JPH09199558A - Method for measuring surface oxygen concentration of semiconductor substrate - Google Patents

Method for measuring surface oxygen concentration of semiconductor substrate

Info

Publication number
JPH09199558A
JPH09199558A JP2325096A JP2325096A JPH09199558A JP H09199558 A JPH09199558 A JP H09199558A JP 2325096 A JP2325096 A JP 2325096A JP 2325096 A JP2325096 A JP 2325096A JP H09199558 A JPH09199558 A JP H09199558A
Authority
JP
Japan
Prior art keywords
oxygen concentration
dislocation
substrate
dent
measured
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
JP2325096A
Other languages
Japanese (ja)
Inventor
Masanori Akatsuka
雅則 赤塚
Koji Sueoka
浩治 末岡
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.)
Nippon Steel Corp
Original Assignee
Sumitomo Sitix Corp
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 Sumitomo Sitix Corp filed Critical Sumitomo Sitix Corp
Priority to JP2325096A priority Critical patent/JPH09199558A/en
Publication of JPH09199558A publication Critical patent/JPH09199558A/en
Pending legal-status Critical Current

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  • Testing Or Measuring Of Semiconductors Or The Like (AREA)

Abstract

PROBLEM TO BE SOLVED: To precisely measure the surface oxygen concentration of a silicon wafer in a short time, by forming a dent on a substrate surface, heat-treating the substrate, measuring the moving distance of dislocation from the dent which is made distinctive by defect selective etching, and estimating the oxygen concentration from the relation between the oxygen concentration and the dislocation moving distance. SOLUTION: After a dent is formed on the surface of a semiconductor substrate by a load of 1-2000g, the substrate is heat-treated at 600-1000 deg.C for 1-60 minutes. By performing defect selective etching to be 0.1-30μm deep, dislocation generated during the heat treatment is made distinctive, and the moving distance of the dislocation from the dent is measured. The surface oxygen concentration of the substrate is estimated from the relation between the previously set oxygen concentration and the dislocation moving distance. For example, dent formation, heat treatment and defect selective etching are previously performed for various kinds of silicon wafers different in oxygen concentration, and the moving distances of the dislocations from the dents are measured. Thereby the relation, shown in figure, between known oxygen concentrations and measured dislocation moving distances is obtained.

Description

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

【0001】[0001]

【発明の属する技術分野】この発明は、LSI等の基板
として用いられる半導体基板の表面酸素濃度の測定方法
に係り、基板表面に圧痕を設けて熱処理し、その後欠陥
選択エッチングで転位を顕在化し転位の圧痕からの移動
距離より酸素濃度を推定することにより、短時間で容易
に測定できる半導体基板の表面酸素濃度測定方法に関す
る。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for measuring the surface oxygen concentration of a semiconductor substrate used as a substrate for an LSI or the like, in which an indentation is provided on the substrate surface for heat treatment, and then dislocation is revealed by defect selective etching. The present invention relates to a method for measuring the surface oxygen concentration of a semiconductor substrate, which can be easily measured in a short time by estimating the oxygen concentration from the moving distance from the indentation.

【0002】[0002]

【従来の技術】シリコン等の半導体結晶中には、結晶成
長時に坩堝から混入した酸素が格子間酸素として存在す
る。この格子間酸素は、LSI等のデバイス製造プロセ
スにおいて、酸素析出物として結晶内に析出し、デバイ
ス特性に影響を与える。そのため、酸素濃度を把握する
ことは非常に重要である。
2. Description of the Related Art In a semiconductor crystal such as silicon, oxygen mixed from a crucible during crystal growth exists as interstitial oxygen. This interstitial oxygen is precipitated in the crystal as an oxygen precipitate in a device manufacturing process such as LSI and affects the device characteristics. Therefore, it is very important to understand the oxygen concentration.

