A first embodiment will be described. The sample is a contact portion of a semiconductor silicon element, and tungsten called a barrier metal is used between the alloy Al—Cu—Si and silicon in order to avoid a reaction between aluminum and silicon. A cross-section sample for TEM was prepared using FIB. The film thickness is about 0.1 μm
It is.
【００２３】図７に試料の断面構造を模式的に示す。シ
リコン基板２１上に部分的に酸化膜２２（ＬＯＣＯＳ）
を形成した後、ボロンリンガラス膜（ＢＰＳＧ）２３を
気相成長法により堆積する。ホトエッチング工程により
コンタクト部分を開口した後、バリアメタルであるタン
グステン２４をＤＣマグネトロンスパッタ法により形成
する。次に、７００℃、３０分間の熱処理を行ってシリ
サイド膜２６を形成する。続いて、Ａｌ−Ｃｕ−Ｓｉ合
金をスパッタ法により形成し、ホトエッチング工程によ
りアルミニウム配線２５を完成させる。タングステンシ
リサイド領域２６で、図中に示した丸印は、電子ビーム
を当てて元素分析を行う位置を示している。FIG. 7 schematically shows the cross-sectional structure of the sample. Partial oxide film 22 (LOCOS) on the silicon substrate 21
After forming, the boron phosphorus glass film (BPSG) 23 is deposited by vapor phase epitaxy. After opening the contact portion by a photoetching process, a barrier metal tungsten 24 is formed by a DC magnetron sputtering method. Next, heat treatment is performed at 700 ° C. for 30 minutes to form the silicide film 26. Subsequently, an Al-Cu-Si alloy is formed by a sputtering method, and the aluminum wiring 25 is completed by a photoetching process. In the tungsten silicide region 26, circles shown in the figure indicate positions where elemental analysis is performed by applying an electron beam.
【００２４】従来は、膜厚方向（ｚ軸方向）の元素濃度
は一定と仮定して、ｘ−ｙ面上での元素濃度分布を測定
していた。実際には膜厚方向に濃度分布があるため、各
点のｚ軸方向の濃度分布計測について述べる。検出器
は、試料面すなわちｘ−ｙ面に対して６０°の角度で設
置したＥＤＸと、ＥＥＬＳを用いた。ＥＥＬＳスペクト
ルでは、ＳｉとＷは、それぞれ９９ｅＶ、１８９７ｅＶ
の位置にピークが観察され、ピーク強度比からＷの平均
濃度は１４.８ａｔ％となった。次に、ＥＤＸ測定で
は、ＳｉとＷは、それぞれ１.７４ｅＶと８.４０ｅＶの
位置に特性Ｘ線のピークが観察され、ピーク強度比から
Ｗの見かけ上の濃度は５.１４ａｔ％となった。ＥＤＸ
によるＷの見かけ上の濃度が、ＥＥＬＳによるＷの平均
濃度より大であるため、定性的には、Ｗは膜の上面から
下面方向に減少していることがわかる。Conventionally, the element concentration distribution on the xy plane has been measured assuming that the element concentration in the film thickness direction (z-axis direction) is constant. Since the concentration distribution actually exists in the film thickness direction, the measurement of the concentration distribution in the z-axis direction at each point will be described. The detector used was EDX and EELS installed at an angle of 60 ° with respect to the sample surface, that is, the xy plane. In the EELS spectrum, Si and W are 99 eV and 1897 eV, respectively.
A peak was observed at the position of, and the average concentration of W was 14.8 at% from the peak intensity ratio. Next, in the EDX measurement, Si and W were observed to have characteristic X-ray peaks at positions of 1.74 eV and 8.40 eV, respectively, and the apparent concentration of W was 5.14 at% from the peak intensity ratio. . EDX
Since the apparent concentration of W according to (1) is higher than the average concentration of W according to EELS, it is qualitatively understood that W decreases from the upper surface to the lower surface of the film.
