JP3295867B2 - Secondary ion mass spectrometry of oxygen in silicon. - Google Patents
Secondary ion mass spectrometry of oxygen in silicon.Info
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- JP3295867B2 JP3295867B2 JP08283394A JP8283394A JP3295867B2 JP 3295867 B2 JP3295867 B2 JP 3295867B2 JP 08283394 A JP08283394 A JP 08283394A JP 8283394 A JP8283394 A JP 8283394A JP 3295867 B2 JP3295867 B2 JP 3295867B2
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- Prior art keywords
- oxygen
- silicon
- mass spectrometry
- oxide film
- cssi
- Prior art date
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Testing Or Measuring Of Semiconductors Or The Like (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、ＭＯＳ ＩＣ等の電子
装置に用いられる単結晶シリコン、多結晶シリコン、ア
モルファスシリコンあるいは酸化シリコン等のシリコン
と酸素を含む試料中に含まれる酸素の濃度を定量評価す
るシリコン中の酸素の二次イオン質量分析法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for quantifying the concentration of oxygen contained in a sample containing silicon and oxygen such as single crystal silicon, polycrystal silicon, amorphous silicon or silicon oxide used in an electronic device such as a MOS IC. The present invention relates to secondary ion mass spectrometry of oxygen in silicon to be evaluated.
【０００２】[0002]
【従来の技術】従来から、ＭＯＳ ＩＣにおいては、ゲ
ート酸化膜として極めて薄い酸化シリコン膜を用いてい
るが、熱処理による酸化膜機能の低下やブレークスルー
等酸化膜に関する装置の製造上の問題が数多く存在し、
酸化膜中の酸素濃度についての情報は極めて重要であ
る。また、シリコン中の微量の酸素はドナー化等により
キャリア濃度に悪影響を与えることも知られている。2. Description of the Related Art Conventionally, in MOS ICs, an extremely thin silicon oxide film is used as a gate oxide film. However, there are many problems in manufacturing an oxide film related device such as deterioration of oxide film function due to heat treatment and breakthrough. Exists,
Information about the oxygen concentration in the oxide film is extremely important. It is also known that a small amount of oxygen in silicon has an adverse effect on the carrier concentration due to donor formation or the like.
【０００３】従来、二次イオン質量分析法（Ｓｅｃｏｎ
ｄａｒｙ Ｉｏｎ Ｍａｓｓ Ｓｐｅｃｔｒｏｍｅｔｒ
ｙ：ＳＩＭＳ）における酸素の定量方法は、一次イオン
にＣｓ+ を用いて試料からスパッタされるＯ- およびＳ
ｉ- の量を検出し、Ｏ- ／Ｓｉ- 比を用いる手法であっ
た。Conventionally, secondary ion mass spectrometry (Secon
dary Ion Mass Spectrometer
y: SIMS) is a method for quantifying oxygen by using O 2 and S − sputtered from a sample using Cs + as a primary ion.
i - amount detecting a, O - / Si - was a method of using the ratio.
【０００４】[0004]
【発明が解決しようとする課題】しかし、この手法によ
ると、Ｏ- の検出感度はマトリクス効果の影響を激しく
受け、ｐｐｍレベルの定量分析には利用可能でも、％オ
ーダの定量分析には利用することができない。また、近
年、酸化シリコン膜中の酸素の定量分析法としてＣｓＯ
+ ／ＣｓＳｉ + 比を用いる手法が提案されているが、こ
の手法においてはｐｐｍオーダから％オーダにわたる範
囲では著しくＣｓＯ+ ／ＣｓＳｉ+ 比が異なるため、ｐ
ｐｍオーダから％オーダにわたる範囲の定量分析を一様
に行うことはできない。However, according to this method,
Then, O-Detection sensitivity is strongly affected by the matrix effect
Can be used for quantitative analysis at the ppm level,
It cannot be used for quantitative analysis of radar. Also nearby
Year, CsO as a quantitative analysis method of oxygen in silicon oxide film
+/ CsSi +A method using the ratio has been proposed.