【0003】シリコンウェーハの酸素濃度の測定には、
一般にはFT−IR等の赤外吸収法が用いられている
(小間ら著、「シリコンの物性と評価法」(丸善)19
87)。しかし、この方法はウェーハ透過光スペクトル
により酸素濃度を求めるため、結晶の表面層のみの酸素
濃度を求めることは不可能であった。そのため、例えば
結晶熱処理時に生じた外方拡散層のみの酸素濃度を測定
することは困難であった。
To measure the oxygen concentration of a silicon wafer,
In general, infrared absorption methods such as FT-IR are used (Koma et al., "Physical properties and evaluation methods of silicon" (Maruzen) 19
87). However, since this method determines the oxygen concentration from the wafer transmitted light spectrum, it was impossible to determine the oxygen concentration only in the surface layer of the crystal. Therefore, for example, it is difficult to measure the oxygen concentration of only the outer diffusion layer generated during the crystal heat treatment.

【0004】表面酸素濃度の測定法としては、他に、二
次イオン質量分析法(Secondary Ion M
ass Spectrometry;以下SIMSと略
す)がある(前掲「シリコンの物性と評価法」198
7)。この方法はウェーハの深さ方向の元素分析を高精
度に行うことができるため、半導体材料の評価には欠か
せない方法である。しかし、原子レベルでのスパッタリ
ング現象を用いているため、我々が必要としているμm
オーダーでの測定には相当の時間を要するといった欠点
がある。
Another method for measuring the surface oxygen concentration is secondary ion mass spectrometry (Secondary Ion M).
Ass Spectrometry; hereinafter abbreviated as SIMS) (above-mentioned "Physical properties and evaluation method of silicon" 198)
7). This method is indispensable for the evaluation of semiconductor materials because it enables highly accurate elemental analysis in the depth direction of the wafer. However, because the sputtering phenomenon at the atomic level is used,
There is a drawback that measurement on the order takes a considerable amount of time.

【0005】[0005]

【発明が解決しようとする課題】上述のごとく、シリコ
ンウェーハにおけるμmオーダーの表面層のみの酸素濃
度を求めることは、従来の赤外吸収法では不可能であ
り、SIMSではかなりの時間を要する問題があった。
As described above, the conventional infrared absorption method cannot determine the oxygen concentration of only the μm-order surface layer of a silicon wafer, and SIMS requires a considerable amount of time. was there.

【0006】この発明は、上述の従来法の現状に鑑み、
シリコンウェーハの表面酸素濃度の測定を精度よく短時
間で測定が可能となる半導体基板の表面酸素濃度測定方
法の提供を目的としている。
The present invention has been made in view of the current state of the conventional method described above.
An object of the present invention is to provide a method for measuring the surface oxygen concentration of a semiconductor substrate, which enables accurate measurement of the surface oxygen concentration of a silicon wafer in a short time.

【0007】[0007]

【課題を解決するための手段】発明者らは、シリコンウ
ェーハにおけるμmオーダーの表面層のみの酸素濃度を
短時間で容易に求めることが可能な測定方法について、
種々検討した結果、基板表面に圧痕を設けて熱処理し、
その後欠陥選択エッチングで顕在化した転位の圧痕から
の移動距離を測定し、酸素濃度と転位移動距離の関係か
ら酸素濃度を推定することが可能であることを知見し、
この発明を完成した。
Means for Solving the Problems The inventors have proposed a measuring method capable of easily obtaining the oxygen concentration of only a μm-order surface layer of a silicon wafer in a short time.
As a result of various examinations, heat treatment was performed by providing an indentation on the substrate surface
After that, it was found that it is possible to estimate the oxygen concentration from the relationship between the oxygen concentration and the dislocation migration distance by measuring the migration distance from the indentation of dislocations revealed by defect selective etching.
The present invention has been completed.

