JPH0342501B2 - - Google Patents
Info
- Publication number
- JPH0342501B2 JPH0342501B2 JP59079466A JP7946684A JPH0342501B2 JP H0342501 B2 JPH0342501 B2 JP H0342501B2 JP 59079466 A JP59079466 A JP 59079466A JP 7946684 A JP7946684 A JP 7946684A JP H0342501 B2 JPH0342501 B2 JP H0342501B2
- Authority
- JP
- Japan
- Prior art keywords
- sio
- film
- defects
- silicon substrate
- pressure
- 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 - Lifetime
Links
- 230000007547 defect Effects 0.000 claims description 34
- 239000010408 film Substances 0.000 claims description 29
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 17
- 229910052710 silicon Inorganic materials 0.000 claims description 17
- 239000010703 silicon Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 16
- 239000000758 substrate Substances 0.000 claims description 12
- 239000010409 thin film Substances 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 31
- 238000000137 annealing Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000007781 pre-processing Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 241000270708 Testudinidae Species 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052743 krypton Inorganic materials 0.000 description 1
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052704 radon Inorganic materials 0.000 description 1
- SYUHGPGVQRZVTB-UHFFFAOYSA-N radon atom Chemical compound [Rn] SYUHGPGVQRZVTB-UHFFFAOYSA-N 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
Description
【発明の詳細な説明】
(1) 発明の技術分野
本発明はシリコン基板上に形成された絶縁薄膜
の欠陥検出方法、詳しくは薄膜形成後にH2O，
O2の低分圧下で熱処理を行い薄膜に存在する欠
陥を顕在化させる方法に関する。[Detailed Description of the Invention] (1) Technical Field of the Invention The present invention relates to a method for detecting defects in an insulating thin film formed on a silicon substrate.
This invention relates to a method of exposing defects existing in a thin film by performing heat treatment under a low partial pressure of O 2 .
(2) 技術の背景
半導体装置の製造工程において、シリコン基板
上に二酸化シリコン（SiO2）の薄膜を形成する
ことが行われる。SiO2膜の形成にはシリコン基
板が配置された1000℃程度の温度の炉中に乾酸素
（dry oxygen）を供給し、Si＋O2→SiO2なる反
応を起させ、または同じ炉中に水蒸気を送りSi＋
2H2O→SiO2＋2H2で示される反応を発生させて、
SiO2の膜を形成する。(2) Background of the Technology In the manufacturing process of semiconductor devices, a thin film of silicon dioxide (SiO 2 ) is formed on a silicon substrate. To form the SiO 2 film, dry oxygen is supplied into a furnace at a temperature of about 1000°C in which a silicon substrate is placed, causing a reaction of Si + O 2 → SiO 2 , or water vapor is introduced into the same furnace. Feed Si+
By generating the reaction shown as 2H 2 O→SiO 2 +2H 2 ,
Form a film of SiO 2 .
(3) 従来技術と問題点
集積回路の集積度を高める目的で、最近は各素
子を小に形成すだけでなくSiO2膜も薄く形成さ
れる傾向にある。従来は1000Å程度の膜厚であつ
たSiO2膜は300Å程度に形成されるようになり、
近い将来それは100Å程度にまで薄くされるであ
ろうと予測されている。(3) Prior art and problems In order to increase the degree of integration of integrated circuits, there is a recent trend not only to make each element smaller but also to make the SiO 2 film thinner. The SiO 2 film, which used to be about 1000 Å thick, is now formed to about 300 Å thick.
It is predicted that in the near future it will be thinned to around 100 Å.
このようなSiO2薄膜についてはその耐圧性が
重要であるが、耐圧劣化の主な原因は薄膜に存在
する欠陥である。良質な耐圧性のよいSiO2膜を
作るについて、SiO2の薄膜に欠陥が存在するか
否かを検出するために第１図の断面図に示される
方式が用いられる。第１図において、１はシリコ
ン基板、２はその上に形成されたSiO2膜を示し、
このSiO2膜２に欠陥があるか否かを検査するに
はその上にアルミニウム（Al）電極３を形成し、
シリコン基板１とAl電極３を電流計４、電圧源
５を介して接続する。SiO2膜２に欠陥があれば
その部分での耐圧が低いから、電流計４の読みを
見ていると欠陥の有無が検知される。しかしかか
る検出方法はAl電極の形成およびそれとシリコ
ン基板との接続に時間を要するので、目視によつ
て欠陥の有無が容易に検出される方法が要望され
ている。 The pressure resistance of such a SiO 2 thin film is important, but the main cause of voltage resistance deterioration is defects existing in the thin film. In order to produce a high-quality SiO 2 film with good pressure resistance, the method shown in the cross-sectional view of FIG. 1 is used to detect whether or not defects exist in the SiO 2 thin film. In FIG. 1, 1 indicates a silicon substrate, 2 indicates a SiO 2 film formed thereon,
To inspect whether or not this SiO 2 film 2 has defects, an aluminum (Al) electrode 3 is formed on it,
A silicon substrate 1 and an Al electrode 3 are connected via an ammeter 4 and a voltage source 5. If there is a defect in the SiO 2 film 2, the breakdown voltage at that part is low, so the presence or absence of a defect can be detected by checking the reading on the ammeter 4. However, since this detection method requires time to form the Al electrode and connect it to the silicon substrate, there is a need for a method that can easily detect the presence or absence of defects visually.