【００２５】ｚ軸方向のＷの濃度分布ｆ(ｚ)を次の一次
式で近似する場合は以下のようになる。 ｆ(ｚ)＝ａ0＋ａ1ｚ 膜厚０.１μｍの試料におけるＥＤＸの検出効率ｇ(６０
°,ｚ)は、経験的に次式で与えられる。When the concentration distribution f (z) of W in the z-axis direction is approximated by the following linear expression, it is as follows. f (z) = a 0 + a 1 z Detection efficiency of EDX in a sample having a film thickness of 0.1 μm g (60
°, z) is empirically given by the following equation.
【００２６】ｇ(６０°,ｚ)＝exp３０(ｚ−０.１) 従って、次式でｚを０と０.１μｍの間で積分して ＣEDX(６０°)＝∫ｆ(ｚ)ｇ(６０°,ｚ)ｄｚ ＝∫（ａ0＋ａ1ｚ）｛exp３０(ｚ−０.１)｝ｄｚ ＝３.１６×１０-2ａ0＋４.３９×１０-3ａ1 一方、ＥＥＬＳによる測定値から次式が得られる。ただ
し、ｚの積分は０と０.１μｍの間で行う。G (60 °, z) = exp30 (z-0.1) Therefore, z is integrated between 0 and 0.1 μm by the following equation, and C EDX (60 °) = ∫f (z) g (60 °, z) dz = ∫ (a 0 + a 1 z) {exp30 (z-0.1)} dz = 3.16 × 10 -2 a 0 + 4.39 × 10 -3 a 1 On the other hand, according to EELS The following formula is obtained from the measured values. However, z integration is performed between 0 and 0.1 μm.
【００２７】ＣEELS＝∫ｆ（ｚ）ｄｚ＝０.１ａ0＋５×
１０-3ａ1＝１.４８×１０-2 この連立方程式を解くと、ａ0＝０.１４０、ａ1＝０.１
６５となる。よって、膜厚方向の元素濃度分布は下式で
表される。 ｆ(ｚ)＝０.１４０＋０.１６５ｚ 以上のようにして各点のｚ軸方向の分布を求め、最終的
にｘ−ｙ−ｚ三次元空間におけるＷ元素濃度分布を示す
と、例えば図８のようになる。図８は、ｘ−ｙ面上のコ
ンタクト端部で、Ｗ濃度は大きなｚ軸依存性を示すこと
を表している。C EELS = ∫f (z) dz = 0.1a 0 + 5 ×
10 −3 a 1 = 1.48 × 10 −2 When this simultaneous equation is solved, a 0 = 0.140, a 1 = 0.1
It becomes 65. Therefore, the element concentration distribution in the film thickness direction is expressed by the following equation. f (z) = 0.140 + 0.165z As described above, the distribution of each point in the z-axis direction is obtained, and finally the W element concentration distribution in the xyz three-dimensional space is shown. Like FIG. 8 shows that the W concentration shows a large z-axis dependence at the contact end portion on the xy plane.
【００２８】次に、第２の実施例を示す。ここでは、Ｅ
ＥＬＳは用いずに、２台のＥＤＸ検出器を使用し、試料
面に対する検出角は０°と６０°に設定してある。ＥＤ
Ｘ検出器の取り出し角が０°の場合、検出効率に対する
膜厚方向の元素濃度分布の影響はほとんどなくなる。す
なわち、第１の実施例におけるＥＥＬＳ検出器と同様の
役割を果たす。従って、この信号強度から平均元素濃度
を算出し、両者の信号強度の差から濃度勾配を算出する
ことができる。Next, a second embodiment will be shown. Here, E
Two EDX detectors were used without using ELS, and the detection angles with respect to the sample surface were set to 0 ° and 60 °. ED
When the take-out angle of the X detector is 0 °, the influence of the element concentration distribution in the film thickness direction on the detection efficiency becomes almost zero. That is, it plays the same role as the EELS detector in the first embodiment. Therefore, the average element concentration can be calculated from this signal intensity, and the concentration gradient can be calculated from the difference in signal intensity between the two.