【0008】すなわち、この発明は、半導体基板の表面
に1〜2000gの荷重で圧痕を付けた後に600℃〜
1000℃の熱処理を1〜60分間行い、欠陥選択エッ
チングを0.1μm〜30μm施して熱処理中に生じた
転位を顕在化し、転位の圧痕からの移動距離を測定し、
予め設定した酸素濃度と転位移動距離の関係から、基板
の表面酸素濃度を推定する半導体基板の表面酸素濃度測
定方法である。
That is, according to the present invention, after indenting the surface of the semiconductor substrate with a load of 1 to 2000 g, the temperature of 600.degree.
The heat treatment at 1000 ° C. is performed for 1 to 60 minutes, the defect selective etching is performed at 0.1 μm to 30 μm to reveal the dislocations generated during the heat treatment, and the moving distance from the dislocation indentation is measured.
This is a method for measuring the surface oxygen concentration of a semiconductor substrate, in which the surface oxygen concentration of the substrate is estimated from the relationship between the preset oxygen concentration and the dislocation movement distance.

【0009】[0009]

【発明の実施の形態】この発明による表面酸素濃度測定
方法は、フローチャートを図1に示すごとく、まず、シ
リコンウェーハの表面に、ビッカース硬度計によって1
〜2000gの荷重で圧痕を付ける。荷重は、転位発生
に充分な応力を付加するには1g以上必要であり、20
00gを超える荷重ではウェーハに割れを生じるため、
1〜2000gとする。
BEST MODE FOR CARRYING OUT THE INVENTION The method for measuring surface oxygen concentration according to the present invention is as follows. First, as shown in the flow chart of FIG.
Make an impression with a load of ~ 2000g. The load must be 1 g or more to apply sufficient stress for dislocation generation.
Since a wafer will crack under a load of more than 00g,
It is 1 to 2000 g.

【0010】圧痕を付けた後、600℃〜1000℃の
炉中で1〜60分間熱処理を行う。熱処理温度が600
℃未満、並びに処理時間が1分未満では転位が充分に運
動できず、また、1000℃を越え、処理時間が60分
を越えると測定中にウェーハ表面からの酸素の外方拡散
が生じてしまい、正確な測定が行えないため、熱処理温
度は600℃〜1000℃、処理時間は1〜60分間と
する。
After making the indentation, heat treatment is performed in a furnace at 600 ° C. to 1000 ° C. for 1 to 60 minutes. Heat treatment temperature is 600
If the temperature is lower than ℃ and the processing time is less than 1 minute, dislocations cannot move sufficiently, and if the temperature exceeds 1000 ° C. and the processing time exceeds 60 minutes, outward diffusion of oxygen from the wafer surface occurs during measurement. Since the accurate measurement cannot be performed, the heat treatment temperature is 600 ° C. to 1000 ° C. and the treatment time is 1 to 60 minutes.

【0011】熱処理に続いて、0.1〜30μmの欠陥
選択エッチングによって転位を顕在化させる。さらに、
転位の圧痕からの移動距離を光学顕微鏡で測定する。欠
陥選択エッチング深さは、0.1μm未満では光学顕微
鏡での観察が困難なため、また、転位は表面から高々3
0μmの深さの領域を移動するため、30μmを越えて
行う必要がないため、エッチング深さは0.1〜30μ
mとする。
Following the heat treatment, dislocations are revealed by defect selective etching of 0.1 to 30 μm. further,
The migration distance of the dislocation from the indentation is measured with an optical microscope. If the defect selective etching depth is less than 0.1 μm, it is difficult to observe with an optical microscope, and dislocations are at most 3 from the surface.
Since the region having a depth of 0 μm is moved, it is not necessary to perform the etching over 30 μm. Therefore, the etching depth is 0.1 to 30 μm.
m.