なお前記した欠陥は、フオトプロセスや洗浄工
程で導入された微細なゴミや金属粒子、金属イオ
ンなどによるものであることが多い。そこで半導
体装置の製造工程においては定期にシリコン基板
上の薄膜につちて欠陥の有無を検査し、欠陥があ
ればその原因を探求して適切な処理をとることが
できるよう欠陥の容易な検出方法が要望されてい
る。 Note that the above-mentioned defects are often caused by fine dust, metal particles, metal ions, etc. introduced during the photo process or cleaning process. Therefore, in the manufacturing process of semiconductor devices, thin films on silicon substrates are regularly inspected for defects, and if defects are found, they can be easily detected so that the cause can be investigated and appropriate treatment can be taken. A method is required.
(4) 発明の目的
本発明は上記従来の問題に鑑み、シリコン基板
上に形成された絶縁膜に欠陥が存在するか否か
を、顕微鏡を用いる目視により容易に検出するこ
とを可能ならしめる欠陥検出方法を提供すること
を目的とする。(4) Purpose of the Invention In view of the above conventional problems, the present invention provides a defect that makes it possible to easily detect whether or not a defect exists in an insulating film formed on a silicon substrate by visual observation using a microscope. The purpose is to provide a detection method.
(5) 発明の構成
そしてこの目的は本発明によれば、シリコン基
板上に絶縁膜を形成した後に新たに該絶縁膜が成
長しない程度の酸素圧または水蒸気圧を有するガ
ス中または真空中で650〜1250℃の温度で熱処理
を行い前記膜に存在した欠陥を顕在化することを
特徴とする薄膜の欠陥検出方法を提供することに
よつて達成される。(5) Structure of the Invention According to the present invention, this object is to form an insulating film on a silicon substrate and then conduct a 650°C process in a gas or vacuum having an oxygen pressure or water vapor pressure that is such that no new insulating film grows. This is achieved by providing a method for detecting defects in a thin film, which is characterized by performing heat treatment at a temperature of ~1250°C to expose defects existing in the film.
(6) 発明の実施例
以下本発明実施例を図面によつて詳説する。第
２図ａを参照すると、シリコン基板１１上に前記
した方法（Si＋O2→SiO2またはSi＋2H2O→SiO2
＋2H2）のいずれかでSiO2膜１２が形成され、そ
してこのSiO2膜１２に欠陥１３が形成されてい
る。かかる欠陥は通常の光学的手段では、効率良
く検出することが出来ないものが多く、たとえ出
来るものでも効率良く検出することは困難であ
る。本発明の方法においてはH2OまたはO2の低
分圧下で、すなわち、H2OまたはO2のほとんど
存在しないアルゴン（Ar）雰囲気中で900℃〜
1200℃の温度の下で熱処理（アニール）を行う。
この時、シリコン基板１１とSiO2膜１２の界面
では、新たなSiO2膜の成長がほとんどないため、
Si＋SiO22SiO ……
の反応が生じているが、SiO2膜に欠陥がない場
合、は平衡状態を保ち、膜厚等に変化は見られ
ない。しかるに、SiO2膜にピンホールや金属イ
オンの局在等の欠陥が存在する場合、欠陥が界面
からSiO2膜表面へのシヨートパスとして働き、
蒸気圧の高いSiOは雰囲気中へ拡散していく。す
ると、反応の平衡は、右方向にずれ、その結
果、欠陥周辺のシリコンおよびSiO2が反応・消
費され、第２図ｂの断面図に示されるようなエツ
チピツト１４が形成される。(6) Embodiments of the invention Examples of the invention will be described in detail below with reference to the drawings. Referring to FIG. 2a, the above method (Si+O 2 →SiO 2 or Si+2H 2 O → SiO 2
+2H 2 ), and defects 13 are formed in this SiO 2 film 12. Many of these defects cannot be detected efficiently by ordinary optical means, and even if they can be detected, it is difficult to detect them efficiently. In the method of the present invention, 900 ° C to
Heat treatment (annealing) is performed at a temperature of 1200℃.
