JP2712759B2 - Small element diffusion analysis - Google Patents
Small element diffusion analysisInfo
- Publication number
- JP2712759B2 JP2712759B2 JP2136798A JP13679890A JP2712759B2 JP 2712759 B2 JP2712759 B2 JP 2712759B2 JP 2136798 A JP2136798 A JP 2136798A JP 13679890 A JP13679890 A JP 13679890A JP 2712759 B2 JP2712759 B2 JP 2712759B2
- Authority
- JP
- Japan
- Prior art keywords
- sample
- ray intensity
- concentration distribution
- electron beam
- apparent
- 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.)
- Expired - Fee Related
Links
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
Description
本発明は、コンピュータシミュレーションを用いて微
小部における元素拡散分析法に関する。The present invention relates to an element diffusion analysis method in a minute part using computer simulation.
組成の異なる複数の物質が接合されている試料におい
て、各物質の接合面においては、成分の拡散が生じてい
るが、この接合面における成分の拡散状態を分析するに
は、原理的にはEPMAを用い、２物質の接合境界線を横切
るように電子ビームを想定して線分析を行えばよいが、
実際には電子ビームを幾ら細く絞っても、試料に入射し
た電子が、試料内で拡散して、Ｘ線発生領域は加速電圧
にもよるが、１μｍ程度の広がりを有し、このため位置
分解能が不足して、接合面における拡散状態の分析はで
きなかった。In a sample in which a plurality of materials with different compositions are bonded, the diffusion of components occurs at the bonding surface of each material.To analyze the diffusion state of components at this bonding surface, in principle, EPMA The line analysis may be performed by assuming an electron beam so as to cross the junction boundary of the two substances.
In fact, no matter how narrow the electron beam is, the electron incident on the sample diffuses in the sample, and the X-ray generation area has a spread of about 1 μm, depending on the acceleration voltage. Was insufficient, and the state of diffusion at the joint surface could not be analyzed.
本発明は、EPMAを用い、EPMAの本来の位置分解能以上
の位置分解能で２物質接合面の拡散状態分析ができる方
法を提供することを目的とする。SUMMARY OF THE INVENTION An object of the present invention is to provide a method capable of analyzing a diffusion state of a two-material junction surface with EPMA using a positional resolution higher than the original positional resolution of the EPMA.
試料面に加速電子ビームを収束させ、試料から放射さ
れるＸ線を分光する分析装置を用い、試料の２物質接合
境界線を横切る走査線に沿って分析を行なう方法におい
て、或る適当な加速電圧で加速された電子ビームで励起
された測定試料から放射される成分元素の特性Ｘ線強度
と、上記と同じ加速電子ビームで励起された成分元素の
標準試料から放射される特性Ｘ線強度とのＸ線強度比か
ら測定試料の接合面付近の見掛け上の元素濃度分布を測
定し、上記測定と同じ条件でしかも接合境界面で拡散が
生じていない理想的な試料を想定してこの想定試料と上
記標準試料についてコンピュータシミュレーションを行
い、想定試料の接合面付近の計算によるＸ線強度比から
見掛け上の成分元素濃度分布を求め、走査線に沿って、
上記測定による見掛け上の元素濃度分布から上記計算に
よる見掛け上の元素濃度分布を引算し、元素拡散状態を
求めるようにした。In a method of analyzing an X-ray radiated from a sample by converging an accelerated electron beam on the sample surface and performing analysis along a scanning line that crosses a boundary between two materials of the sample, an appropriate acceleration is used. The characteristic X-ray intensity of the component element emitted from the measurement sample excited by the electron beam accelerated by the voltage and the characteristic X-ray intensity emitted from the standard sample of the component element excited by the same accelerated electron beam as described above The apparent element concentration distribution in the vicinity of the joint surface of the measurement sample was measured from the X-ray intensity ratio of the measurement sample. And the above-mentioned standard sample are subjected to computer simulation, and the apparent component element concentration distribution is obtained from the X-ray intensity ratio by calculation near the joint surface of the assumed sample, and along the scanning line,
The apparent element concentration distribution obtained by the above calculation was subtracted from the apparent element concentration distribution obtained by the above measurement to obtain the element diffusion state.