【0012】この発明は転位の圧痕からの移動距離から
酸素濃度を得ることを特徴とするが、このため、予め酸
素濃度が異なる種々のシリコンウェーハについて、上記
の圧痕付け、熱処理、欠陥選択エッチングをそれぞれ施
し、転位の圧痕からの移動距離を測定し、既知の酸素濃
度と測定した転位移動距離の関係を求めておく必要があ
る。この酸素濃度と転位移動距離の関係を図2に示す。
The present invention is characterized in that the oxygen concentration is obtained from the distance traveled from the dislocation indentation. Therefore, various silicon wafers having different oxygen concentrations are subjected to the above-mentioned indentation, heat treatment, and defect selective etching. It is necessary to perform each of them, measure the moving distance of the dislocation from the indentation, and obtain the relationship between the known oxygen concentration and the measured dislocation moving distance. The relationship between the oxygen concentration and the dislocation movement distance is shown in FIG.

【0013】図2より明らかなように、ウェーハ中の酸
素濃度が高くなるにつれて、転位の移動距離が短くなる
ことが分かる。この酸素濃度と転位移動距離の関係か
ら、未知の酸素濃度のシリコンウェーハの酸素濃度を容
易に知ることができる。
As is clear from FIG. 2, it is understood that the dislocation migration distance becomes shorter as the oxygen concentration in the wafer becomes higher. From the relationship between the oxygen concentration and the dislocation movement distance, the oxygen concentration of a silicon wafer having an unknown oxygen concentration can be easily known.

【0014】[0014]

【実施例】【Example】

実施例1 酸素濃度が未知であるシリコンウェーハの酸素濃度をこ
の発明による測定方法を用いて測定した。まず、ウェー
ハ表面にビッカース硬度計で100gの荷重で圧痕を付
けた。次に、900℃の炉中で30分間熱処理を行っ
た。炉への投入取り出しは、シリコンウェーハに熱応力
による欠陥が導入されないように、ボート速度(15c
m/分)、ウェーハ間隔(20mm)で行った。続い
て、深さ5μmの欠陥選択エッチングを行った。
Example 1 The oxygen concentration of a silicon wafer whose oxygen concentration is unknown was measured using the measuring method according to the present invention. First, the surface of the wafer was indented with a Vickers hardness meter under a load of 100 g. Next, heat treatment was performed for 30 minutes in a furnace at 900 ° C. The loading and unloading to and from the furnace are performed at a boat speed (15c) so that defects due to thermal stress are not introduced into the silicon wafer.
m / min) and the wafer interval (20 mm). Subsequently, defect selective etching having a depth of 5 μm was performed.

【0015】さらに、転位移動距離を光学顕微鏡で測定
した。圧痕から広がる転位の様子を図3に示す。この転
位移動距離を測定したところ90μmであった。酸素濃
度と転位移動距離の関係を求めた図2からこのウェーハ
の表面酸素濃度は、11×1017cm-3(old AS
TM)と推測される。
Further, the dislocation movement distance was measured with an optical microscope. The state of dislocations spreading from the indentation is shown in FIG. The dislocation movement distance was measured and found to be 90 μm. From the relationship between oxygen concentration and dislocation migration distance obtained in FIG. 2, the surface oxygen concentration of this wafer was 11 × 10 17 cm −3 (old AS
TM).

【0016】当該ウェーハの同一箇所の表面酸素濃度を
SIMSで測定したところ、11×1017cm-3(ol
d ASTM)とこの発明による測定方法と同じ測定結
果が得られた。従って、転位移動距離を光学顕微鏡で測
定し図2の換算グラフから容易に酸素濃度を正確に推定
できることが分かる。
When the surface oxygen concentration at the same location on the wafer was measured by SIMS, it was 11 × 10 17 cm -3 (ol
d ASTM) and the same measurement results as the measurement method according to the present invention were obtained. Therefore, it can be understood that the oxygen concentration can be easily and accurately estimated from the conversion graph of FIG. 2 by measuring the dislocation movement distance with an optical microscope.

【0017】実施例2 次に、SIMSとこの発明の方法での測定時間の比較を
行った。ウェーハ面内100点を深さ10μmまで測定
したときの測定時間を表1にまとめた。この発明による
測定方法はSIMSに比べて、測定時間を大幅に短縮で
きることが分かる。
Example 2 Next, a comparison was made between SIMS and the measurement time of the method of the present invention. Table 1 shows the measurement time when 100 points on the wafer surface were measured to a depth of 10 μm. It can be seen that the measuring method according to the present invention can significantly reduce the measuring time as compared with SIMS.

