JPH0445531A - Etching solution for silicon oxide film - Google Patents

Etching solution for silicon oxide film

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Publication number
JPH0445531A
JPH0445531A JP15469890A JP15469890A JPH0445531A JP H0445531 A JPH0445531 A JP H0445531A JP 15469890 A JP15469890 A JP 15469890A JP 15469890 A JP15469890 A JP 15469890A JP H0445531 A JPH0445531 A JP H0445531A
Authority
JP
Japan
Prior art keywords
etching solution
concentration
bhf
oxide film
hydrofluoric acid
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.)
Granted
Application number
JP15469890A
Other languages
Japanese (ja)
Other versions
JP3109083B2 (en
Inventor
Kaori Watanabe
かおり 渡邊
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.)
NEC Corp
Original Assignee
NEC Corp
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Filing date
Publication date
Application filed by NEC Corp filed Critical NEC Corp
Priority to JP02154698A priority Critical patent/JP3109083B2/en
Publication of JPH0445531A publication Critical patent/JPH0445531A/en
Application granted granted Critical
Publication of JP3109083B2 publication Critical patent/JP3109083B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Abstract

PURPOSE:To manufacture a high quality and high yield semiconductor device by adding 0.5 to 15wt.% H2O2 in a buffer hydroxide acid (BHF) which includes 0.1 to 10wt.% hydroxide acid in terms of an etching solution. CONSTITUTION:An etching solution (BFH/H2O2) (HF: 6%, NF4F: 30%, H2O2: 1%), which contains hydrogen peroxide (H2O2) is adopted in the BHF, which contains hydrofluoric acid as an etching solution. In terms of the BFH/H2O2, there is no uptake of Cu. In any case of metal impurities, the uptake fails to exceed the detection limit. Within the range where the concentration of HF is 0.1 to 10wt.% and the concentration of H2O2 is 0.5 to 15wt.%, there is no uptake of impurities. When the HF and H2O2 concentration fails to exceed the aforesaid range, the controllability required for mixing a solution is deteriorated. On the other hand, when the concentration exceeds the above range, economic performance will be deteriorated. Therefore, the aforesaid range is proper to the concentration of HF and H2O2 as well.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明はシリコン酸化膜のエツチング液に関し、特に金
属不純物の取り込みが少なく、且つ金属不純物の除去能
力に優れている上に、微粒子の付着が極めて少ないエツ
チング液に関する。
[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to an etching solution for silicon oxide films, and in particular, it has a low incorporation of metal impurities, an excellent ability to remove metal impurities, and an etching solution that prevents the adhesion of fine particles. Regarding extremely small amount of etching solution.

[従来の技術] 従来、この種のシリコン酸化膜のエツチング液は、弗酸
、弗化アンモニウム及び純水のみを成分とする緩衝弗酸
溶液(BHF)を使用している。
[Prior Art] Conventionally, this type of etching solution for silicon oxide films uses a buffered hydrofluoric acid solution (BHF) containing only hydrofluoric acid, ammonium fluoride, and pure water.

[発明が解決しようとする課題] 上述した従来のエツチング液では、BHF中でシリコン
酸化膜を浸漬処理することによって、シリコン単結晶面
が露出する。この露出したシリコン単結晶面は極めて活
性であり、薬液中等からの微粒子や金属不純物が付着し
やすくなる。
[Problems to be Solved by the Invention] In the conventional etching solution described above, the silicon single crystal plane is exposed by immersing the silicon oxide film in BHF. This exposed silicon single crystal surface is extremely active, making it easy for fine particles and metal impurities from chemical solutions to adhere to it.

近年、半導体素子の微細化が進むにつれて、微粒子や金
属不純物が半導体素子の物性あるいは歩留りに与える影
響が益々重大になってきている。
In recent years, as the miniaturization of semiconductor devices has progressed, the influence of fine particles and metal impurities on the physical properties and yield of semiconductor devices has become increasingly important.

一般にデバイス特性に悪影響を与える微粒子の大きさは
設計ルールの約10分の1と言われており、4 MDR
AMでは0,111m以下の微粒子が半導体製造上問題
となっている。
Generally, the size of particles that adversely affect device characteristics is said to be about one-tenth of the design rule, and 4 MDR
In AM, fine particles of 0.111 m or less are a problem in semiconductor manufacturing.