At this time, since there is almost no new SiO 2 film growth at the interface between the silicon substrate 11 and the SiO 2 film 12, a reaction of Si + SiO 2 2SiO occurs, but if there are no defects in the SiO 2 film, An equilibrium state is maintained, and no change is observed in the film thickness, etc. However, if defects such as pinholes or localized metal ions exist in the SiO 2 film, the defects act as short paths from the interface to the SiO 2 film surface,
SiO, which has a high vapor pressure, diffuses into the atmosphere. Then, the reaction equilibrium shifts to the right, and as a result, silicon and SiO 2 around the defect are reacted and consumed, forming an etch pit 14 as shown in the cross-sectional view of FIG. 2b.
この反応によるSiO2の消費で、前述なシヨー
トパスは、更に拡大されるため、熱処理時間が長
い程エツチピツトの径は大きくなり、ついには顕
微鏡観察が可能な大きさになる。 The consumption of SiO 2 by this reaction further expands the shot path, so the longer the heat treatment time, the larger the diameter of the etch pit becomes, eventually reaching a size that allows microscopic observation.
本発明によるSiO2薄膜の欠陥検出の具体例は
次の表に示される如きものであつた。 A specific example of detecting defects in a SiO 2 thin film according to the present invention is as shown in the following table.
■■■ 亀の甲 ［0004］ ■■■
最初の例を見ると、前処理におけるなんらかの
原因で欠陥が形成されていて、それが本発明方法
で容易に単位面積当り150個あつたことが検出さ
れ、前処理が不良であつたことを示す。■■■ Tortoise shell [0004] ■■■ Looking at the first example, defects were formed due to some cause in the pretreatment, and the method of the present invention easily detected that there were 150 defects per unit area. Indicates that the pretreatment was poor.
次の前処理無しの例は、ピツトが数個しか検出
されていないから、それは前処理以外のなんらか
のものによる欠陥であることを示す。 In the following example without preprocessing, only a few pits are detected, indicating that the defect is caused by something other than preprocessing.
最後の例は、前処理を行つたにもかかわらず、
ピツトが検出されなかつたことから、酸化雰囲気
中に混入したHClにより欠陥形成が妨げられたこ
とが推定出来る。 In the last example, despite preprocessing,
Since no pits were detected, it can be assumed that HCl mixed into the oxidizing atmosphere prevented defect formation.
前記したH2OまたはO2の低分圧について説明
する。第３図はH2Oによるシリコンの酸化につ
いて圧力と温度との関係を示す線図で、例えば
900℃においては圧力が10-4Torr以下であれば前
記したSiとSiO2のエツチングが発生することを
示す（Phys.Stat.Sol.(a)17104（1973））。図におい
て、Ａは酸化膜領域（Oxidized Surface
Region）、Ｂはきれいな表面領域（Clean
Surface Region）、破線ＣはSi＋SiO2上のSiOの
蒸気圧、破線Ｄは蒸気圧を示す。 The low partial pressure of H 2 O or O 2 mentioned above will be explained. Figure 3 is a diagram showing the relationship between pressure and temperature for the oxidation of silicon by H 2 O.
At 900°C, etching of Si and SiO 2 described above occurs if the pressure is below 10 -4 Torr (Phys. Stat. Sol. (a) 17104 (1973)). In the figure, A is an oxide film region (Oxidized Surface
Region), B is the clean surface region (Clean
The broken line C shows the vapor pressure of SiO on Si+ SiO2 , and the broken line D shows the vapor pressure.
また第４図では、例えば900℃でのシリコン酸
化において、圧力が10-5mmHg.以上あれば前記し
たエツチングが発生することを示す（JAP
Vol.33、2089、1962、Oxidation and Reduction
of silicon，p.2091）。なお図において、Ａ，Ｂ，
Ｃ，Ｄは第３図の場合と同じ場合を表す。 Figure 4 also shows that in silicon oxidation at 900°C, for example, if the pressure is 10 -5 mmHg. or more, the above-mentioned etching occurs (JAP
Vol.33, 2089, 1962, Oxidation and Reduction
of silicon, p.2091). In the figure, A, B,
C and D represent the same cases as in FIG.
そして本発明の方法においては、H2O，O2の
蒸気の如き低分圧状態を作り出すために不活性ガ
ス雰囲気でアニールを行うものである。 In the method of the present invention, annealing is performed in an inert gas atmosphere to create a low partial pressure state such as H 2 O, O 2 vapor.