In the above method, the range from ppm order to% order is
Surrounded by CsO+/ CsSi+Because the ratios are different, p
Uniform quantitative analysis ranging from pm order to% order
Can not be done.
【０００５】本発明は、電子装置に用いられるシリコン
と酸素を含む試料中に存在する酸素の深さ方向あるいは
面方向の濃度分布を正確に評価し、また、酸素濃度分布
によって電子装置の特性を評価することを特徴とするシ
リコン中の酸素の二次イオン質量分析法を提供すること
を目的とする。The present invention accurately evaluates the concentration distribution of oxygen present in a sample containing silicon and oxygen used in an electronic device in a depth direction or a plane direction, and furthermore, the characteristics of the electronic device are determined by the oxygen concentration distribution. An object of the present invention is to provide a secondary ion mass spectrometry for oxygen in silicon, which is characterized by being evaluated.
【０００６】[0006]
【課題を解決するための手段】本発明にかかるシリコン
中の酸素の二次イオン質量分析法においては、前記の課
題を解決するために、Ｃｓ+ イオンをシリコンと酸素を
含む試料に照射し、該試料からスパッタされるＣｓ，
Ｏ，Ｓｉから形成される三原子複合イオンＣｓＯＳｉ+
およびＣｓ，Ｓｉから形成される二原子複合イオンＣｓ
Ｓｉ+ の量を検出し、ＣｓＯＳｉ+ ／ＣｓＳｉ+ 比と酸
素濃度の関係を示す検量線を作成し、該検量線を用いて
シリコンと酸素を含む試料中の酸素の深さ方向および面
方向濃度分布を定量する過程を採用した。In the secondary ion mass spectrometry of oxygen in silicon according to the present invention, a sample containing silicon and oxygen is irradiated with Cs + ions to solve the above-mentioned problems. Cs sputtered from the sample,
Triatomic complex ion CsOSi + formed from O, Si
Complex ion Cs formed from Cs and Si
The amount of Si + is detected, a calibration curve showing the relationship between the CsOSi + / CsSi + ratio and the oxygen concentration is created, and the depth direction and the in-plane concentration of oxygen in the sample containing silicon and oxygen are prepared using the calibration curve. The process of quantifying the distribution was adopted.
【０００７】この場合、検量線を作成する際、高濃度試
料として厚さ１０ｎｍ以上の酸化シリコン膜を用い、ま
たこの場合、酸化シリコン膜と下地との界面から１０ｎ
ｍ以上表面方向に離れた部分からＣｓＯＳｉ+ ／ＣｓＳ
ｉ+ 比を求めることによってＣｓＯＳｉ+ ／ＣｓＳｉ+
比を正確に求めることができる。In this case, when a calibration curve is prepared, a silicon oxide film having a thickness of 10 nm or more is used as a high-concentration sample, and in this case, 10 n from the interface between the silicon oxide film and the base.
m CsOSi + / CsS
By determining the i + ratio, CsOSi + / CsSi +
The ratio can be determined accurately.
【０００８】また、これらの場合、Ｃｓ+ イオンをシリ
コンと酸素を含む試料に、その法線方向に対して５５〜
７０度の範囲で照射することによって、試料の表面に溜
まるＣｓの量を低減して、ＣｓＯＳｉ+ シグナルを安定
化することができる。In these cases, Cs + ions are added to a sample containing silicon and oxygen by 55 to 55
By irradiating in the range of 70 degrees, the amount of Cs accumulated on the surface of the sample can be reduced, and the CsOSi + signal can be stabilized.