今、２物質の接合面で拡散の生じていない第３図の曲
線ａに示すような濃度分布を示す理想化された試料を想
定し、それを有限の位置分解能を有するEPMAで線分析し
たとすれば、測定結果として、第３図の曲線ｂに示すよ
うな元素Ａの見掛け上の濃度分布曲線が得られると考え
られる。この曲線ｂの形状は、EPMAの電子加速電圧，試
料によって決まる。実際の試料をEPMAによって分析を行
えば、第３図の曲線ｃに示すように、理想的な接合境界
面を想定した試料から得られるであろう曲線ｂより、更
に崩れた形状となる。この理由としては、実際の試料で
は、接合面で拡散が起こっていることが考えられる。こ
こで２つの濃度分布曲線b,cの同一位置における差をと
れば、この差（第４図の曲線ｄ）は、曲線ｂが理想の濃
度分布曲線であるａに対応しているから、理想の濃度分
布曲線からのずれ即ち元素Ａの拡散状態を表しているこ
とになる。 実際上第３図ａのような濃度分布の試料は得られない
ので、曲線ｂを実測的に得ることは不可能である。本発
明は、この曲線ｂを計算によって求めようとするもので
ある。 本発明は、上述した計算を本願出願人が出願した特願
昭63-45287号におけるコンピュータシミュレーションに
よるＸ線強度計算方法を用いて行う。上記コンピュータ
シミュレーションは、接合面で拡散の起きていない理想
的な試料を考え、電子ビームの加速電圧Ｅと電子ビーム
の照射位置における試料組成とから、特性Ｘ線強度を計
算するものである。 試料接合面における濃度分布は、実際には接合面を境
に濃度が急変していても、電子ビームの収束径や試料内
における電子の軌跡等によって、隣接する物質内の元素
に電子が衝突して、隣接する物質内の元素濃度の影響を
受けることになる。例えば、電子ビームの入射位置が接
合面であれば、隣接している物質の平均濃度が測定値と
して得られる。電子ビームの入射点が接合面から離れる
に従って、隣接する物質の影響が少なくなるので、特性
Ｘ線強度の測定による元素濃度分布は、一見元素が拡散
したように、接合面周辺で緩やかな変化状態となる。接
合面で元素拡散が起きていない試料を想定して、コンピ
ュータシミュレーションによって得られるＸ線強度から
濃度分布データを求めることで、接合面で拡散していな
い基準試料における見掛け上の濃度分布データ第３図ｂ
を得ることができ、測定試料を測定して得られた見掛け
上の濃度分布データとの比較によって元素拡散状態を分
析することが可能になる。Now, assuming an idealized sample having a concentration distribution as shown by a curve a in FIG. 3 in which no diffusion occurs at the bonding surface of the two substances, and performing a line analysis with EPMA having a finite positional resolution. Then, it is considered that an apparent concentration distribution curve of the element A as shown by a curve b in FIG. 3 is obtained as a measurement result. The shape of this curve b is determined by the electron acceleration voltage of EPMA and the sample. When an actual sample is analyzed by EPMA, as shown by a curve c in FIG. 3, the shape becomes more broken than a curve b which would be obtained from a sample assuming an ideal bonding interface. The reason may be that diffusion occurs at the bonding surface in the actual sample. Here, if the difference at the same position between the two density distribution curves b and c is taken, this difference (curve d in FIG. 4) indicates that the curve b corresponds to the ideal density distribution curve a. From the concentration distribution curve, that is, the diffusion state of the element A. Since a sample having a concentration distribution as shown in FIG. 3A cannot be obtained in practice, it is impossible to actually obtain the curve b. The present invention seeks to find this curve b by calculation. In the present invention, the above-described calculation is performed using the X-ray intensity calculation method by computer simulation in Japanese Patent Application No. 63-45287 filed by the present applicant. In the computer simulation, the characteristic X-ray intensity is calculated from the acceleration voltage E of the electron beam and the sample composition at the irradiation position of the electron beam, considering an ideal sample in which diffusion does not occur at the bonding surface. Regarding the concentration distribution at the sample joint surface, even if the concentration actually changes suddenly at the joint surface, electrons collide with elements in adjacent substances due to the convergence diameter of the electron beam and the electron trajectory in the sample. Therefore, it is affected by the element concentration in the adjacent substance. For example, if the incident position of the electron beam is at the bonding surface, the average concentration of adjacent substances can be obtained as a measured value. The influence of adjacent substances decreases as the point of incidence of the electron beam moves away from the bonding surface. Therefore, the element concentration distribution obtained by measuring characteristic X-ray intensity gradually changes around the bonding surface, as if the elements were diffused at first glance. Becomes By assuming a sample in which element diffusion does not occur at the bonding surface, the concentration distribution data is obtained from the X-ray intensity obtained by computer simulation. Figure b
Can be obtained, and the element diffusion state can be analyzed by comparison with apparent concentration distribution data obtained by measuring a measurement sample.