上記した如く本発明の方法によれば、顕微鏡で
SiO2膜の欠陥を検出できるだけでなく、欠陥の
原因の所在についての手がかりが与えられる。な
お欠陥顕在化のためのアニールに用いるガスは
Arに限定されるものではなく、ヘリウム（He）、
ネオオン（Ne）、キセノン（Xe）、ラドン
（Rn）、クリプトン（Kr）も用いうるし、または
真空中アニールであつてもよい。 As described above, according to the method of the present invention, it is possible to
Not only can it detect defects in the SiO 2 film, but it can also provide clues as to the source of the defects. The gas used for annealing to expose defects is
Not limited to Ar, helium (He),
Neon (Ne), xenon (Xe), radon (Rn), and krypton (Kr) may also be used, or vacuum annealing may be used.
なお上記はSiO2膜を例に説明したが、本発明
の適用範囲はその場合に限定されるものでなく、
シリコン窒化膜（Si3N4膜）の場合にも及ぶもの
である。 Note that although the above explanation was given using an SiO 2 film as an example, the scope of application of the present invention is not limited to that case.
This also applies to silicon nitride films (Si 3 N 4 films).
(7) 発明の効果
以上詳細に説明した如く本発明の方法によれ
ば、シリコン基板上に形成されたSiO2または
Si3N4薄膜に存在する欠陥が、アルゴンアニール
によつて顕在化し、顕微鏡による目視で検出可能
となり、半導体装置の製造工程の管理にきわめて
有効である。(7) Effects of the invention As explained in detail above, according to the method of the present invention, SiO 2 or
Defects present in the Si 3 N 4 thin film are exposed by argon annealing and can be visually detected using a microscope, which is extremely effective in controlling the manufacturing process of semiconductor devices.
第１図は従来のSiO2膜の欠陥検出方法を示す
図、第２図は本発明の実施例の断面図、第３図と
第４図はシリコン酸化における温度と圧力の関係
を示す線図である。
１１……シリコン基板、１２……SiO2膜、１
３……欠陥、１４……ピツト。
Fig. 1 is a diagram showing a conventional method for detecting defects in SiO 2 film, Fig. 2 is a cross-sectional view of an embodiment of the present invention, and Figs. 3 and 4 are diagrams showing the relationship between temperature and pressure in silicon oxidation. It is. 11...Silicon substrate, 12...SiO 2 film, 1
3...Defect, 14...Pits.
Claims (1)
に該絶縁膜が成長しない程度の酸素分圧または水
蒸気圧を有するガス中または真空中で650〜1250
℃の温度で熱処理を行い前記膜に存在した欠陥を
顕在化することを特徴とする薄膜の欠陥検出方
法。1 650 to 1250 in a gas or vacuum having an oxygen partial pressure or water vapor pressure that does not allow new growth of the insulating film after forming the insulating film on the silicon substrate
1. A method for detecting defects in a thin film, which comprises performing heat treatment at a temperature of 0.degree. C. to expose defects existing in the film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7946684A JPS60224239A (en) | 1984-04-20 | 1984-04-20 | Defect detecting method of thin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7946684A JPS60224239A (en) | 1984-04-20 | 1984-04-20 | Defect detecting method of thin film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60224239A JPS60224239A (en) | 1985-11-08 |
| JPH0342501B2 true JPH0342501B2 (en) | 1991-06-27 |
Family
ID=13690657
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7946684A Granted JPS60224239A (en) | 1984-04-20 | 1984-04-20 | Defect detecting method of thin film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60224239A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0196804B1 (en) * | 1985-03-11 | 1991-01-23 | Nippon Telegraph And Telephone Corporation | Method and apparatus for testing integrated electronic device |
| JP2006203089A (en) * | 2005-01-24 | 2006-08-03 | Shin Etsu Handotai Co Ltd | Evaluation method of silicon wafer |
| JP5729098B2 (en) * | 2011-04-07 | 2015-06-03 | 信越半導体株式会社 | Evaluation method of silicon single crystal wafer |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5618437A (en) * | 1979-07-25 | 1981-02-21 | Fujitsu Ltd | Inspection method for semiconductor crystal |
| JPS5772340A (en) * | 1980-10-23 | 1982-05-06 | Toshiba Corp | Quality evaluating method for single crystal silicon wafer |
| JPS6017926A (en) * | 1983-07-08 | 1985-01-29 | Matsushita Electronics Corp | Crystal defect detecting method of sapphire |
-
1984
- 1984-04-20 JP JP7946684A patent/JPS60224239A/en active Granted
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5618437A (en) * | 1979-07-25 | 1981-02-21 | Fujitsu Ltd | Inspection method for semiconductor crystal |
| JPS5772340A (en) * | 1980-10-23 | 1982-05-06 | Toshiba Corp | Quality evaluating method for single crystal silicon wafer |
| JPS6017926A (en) * | 1983-07-08 | 1985-01-29 | Matsushita Electronics Corp | Crystal defect detecting method of sapphire |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60224239A (en) | 1985-11-08 |
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