【００２９】次に、第３の実施例について説明する。試
料としては図７に断面構造を示す第１の実施例の場合と
同じ半導体シリコン素子のコンタクト部を用いた。検出
器としては検出角度を６０°及び３０°とした２台のＥ
ＤＸと１台のＥＥＬＳを用いた。すなわち、第１の実施
例の場合に比較して検出角度が３０°のＥＤＸ検出器を
１台増やして測定を行った。Next, a third embodiment will be described. As the sample, the same contact portion of the semiconductor silicon element as that of the first embodiment whose sectional structure is shown in FIG. 7 was used. Two detectors with detection angles of 60 ° and 30 °
DX and one EELS were used. That is, as compared with the case of the first embodiment, the number of EDX detectors having a detection angle of 30 ° was increased by one and the measurement was performed.
【００３０】前述のように、検出角度が６０°のＥＤＸ
によるＷ元素濃度の実測値ＣEDX(６０°)は５.１４ａｔ
％、ＥＥＳＬによるＷ元素濃度の測定値ＣEELSは１４.
８ａｔ％であり、本実施例で新たに測定した検出角度が
３０°のＥＤＸによるＷ元素濃度の実測値ＣEDX(３０
°)は３.８０ａｔ％であった。いま、試料のｚ方向の元
素濃度分布は次の２次の多項式で表されるとする。As described above, the EDX with the detection angle of 60 °
The actual measured value C EDX (60 °) of W element concentration by 5.14at
%, The measured value C EELS of the W element concentration by EESL is 14.
8 at%, and the actual measurement value of the W element concentration C EDX (30
°) was 3.80 at%. Now, assume that the element concentration distribution in the z direction of the sample is expressed by the following quadratic polynomial.
【００３１】ｆ(ｚ)＝ａ0＋ａ1ｚ＋ａ2ｚ2 ２台のＥＤＸによる見かけの検出濃度ＣEDX(６０°)，
ＣEDX(３０°)は各々次式で表される。 ＣEDX(６０°)＝∫ｆ(ｚ)ｇ(６０°,ｚ)ｄｚ ＣEDX(３０°)＝∫ｆ(ｚ)ｇ(３０°,ｚ)ｄｚ 検出角度がそれぞれ６０°と３０°の時のＥＤＸの検出
効率ｇ(６０°,ｚ)，ｇ(３０°,ｚ)は経験的に次式で与
えられる。F (z) = a 0 + a 1 z + a 2 z 2 Apparent detection density C EDX (60 °) by two EDX units,
C EDX (30 °) is expressed by the following equations. C EDX (60 °) = ∫f (z) g (60 °, z) dz C EDX (30 °) = ∫f (z) g (30 °, z) dz The detection angles are 60 ° and 30 °, respectively. The detection efficiencies g (60 °, z) and g (30 °, z) of the EDX at this time are empirically given by the following equations.
【００３２】ｇ(６０°,ｚ)＝exp３０(ｚ−０.１) ｇ(３０°,ｚ)＝exp４０(ｚ−０.１) これらの関係式を用いると次の連立方程式が得られる。 ＣEDX(６０°)＝0.317ａ0+2.28×10-3ａ1+1.81×10-4ａ
2＝5.14×10-3 ＣEDX(３０°)＝0.0246ａ0+1.89×10-3ａ1+1.56×10-4
ａ2＝3.80×10-3 ＣEELS＝0.1ａ0+5×10-2ａ1+3.33×10-4ａ2＝1.48×10
-2 これを解くことによりａ0，ａ1，ａ2が求められ、次式
で表されるＷ元素の濃度分布ｆ(ｚ)が得られる。G (60 °, z) = exp30 (z-0.1) g (30 °, z) = exp40 (z-0.1) The following simultaneous equations are obtained by using these relational expressions. C EDX (60 °) = 0.317a 0 + 2.28 × 10 -3 a 1 + 1.81 × 10 -4 a
2 = 5.14 x 10 -3 C EDX (30 °) = 0.0246a 0 +1.89 x 10 -3 a 1 +1.56 x 10 -4
a 2 = 3.80 × 10 -3 C EELS = 0.1a 0 + 5 × 10 -2 a 1 + 3.33 × 10 -4 a 2 = 1.48 × 10
-2 By solving this, a 0 , a 1 , and a 2 are obtained, and the concentration distribution f (z) of W element represented by the following equation is obtained.