【０００９】[0009]
【作用】本発明のように、Ｃｓ+ イオンをシリコンと酸
素を含む試料に照射し、この試料からスパッタされるＣ
ｓ，Ｏ，Ｓｉから形成される三原子複合イオンＣｓＯＳ
ｉ+ およびＣｓ，Ｓｉから形成される二原子複合イオン
ＣｓＳｉ+ の量を検出して、ＣｓＯＳｉ+ ／ＣｓＳｉ+
比と酸素濃度の関係を示す検量線を作成し、この検量線
を用いてシリコンと酸素を含む試料中の酸素の深さ方向
および面方向濃度分布を定量すると、従来の二次イオン
質量分析法において問題になっていたマトリクス効果に
よる影響を取り除くことができ、ｐｐｍオーダから％オ
ーダにわたる範囲のシリコン中の酸素の量を一様に定量
することができる。According to the present invention, a sample containing silicon and oxygen is irradiated with Cs + ions, and Cs +
Trisomic complex ion CsOS formed from s, O, Si
By detecting the amount of the diatomic complex ion CsSi + formed from i + and Cs, Si, CsOSi + / CsSi +
When a calibration curve showing the relationship between the ratio and the oxygen concentration is created, and the depth and surface concentration distributions of oxygen in a sample containing silicon and oxygen are quantified using the calibration curve, the conventional secondary ion mass spectrometry In this method, the influence of the matrix effect, which has been a problem, can be removed, and the amount of oxygen in silicon ranging from the order of ppm to the order of% can be uniformly determined.
【００１０】[0010]
【実施例】以下、本発明の一実施例を説明する。この実
施例においては、フローティングゾーン法によって形成
されたＳｉ基板中にドーズ量を変えてイオン注入した試
料、およびチョクラルスキ法によって引き上げられたＣ
Ｚ−Ｓｉ基板上に熱酸化によって厚さ５０ｎｍの酸化シ
リコン膜を形成した試料を用いて検量線を作成し、この
検量線を用いてシリコン中の酸素の量を定量した。An embodiment of the present invention will be described below. In this embodiment, a sample obtained by ion-implanting a Si substrate formed by the floating zone method at a different dose and C pulled up by the Czochralski method were used.
A calibration curve was created using a sample in which a 50-nm-thick silicon oxide film was formed on a Z-Si substrate by thermal oxidation, and the amount of oxygen in silicon was quantified using the calibration curve.
【００１１】この実施例において、ドーズ量を変えて酸
素（16Ｏ+ ）をイオン注入したＦＺ−Ｓｉ基板の酸素イ
オン注入条件は下記のとおりである。 [0011] In this embodiment, oxygen ion implantation conditions of FZ-Si substrate by changing the dose amount of oxygen (16 O +) is ion-implanted are as follows.
【００１２】図１は、本発明の一実施例の検量線の説明
図である。この図において、横軸は酸素濃度を示し、縦
軸はＣｓＯＳｉ+ ／ＣｓＳｉ+ 強度比を示している。こ
の図によると、二次イオン強度比（○）は酸素濃度に対
して１×１０17〜５×１０22ｃｍ-3まで直線性を示して
いる。この場合、１×１０17ｃｍ-3は２ｐｐｍに値し、
５×１０22ｃｍ-3は酸化シリコン中の酸素濃度に対応す
る。FIG. 1 is an explanatory diagram of a calibration curve according to one embodiment of the present invention. In this figure, the horizontal axis indicates the oxygen concentration, and the vertical axis indicates the CsOSi + / CsSi + intensity ratio. According to this figure, the secondary ion intensity ratio (○) shows a linearity from 1 × 10 17 to 5 × 10 22 cm −3 with respect to the oxygen concentration. In this case, 1 × 10 17 cm −3 is equivalent to 2 ppm,
5 × 10 22 cm −3 corresponds to the oxygen concentration in silicon oxide.