本発明の一実施例の測定動作を説明する。測定前に、
第１図に示すような、接合面を有する測定試料Ｓにおい
て、測定したい接合面における隣接物質X,Yの組成を調
査しておく、適当な加速電圧Ｅ0による電子ビーム（ビ
ーム径;10nm〜１μｍ）で試料Ｓの上記測定領域を走査
（走査ピッチ；ビーム径とほぼ同程度）し、測定試料Ｓ
の電子ビーム走査点（第２図,1,2,3……）における測定
元素Ａの夫々の特性Ｘ線強度ＩASを測定し、上記元素Ａ
の純品標準試料Ｋの特性Ｘ線強度ＩAKを測定する。上記
測定によって得られた試料Ｓの特性Ｘ線強度ＩASと、標
準試料Ｋの特性Ｘ線強度ＩAKとの比によって、各元素Ａ
のＸ線強度比ＫAEを求め、第３図に示すような、見掛け
上の濃度分布図を作成する。測定値は曲線ｃで、計算値
は曲線ｂで示してある。Ｘ線強度比は見掛け上の元素濃
度を示す数値である。予め調査した物質X,Yの組成，電
子ビームの加速電圧Ｅ0，電子ビームの上記走査点を設
定し、測定試料Ｓと同じ元素構成で接合面で拡散が生じ
ていない試料を想定し、この想定試料についてコンピュ
ータシミュレーションを行うと共に、測定元素Ａの標準
試料Ｋのコンピュータシミュレーションを行い、各照射
点における元素Ａの上記想定試料と標準試料とのコンピ
ュータシミュレーションによるＸ強度から計算上のＸ線
強度比ＫACを計算する。コンピュータシミュレーション
において、走査点内における電子ビームの照射点は、走
査点内において均一確率に分散されているとして計算す
る。計算によるＸ線強度比ＫACに適当な計数を掛けて、
接合面から離れた走査点においては、実測によるＸ線強
度比ＫAEと等しくなるようにする。濃度が低い物質側の
各走査点において、実測によるＸ線強度比ＫAEから計算
によるＸ線強度比ＫACを引算し、その差を求め、走査点
における強度比差を拡散度合い分布表として、第４図に
示すように表示する。この図が元素Ａの拡散状態を表し
ている。A measurement operation according to one embodiment of the present invention will be described. Before measurement
As shown in FIG. 1, the sample S having a bonding surface, adjacent material X at the bonding surface to be measured, previously investigated the composition of Y, appropriate acceleration voltage E 0 by the electron beam (beam diameter; 10 nm to 1 μm) to scan the above-mentioned measurement area of the sample S (scanning pitch; almost the same as the beam diameter),
Electron beam scanning point (Fig. 2, 1, 2, 3 ...) of the measured characteristic X-ray intensity I AS of each of the measurement element A in the above element A
The characteristic X-ray intensity I AK of the pure sample standard sample K is measured. The ratio of the characteristic X-ray intensity I AS of the sample S obtained by the above measurement to the characteristic X-ray intensity I AK of the standard sample K is determined by each element A
The X-ray intensity ratio K AE is determined to create an apparent concentration distribution diagram as shown in FIG. The measured value is shown by curve c and the calculated value is shown by curve b. The X-ray intensity ratio is a numerical value indicating an apparent element concentration. The composition of the substances X and Y investigated in advance, the acceleration voltage E 0 of the electron beam, and the scanning point of the electron beam are set, and a sample having the same element configuration as the measurement sample S and having no diffusion at the bonding surface is assumed. A computer simulation is performed on the assumed sample, and a computer simulation is performed on the standard sample K of the measurement element A. The calculated X-ray intensity ratio is calculated from the X intensity of the assumed sample and the standard sample of the element A at each irradiation point by the computer simulation. Calculate K AC . In the computer simulation, the calculation is performed on the assumption that the irradiation points of the electron beam within the scanning point are dispersed with uniform probability within the scanning point. Multiply the calculated X-ray intensity ratio K AC by an appropriate count,
At a scanning point away from the bonding surface, the X-ray intensity ratio KAE is set to be equal to the actually measured X-ray intensity ratio KAE . At each scanning point on the substance side having a low concentration, the calculated X-ray intensity ratio K AC is subtracted from the actually measured X-ray intensity ratio K AE , the difference is obtained, and the intensity ratio difference at the scanning point is used as a diffusion degree distribution table. , Are displayed as shown in FIG. This figure shows the diffusion state of the element A.