【００３３】ｆ(ｚ)＝６.６６ｚ−５５.５ｚ2 図１０は、この濃度分布を図示したものである。図１０
と図８を比較すると明らかなように、ＥＤＸ検出器の数
を増やすことで試料の厚さ方向の濃度分布の測定精度が
向上する。次に、第４の実施例について説明する。本実
施例では、図４に示すように、ＥＤＸ検出器の検出角度
θを試料面に対して＋４５°から−４５°まで走査して
信号を取り込むことで、ＷとＳｉに対する信号を各検出
角度の関数として得る。各検出角度θにおけるＥＤＸ検
出器の検出効率ｇ(θ,ｚ)は、計算によりあるいは経験
的に知ることができるので、前述の方法と同様にして元
素の膜厚方向濃度分布を演算することができる。この場
合、データ数が増えた分だけ測定精度を上げることがで
きる。F (z) = 6.66z-55.5z 2 FIG. 10 illustrates this concentration distribution. FIG.
As is clear from a comparison between FIG. 8 and FIG. 8, increasing the number of EDX detectors improves the measurement accuracy of the concentration distribution of the sample in the thickness direction. Next, a fourth embodiment will be described. In the present embodiment, as shown in FIG. 4, by scanning the detection angle θ of the EDX detector from + 45 ° to −45 ° with respect to the sample surface and capturing signals, the signals for W and Si are detected at the respective detection angles. Get as a function of. Since the detection efficiency g (θ, z) of the EDX detector at each detection angle θ can be known by calculation or empirically, the concentration distribution of the element in the film thickness direction can be calculated in the same manner as the above method. it can. In this case, it is possible to improve the measurement accuracy by the amount of increased data.
【００３４】[0034]
【発明の効果】本発明によれば、試料の平面方向で高い
空間分解能を維持したまま、試料の膜厚（三次元）方向
の元素濃度分布を求めることが可能になる。According to the present invention, it is possible to obtain the element concentration distribution in the film thickness (three-dimensional) direction of the sample while maintaining a high spatial resolution in the plane direction of the sample.
【図１】分析電子顕微鏡の概略図。FIG. 1 is a schematic view of an analytical electron microscope.
【図２】特性Ｘ線発生の模式図。FIG. 2 is a schematic diagram of characteristic X-ray generation.
【図３】膜厚方向の元素濃度分布の違いによるＥＤＸ検
出効率の差を説明する図。FIG. 3 is a diagram illustrating a difference in EDX detection efficiency due to a difference in element concentration distribution in the film thickness direction.
【図４】ＥＤＸ検出器を角度走査する例の説明図。FIG. 4 is an explanatory diagram of an example in which an EDX detector is angularly scanned.
【図５】膜厚方向の元素濃度分布の説明図。FIG. 5 is an explanatory diagram of an element concentration distribution in the film thickness direction.
【図６】試料形状を利用して膜厚方向の元素濃度分布を
求める例の説明図。FIG. 6 is an explanatory diagram of an example of obtaining an element concentration distribution in the film thickness direction using a sample shape.
【図７】試料の断面模式図。FIG. 7 is a schematic sectional view of a sample.
【図８】ｘ−ｙ−ｚ方向の元素濃度分布実測例。FIG. 8 is an example of actual measurement of element concentration distribution in xyz directions.