【００１３】したがって、この実施例によると、ｐｐｍ
オーダから％オーダまでの検量線を作ることができ、一
様にｐｐｍオーダから％オーダの範囲にわたって酸素定
量分析を行うことができる。一方、この図に書き込まれ
た従来法によるＣｓＯ+ ／ＣｓＳｉ+ 強度比（□）は酸
素濃度が５×１０21ｃｍ-3を越えると急激に増大し、低
濃度領域における直線から大きく外れている。したがっ
て、従来法では、一様にｐｐｍオーダから％オーダまで
の範囲の酸素定量分析を行うことが不可能である。Therefore, according to this embodiment,
A calibration curve from order to% order can be made, and oxygen quantitative analysis can be uniformly performed over a range from ppm order to% order. On the other hand, the CsO + / CsSi + intensity ratio (□) according to the conventional method written in this figure rapidly increases when the oxygen concentration exceeds 5 × 10 21 cm -3 and largely deviates from the straight line in the low concentration region. . Therefore, in the conventional method, it is impossible to uniformly perform the oxygen quantitative analysis in the order of ppm to%.
【００１４】図２は、一次イオンの入射角が６０度のと
きの酸化シリコン膜の深さ方向の酸素量の分析結果説明
図である。この図において、横軸は酸化シリコン膜の深
さを示し、縦軸は強度（イオン個数）を示している。こ
の図は、シリコン基板の上に厚さ５０ｎｍの酸化シリコ
ン膜を形成した試料の深さ方向の酸素量を分析した結果
を示しているが、酸化シリコン膜中の、酸化シリコン膜
とシリコン基板の界面近傍の１０ｎｍの領域ではＣｓＯ
Ｓｉ+ のシグナルに異常が見られる。これは、界面近傍
で表面一次イオン濃度が変化するためと考えられる。し
たがって、酸素の定量分析の検量線を作成する場合はシ
リコン基板の上に厚さ１０ｎｍ以上の酸化シリコン膜を
用い、さらに、シリコン基板と酸化シリコン膜の界面１
０ｎｍ領域を外れた領域でのシグナルを用いることが望
ましい。FIG. 2 is an explanatory view of the analysis result of the oxygen amount in the depth direction of the silicon oxide film when the incident angle of the primary ions is 60 degrees. In this figure, the horizontal axis indicates the depth of the silicon oxide film, and the vertical axis indicates the intensity (number of ions). This figure shows the result of analyzing the oxygen amount in the depth direction of a sample in which a silicon oxide film having a thickness of 50 nm is formed on a silicon substrate. In a 10 nm region near the interface, CsO
Abnormalities are seen in the Si + signal. This is considered because the surface primary ion concentration changes near the interface. Therefore, when preparing a calibration curve for quantitative analysis of oxygen, a silicon oxide film having a thickness of 10 nm or more is used on a silicon substrate, and further, an interface 1 between the silicon substrate and the silicon oxide film is used.
It is desirable to use a signal in a region outside the 0 nm region.
【００１５】図３は、一次イオンの入射角が５０度のと
きの酸化シリコン膜の深さ方向の酸素量の分析結果説明
図である。この図において、横軸は酸化シリコン膜の深
さを示し、縦軸は強度（イオン個数）を示している。こ
の図によると、ＣｓＳｉ+ のシグナルに比べてＣｓＯＳ
ｉ+ のシグナルが不安定であることがわかる。FIG. 3 is an explanatory diagram of the analysis result of the oxygen amount in the depth direction of the silicon oxide film when the incident angle of the primary ions is 50 degrees. In this figure, the horizontal axis indicates the depth of the silicon oxide film, and the vertical axis indicates the intensity (number of ions). According to this figure, CSOS compared to signals CsSi +
It can be seen that the signal of i + is unstable.
【００１６】また、ＣｓＯＳｉ+ のシグナルはＣｓ+ の
シグナルに影響を受け、Ｃｓ+ のシグナルとは正反対の
挙動を示している。絶縁体中でのアルカリ金属は動きや
すく、必要以上に試料表面にＣｓを溜めることはＣｓＯ
Ｓｉ+ のシグナルを不安定状態に導くと考えられる。[0016] In addition, CsOSi + of the signal is affected by the Cs + of the signal, the Cs + signal shows the opposite behavior. Alkali metals in insulators are easy to move, and storing Cs on the sample surface more than necessary is
It is considered that the Si + signal leads to an unstable state.