本発明によれば、コンピュータシミュレーションによ
って、組成の異なる多種の物質が接合されている試料に
おいて、接合面における指定元素の隣接物質への拡散状
態を把握することが可能になった。ADVANTAGE OF THE INVENTION According to this invention, it became possible to grasp | ascertain the spreading | diffusion state of the designated element in the joining surface to the adjacent substance in the sample to which various kinds of materials with different compositions are joined by computer simulation.
第１図は測定域における試料の断面図、第２図は電子ビ
ームの走査点説明図、第３図は測定領域における見掛け
上の濃度分布図、第４図は測定元素の拡散状態図であ
る。FIG. 1 is a sectional view of a sample in a measurement area, FIG. 2 is an explanatory view of an electron beam scanning point, FIG. 3 is an apparent concentration distribution chart in the measurement area, and FIG. .
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平３−209148（ＪＰ，Ａ) 特開 平３−209147（ＪＰ，Ａ) 特開 平３−295452（ＪＰ，Ａ) 特開 平４−2956（ＪＰ，Ａ) 特開 昭59−194336（ＪＰ，Ａ) ────────────────────────────────────────────────── ─── Continuation of the front page (56) References JP-A-3-209148 (JP, A) JP-A-3-209147 (JP, A) JP-A-3-295452 (JP, A) JP-A-4- 2956 (JP, A) JP-A-59-194336 (JP, A)
Claims (1)
から放射されるＸ線を分光する分析装置を用い、試料の
２物質接合境界線を横切る走査線に沿って分析を行なう
方法において、或る適当な加速電圧で加速された電子ビ
ームで励起された測定試料から放射される成分元素の特
性Ｘ線強度と、上記と同じ加速電子ビームで励起された
成分元素の標準試料から放射される特性Ｘ線強度とのＸ
線強度比から測定試料の接合面付近の見掛け上の元素濃
度分布を測定し、上記測定と同じ条件でしかも接合境界
面で拡散が生じていない理想的な試料を想定して、この
想定試料と前記標準試料についてコンピュータシミュレ
ーションを行ない、上記想定試料の接合面付近の上記計
算によるＸ線強度と標準試料の上記計算によるＸ線強度
の比から見掛け上の成分元素濃度分布を求め、走査線に
沿って、上記測定による見掛け上の元素濃度分布から上
記計算による見掛け上の元素濃度分布を引算し、元素拡
散状態を求めることを特徴とする微小部元素拡散分析
法。1. A method for analyzing an X-ray radiated from a sample by converging an accelerated electron beam on the surface of the sample and performing analysis along a scanning line crossing a boundary between two materials of the sample. The characteristic X-ray intensity of the component element emitted from the measurement sample excited by the electron beam accelerated by a certain appropriate acceleration voltage, and the emission from the standard sample of the component element excited by the same accelerated electron beam as described above X with characteristic X-ray intensity
Measure the apparent element concentration distribution near the joint surface of the measurement sample from the line intensity ratio, and assuming an ideal sample under the same conditions as above but without diffusion at the joint interface, A computer simulation is performed on the standard sample, and an apparent component element concentration distribution is determined from the ratio of the calculated X-ray intensity near the joint surface of the assumed sample to the calculated X-ray intensity of the standard sample. The elemental diffusion state is obtained by subtracting the apparent elemental concentration distribution by the above calculation from the apparent elemental concentration distribution by the above measurement.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2136798A JP2712759B2 (en) | 1990-05-25 | 1990-05-25 | Small element diffusion analysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2136798A JP2712759B2 (en) | 1990-05-25 | 1990-05-25 | Small element diffusion analysis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0431757A JPH0431757A (en) | 1992-02-03 |
| JP2712759B2 true JP2712759B2 (en) | 1998-02-16 |
Family
ID=15183767
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2136798A Expired - Fee Related JP2712759B2 (en) | 1990-05-25 | 1990-05-25 | Small element diffusion analysis |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2712759B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002039976A (en) * | 2000-07-19 | 2002-02-06 | Shimadzu Corp | Correction method of measurement data of electron beam micro analyzer |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7245695B2 (en) * | 2005-04-11 | 2007-07-17 | Jordan Valley Applied Radiation Ltd. | Detection of dishing and tilting using X-ray fluorescence |
-
1990
- 1990-05-25 JP JP2136798A patent/JP2712759B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002039976A (en) * | 2000-07-19 | 2002-02-06 | Shimadzu Corp | Correction method of measurement data of electron beam micro analyzer |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0431757A (en) | 1992-02-03 |
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