【図９】ＥＤＸ検出効率の膜厚及び検出角度依存性を説
明する図。FIG. 9 is a diagram illustrating the dependence of EDX detection efficiency on film thickness and detection angle.
【図１０】膜厚方向の元素濃度分布を示す図。FIG. 10 is a diagram showing an element concentration distribution in the film thickness direction.
１…試料、２…ＥＤＸ検出器、３…ＥＥＬＳ検出器、４
…電子線、５…特性Ｘ線、６…電子銃、７…収束レン
ズ、８…対物レンズ、９…投射レンズ、１０…電子顕微
鏡像、１１…スリット、１２…演算装置、２１…シリコ
ン（Ｓｉ）、２２…シリコン酸化膜（ＳｉＯ2）、２３
…ボロホスホシリケートガラス（ＢＰＳＧ）、２４…タ
ングステン膜、２５…Ａｌ−Ｃｕ−Ｓｉ膜、２６…シリ
サイド領域1 ... Sample, 2 ... EDX detector, 3 ... EELS detector, 4
... electron beam, 5 ... characteristic X-ray, 6 ... electron gun, 7 ... converging lens, 8 ... objective lens, 9 ... projection lens, 10 ... electron microscope image, 11 ... slit, 12 ... arithmetic unit, 21 ... silicon (Si ), 22 ... Silicon oxide film (SiO 2 ), 23
... Borophosphosilicate glass (BPSG), 24 ... Tungsten film, 25 ... Al-Cu-Si film, 26 ... Silicide region
───────────────────────────────────────────────────── フロントページの続き (72)発明者 斎藤 雅和 茨城県日立市大みか町七丁目１番１号 株 式会社日立製作所日立研究所内 (72)発明者 砂子澤 成人 茨城県ひたちなか市市毛882番地 株式会 社日立製作所計測器事業部内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Masakazu Saito Inventor Masakazu Saito 7-1-1 Omika-cho, Hitachi City, Ibaraki Hitachi Ltd. Hitachi Research Laboratory, Ltd. Bachi Stock Company Hitachi Ltd. Measuring Instruments Division
Claims (7)
性Ｘ線による濃度信号と、試料を透過した電子線の電子
エネルギー損失スペクトルから得られる濃度信号とを演
算することにより試料の膜厚方向の元素濃度分布を求め
ることを特徴とする三次元元素濃度分布測定方法。1. An element in a film thickness direction of a sample by calculating a concentration signal by a characteristic X-ray generated from the sample by electron beam irradiation and a concentration signal obtained from an electron energy loss spectrum of an electron beam transmitted through the sample. A three-dimensional element concentration distribution measuring method characterized by obtaining a concentration distribution.
性Ｘ線を検出角度を異にする複数の検出器で計測し、各
検出器の信号強度を演算することにより試料の膜厚方向
の元素濃度分布を求めることを特徴とする三次元元素濃
度分布測定方法。2. A characteristic X-ray generated from a sample by electron beam irradiation is measured by a plurality of detectors having different detection angles, and the signal intensity of each detector is calculated to calculate the element concentration in the film thickness direction of the sample. A three-dimensional element concentration distribution measuring method characterized by obtaining a distribution.
性Ｘ線を検出角度を変化させて複数回計測し、各検出角
度における信号強度を演算することにより試料の膜厚方
向の元素濃度分布を求めることを特徴とする三次元元素
濃度分布測定方法。3. A characteristic X-ray generated from a sample by electron beam irradiation is measured a plurality of times by changing a detection angle, and a signal intensity at each detection angle is calculated to obtain an element concentration distribution in the film thickness direction of the sample. A three-dimensional element concentration distribution measuring method characterized by the following.
性Ｘ線を、試料による遮蔽状態の異なる複数の方向から
計測し、試料によって遮蔽された特性Ｘ線強度の変化か
ら試料の膜厚方向の元素濃度分布を求めることを特徴と
する三次元元素濃度分布測定方法。4. A characteristic X-ray generated from a sample by electron beam irradiation is measured from a plurality of directions in which the sample has different shielding states, and an element in the film thickness direction of the sample is determined from the change in the characteristic X-ray intensity shielded by the sample. A three-dimensional element concentration distribution measuring method characterized by obtaining a concentration distribution.