【００１７】図４は、Ｃｓ+ イオンの法線に対する入射
角とスパッタリングイールドの関係説明図である。この
図に示されるように、一次イオンの法線に対する入射角
が５５〜７０度であるとき、スパッタリングイールドが
大きくなっている。したがって、Ｃｓ+ 一次イオン入射
角をスパッタリングイールドが大きい５５〜７０度に保
ち、表面Ｃｓ濃度を最小限に抑えることが望ましい。FIG. 4 is a diagram illustrating the relationship between the incident angle of the Cs + ion with respect to the normal line and the sputtering yield. As shown in this figure, when the incident angle of the primary ions with respect to the normal line is 55 to 70 degrees, the sputtering yield is large. Therefore, it is desirable to keep the Cs + primary ion incident angle at 55 to 70 degrees where the sputtering yield is large and to minimize the surface Cs concentration.
【００１８】なお、この実施例においては、酸素をイオ
ン注入したシリコン基板およびシリコン基板の上に酸化
シリコン膜を形成した試料を用いた例を説明したが、Ｓ
ｉを添加したＡｌ−Ｃｕ合金からなる配線中の酸素を定
量する場合等、シリコンと酸素を含む試料中の酸素を定
量する場合に適用することができる。In this embodiment, an example using a silicon substrate into which oxygen has been ion-implanted and a sample having a silicon oxide film formed on the silicon substrate has been described.
The present invention can be applied to a case where oxygen in a sample containing silicon and oxygen is determined, such as a case where oxygen in an Al-Cu alloy to which i is added is determined.
【００１９】[0019]
【発明の効果】以上説明したように、本発明によるシリ
コンと酸素を含む試料中の酸素の定量分析方法は、ｐｐ
ｍ〜％オーダまで酸素を一様に定量することができ、電
子装置の特性の評価技術の向上に寄与するところが大き
い。As described above, the method for quantitatively analyzing oxygen in a sample containing silicon and oxygen according to the present invention is based on pp.
Oxygen can be uniformly quantified in the order of m to%, which greatly contributes to the improvement of the technology for evaluating the characteristics of electronic devices.
【図１】本発明の一実施例の検量線の説明図である。FIG. 1 is an explanatory diagram of a calibration curve according to one embodiment of the present invention.
【図２】一次イオンの入射角が６０度のときの酸化シリ
コン膜の深さ方向の酸素量の分析結果説明図である。FIG. 2 is an explanatory diagram of an analysis result of an oxygen amount in a depth direction of a silicon oxide film when an incident angle of a primary ion is 60 degrees.
【図３】一次イオンの入射角が５０度のときの酸化シリ
コン膜の深さ方向の酸素量の分析結果説明図である。FIG. 3 is an explanatory diagram of an analysis result of an oxygen amount in a depth direction of a silicon oxide film when an incident angle of a primary ion is 50 degrees.
【図４】Ｃｓ+ イオンの法線に対する入射角とスパッタ
リングイールドの関係説明図である。FIG. 4 is an explanatory diagram showing a relationship between an incident angle of Cs + ions with respect to a normal line and a sputtering yield.