【0018】[0018]

【表1】 [Table 1]

【0019】[0019]

【発明の効果】この発明は、シリコンウェーハにおける
μmオーダーの表面層のみの酸素濃度を求めることは、
従来の赤外吸収法では不可能であり、SIMSではかな
りの時間を要する問題があったが、実施例より明らかな
ように、半導体基板の表面領域の酸素濃度を短時間で正
確に実施できるようになった。
According to the present invention, it is possible to obtain the oxygen concentration of only the surface layer of the μm order in a silicon wafer.
The conventional infrared absorption method is not possible, and SIMS has a problem that it takes a considerable amount of time. However, as is clear from the examples, the oxygen concentration in the surface region of the semiconductor substrate can be accurately measured in a short time. Became.

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

【図1】この発明による半導体基板の表面酸素濃度測定
方法の工程を示すフローチャート図である。
FIG. 1 is a flowchart showing steps of a method for measuring surface oxygen concentration of a semiconductor substrate according to the present invention.

【図2】酸素濃度と転位移動距離の関係を示すグラフで
ある。
FIG. 2 is a graph showing the relationship between oxygen concentration and dislocation movement distance.

【図3】圧痕から広がる転位の様子を示す顕微鏡写真を
トレースした説明図である。
FIG. 3 is an explanatory diagram tracing a micrograph showing a state of dislocations spreading from an indentation.

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】 半導体基板の表面に1〜2000gの荷
重で圧痕を付けた後に600℃〜1000℃の熱処理を
1〜60分間行い、欠陥選択エッチングを0.1μm〜
30μm施して熱処理中に生じた転位を顕在化し、転位
の圧痕からの移動距離を測定し、予め設定した酸素濃度
と転位移動距離の関係から、基板の表面酸素濃度を推定
する半導体基板の表面酸素濃度測定方法。
1. A semiconductor substrate is indented with a load of 1 to 2000 g and then heat treated at 600 ° C. to 1000 ° C. for 1 to 60 minutes to perform defect selective etching of 0.1 μm to 0.1 μm.
The surface oxygen concentration of the semiconductor substrate is estimated by demonstrating the dislocation generated during the heat treatment by applying 30 μm, measuring the displacement distance of the dislocation from the indentation, and estimating the surface oxygen concentration of the substrate from the preset relationship between the oxygen concentration and the dislocation displacement distance. Concentration measurement method.
JP2325096A 1996-01-16 1996-01-16 Method for measuring surface oxygen concentration of semiconductor substrate Pending JPH09199558A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2325096A JPH09199558A (en) 1996-01-16 1996-01-16 Method for measuring surface oxygen concentration of semiconductor substrate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2325096A JPH09199558A (en) 1996-01-16 1996-01-16 Method for measuring surface oxygen concentration of semiconductor substrate

Publications (1)

Publication Number Publication Date
JPH09199558A true JPH09199558A (en) 1997-07-31

Family

ID=12105360

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2325096A Pending JPH09199558A (en) 1996-01-16 1996-01-16 Method for measuring surface oxygen concentration of semiconductor substrate

Country Status (1)

Country Link
JP (1) JPH09199558A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT515421A4 (en) * 2014-02-25 2015-09-15 Holcim Technology Ltd Apparatus for preheating cement raw meal for cement clinker production
JP2016111044A (en) * 2014-12-02 2016-06-20 信越半導体株式会社 Evaluation method for silicon wafer

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT515421A4 (en) * 2014-02-25 2015-09-15 Holcim Technology Ltd Apparatus for preheating cement raw meal for cement clinker production
JP2016111044A (en) * 2014-12-02 2016-06-20 信越半導体株式会社 Evaluation method for silicon wafer

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