線照射軸の回りに回転して試料から発生する特性Ｘ線を
複数回計測し、計測した信号強度を演算することにより
試料の膜厚方向の元素濃度分布を求めることを特徴とす
る三次元元素濃度分布測定方法。5. A film of a sample is obtained by using a sample having an asymmetric shape, rotating the sample around an electron beam irradiation axis, measuring the characteristic X-rays generated from the sample a plurality of times, and calculating the measured signal intensity. A three-dimensional element concentration distribution measuring method characterized by obtaining an element concentration distribution in the thickness direction.
おいて、試料に電子線を照射し、試料から発生する特性
Ｘ線と試料を透過した電子線の電子エネルギー損失スペ
クトルを検出し、電子エネルギー損失スペクトル強度か
ら試料の膜厚方向の平均元素濃度を求め、特性Ｘ線信号
と電子エネルギー損失スペクトル信号との差から試料膜
厚方向の元素濃度分布の濃度勾配を求めることを特徴と
する元素分析方法。6. In an elemental analysis method using an analytical electron microscope, a sample is irradiated with an electron beam, and a characteristic X-ray generated from the sample and an electron energy loss spectrum of the electron beam transmitted through the sample are detected to obtain an electron energy loss spectrum. An elemental analysis method, characterized in that the average elemental concentration in the film thickness direction of the sample is obtained from the intensity, and the concentration gradient of the elemental concentration distribution in the sample film thickness direction is obtained from the difference between the characteristic X-ray signal and the electron energy loss spectrum signal.
により発生した電子線を試料に照射する手段と、試料か
ら発生した特性Ｘ線を検出する第１の検出器と、試料を
透過した電子線の電子エネルギー損失スペクトルを検出
する第２の検出器と、前記第１の検出器及び第２の検出
器の出力を演算して試料の膜厚方向の元素分布を求める
演算手段とを含むことを特徴とする三次元元素濃度分布
測定装置。7. An electron beam generating means, a means for irradiating the sample with an electron beam generated by the electron beam generating means, a first detector for detecting a characteristic X-ray generated from the sample, and a sample which has passed through the sample. A second detector for detecting an electron energy loss spectrum of the electron beam; and a calculating means for calculating outputs of the first detector and the second detector to obtain an element distribution in the film thickness direction of the sample. A three-dimensional element concentration distribution measuring device characterized in that
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|---|---|---|---|
| JP27595195A JP3323042B2 (en) | 1995-10-24 | 1995-10-24 | Method and apparatus for measuring three-dimensional element concentration distribution |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27595195A JP3323042B2 (en) | 1995-10-24 | 1995-10-24 | Method and apparatus for measuring three-dimensional element concentration distribution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH09119907A true JPH09119907A (en) | 1997-05-06 |
| JP3323042B2 JP3323042B2 (en) | 2002-09-09 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP27595195A Expired - Fee Related JP3323042B2 (en) | 1995-10-24 | 1995-10-24 | Method and apparatus for measuring three-dimensional element concentration distribution |
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| Country | Link |
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| JP (1) | JP3323042B2 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20030055841A (en) * | 2001-12-27 | 2003-07-04 | 삼성전자주식회사 | Method for measuring thickness of a BPSG film and measuring density of impurity in the BPSG film |
| WO2008099501A1 (en) * | 2007-02-16 | 2008-08-21 | Fujitsu Limited | Electronic microscope, and observing method |
| JPWO2008099501A1 (en) * | 2007-02-16 | 2010-05-27 | 富士通株式会社 | Electron microscope and observation method |
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| JP5254046B2 (en) * | 2007-02-16 | 2013-08-07 | 富士通株式会社 | Electron microscope and observation method |
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