フロントページの続き (58)調査した分野(Int.Cl.7，ＤＢ名) G01N 23/225 G01N 27/62 H01L 21/66 Continuation of the front page (58) Field surveyed (Int.Cl. 7 , DB name) G01N 23/225 G01N 27/62 H01L 21/66
Claims (4)
料に照射し、該試料からスパッタされるＣｓ，Ｏ，Ｓｉ
から形成される三原子複合イオンＣｓＯＳｉ + およびＣ
ｓ，Ｓｉから形成される二原子複合イオンＣｓＳｉ+ の
量を検出し、ＣｓＯＳｉ+ ／ＣｓＳｉ+ 比と酸素濃度の
関係を示す検量線を作成し、該検量線を用いてシリコン
と酸素を含む試料中の酸素の深さ方向および面方向濃度
分布を定量することを特徴とするシリコン中の酸素の二
次イオン質量分析法。1. Cs+Ions containing silicon and oxygen
Cs, O, Si sputtered from the sample
Complex ion CsOSi formed from +And C
Diatomic complex ion CsSi formed from s, Si+of
The amount of CsOSi+/ CsSi+Ratio and oxygen concentration
Create a calibration curve showing the relationship and use the calibration curve to
And planar concentrations of oxygen in samples containing oxygen and oxygen
Characterizing oxygen distribution in silicon characterized by quantifying distribution
Secondary ion mass spectrometry.
厚さ１０ｎｍ以上の酸化シリコン膜を用いることを特徴
とする請求項１に記載されたシリコン中の酸素の二次イ
オン質量分析法。2. The secondary ion mass spectrometry of oxygen in silicon according to claim 1, wherein a silicon oxide film having a thickness of 10 nm or more is used as the high-concentration sample when preparing the calibration curve.
る際、酸化シリコン膜と下地との界面から１０ｎｍ以上
表面方向に離れた部分からＣｓＯＳｉ+ ／ＣｓＳｉ+ 比
を求めることを特徴とする請求項１または請求項２に記
載されたシリコン中の酸素の二次イオン質量分析法。3. The method according to claim 1, wherein when the calibration curve is formed using the silicon oxide film, the CsOSi + / CsSi + ratio is obtained from a portion separated from the interface between the silicon oxide film and the base by 10 nm or more in the surface direction. The secondary ion mass spectrometry of oxygen in silicon according to claim 1 or 2.
料に、その法線方向に対して５５〜７０度の範囲で照射
しＣｓＯＳｉ+ 、ＣｓＳｉ+ の量を求めることを特徴と
する請求項１、請求項２または請求項３に記載されたシ
リコン中の酸素の二次イオン質量分析法。4. The method according to claim 1, wherein the sample containing silicon and oxygen is irradiated with Cs + ions in a range of 55 to 70 degrees with respect to the normal direction of the sample to obtain the amounts of CsOSi + and CsSi +. The secondary ion mass spectrometry of oxygen in silicon according to claim 2 or 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP08283394A JP3295867B2 (en) | 1994-04-21 | 1994-04-21 | Secondary ion mass spectrometry of oxygen in silicon. |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP08283394A JP3295867B2 (en) | 1994-04-21 | 1994-04-21 | Secondary ion mass spectrometry of oxygen in silicon. |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07294462A JPH07294462A (en) | 1995-11-10 |
| JP3295867B2 true JP3295867B2 (en) | 2002-06-24 |
Family
ID=13785415
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP08283394A Expired - Fee Related JP3295867B2 (en) | 1994-04-21 | 1994-04-21 | Secondary ion mass spectrometry of oxygen in silicon. |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111116181B (en) * | 2018-10-31 | 2022-04-15 | 南京梅山冶金发展有限公司 | Refractory material lining of torpedo car and construction process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP4574293B2 (en) * | 2004-09-08 | 2010-11-04 | 富士通株式会社 | Crystallinity evaluation method |
| JP6805015B2 (en) * | 2017-02-10 | 2020-12-23 | グローバルウェーハズ・ジャパン株式会社 | Calibration curve preparation method, carbon concentration measurement method, and silicon wafer manufacturing method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111116181B (en) * | 2018-10-31 | 2022-04-15 | 南京梅山冶金发展有限公司 | Refractory material lining of torpedo car and construction process |
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| Publication number | Publication date |
|---|---|
| JPH07294462A (en) | 1995-11-10 |
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