このシリコン基板上の微粒子が与える影響としては、例
えばリソグラフィ工程においてはパターン欠陥を引き起
こす原因となる。また、拡散・酸化工程においては、異
常拡散や酸化膜厚異常の原因となったりする。特に集積
度の増大に伴い、ゲート酸化膜や容量絶縁膜が薄くなる
につれて半導体基板上の微粒子が原因となり、ピンホー
ルと呼ばれる微小な欠陥が酸化膜・絶縁膜に形成され、
絶縁耐圧を著しく劣化させる傾向が大いにある。
For example, the fine particles on the silicon substrate cause pattern defects in a lithography process. Furthermore, in the diffusion/oxidation process, it may cause abnormal diffusion or abnormal oxide film thickness. In particular, as the degree of integration increases, gate oxide films and capacitor insulating films become thinner, and fine particles on the semiconductor substrate cause minute defects called pinholes to form in the oxide and insulating films.
There is a strong tendency to significantly degrade dielectric strength.

このため、半導体素子の特性を劣化させ、歩留りの低下
および品質の低下を招くという問題があった。
Therefore, there has been a problem in that the characteristics of the semiconductor element are deteriorated, leading to a decrease in yield and quality.

ところで、B)IFあるいは希弗酸(DHF)は、自然
酸化膜の除去が行えることから、Fe、 kQ等の金属
不純物の取り込みは起こりにくくなる。しかしながら、
BHFあるいはDi−IFで処理を行うと、シリコン結
晶面が露出するため、薬液中あるいはシリコン基板上に
シリコンよりもイオン化傾向の小さな金属(例えばCu
、 Ag等)が含まれていると、それらの金属がシリコ
ン基板表面に付着・析出するという問題がある。
By the way, since B) IF or dilute hydrofluoric acid (DHF) can remove a natural oxide film, the incorporation of metal impurities such as Fe and kQ becomes less likely to occur. however,
When processing with BHF or Di-IF, the silicon crystal plane is exposed, so metals that have a smaller ionization tendency than silicon (for example, Cu) are placed in the chemical solution or on the silicon substrate.
, Ag, etc.), there is a problem that these metals adhere and precipitate on the silicon substrate surface.

以上述べたように、従来のシリコン酸化膜のエツチング
液は、薬液中あるいはシリコン基板がCu。
As mentioned above, conventional etching solutions for silicon oxide films are used when the chemical solution or the silicon substrate is Cu.

Ag等に汚染された場合これらの金属不純物の析出が起
こり、さらに微粒子がシリコン基板に付着しやすくなる
という欠点を持ち合わせていた。
If it is contaminated with Ag or the like, these metal impurities will precipitate, and furthermore, it has the disadvantage that fine particles tend to adhere to the silicon substrate.

本発明の目的は、活性なシリコン単結晶面の露出を阻止
することにより、前記欠点を解決したシリコン酸化膜の
エツチング液を提供することにある。
SUMMARY OF THE INVENTION An object of the present invention is to provide a silicon oxide film etching solution which solves the above-mentioned drawbacks by preventing the exposure of active silicon single crystal planes.

〔課題を解決するための手段〕[Means to solve the problem]

前記目的を達成するため、本発明に係るシリコン酸化膜
のエツチング液においては、緩衝弗酸溶液中にシリコン
基板を浸漬し、シリコン酸化膜をエツチング処理するエ
ツチング液であって、弗酸を含む緩衝弗酸溶液中に、過
酸化水素を含むものであり、また、前記緩衝弗酸溶液中
に含まれる弗酸の濃度は、0.1乃至10重量%の範囲
であり、前記過酸化水素の濃度は、0.5乃至15重量
%の範囲である。
In order to achieve the above object, an etching solution for a silicon oxide film according to the present invention is an etching solution for etching a silicon oxide film by immersing a silicon substrate in a buffered hydrofluoric acid solution. Hydrofluoric acid solution contains hydrogen peroxide, and the concentration of hydrofluoric acid contained in the buffered hydrofluoric acid solution is in the range of 0.1 to 10% by weight, and the concentration of hydrogen peroxide is in the range of 0.1 to 10% by weight. ranges from 0.5 to 15% by weight.

[実施例] 次に本発明について図面を参照して説明する。[Example] Next, the present invention will be explained with reference to the drawings.

(実施例1) 第1図は本発明及び従来のエツチング液中からの金属不
純物の取り込み量を評価した結果を示す図であり、第1
図(a)、 (b)はそれぞれ原子吸光分析及び少数キ
ャリアの再結合ライフタイムの測定結果を示す図である
(Example 1) FIG. 1 is a diagram showing the results of evaluating the amount of metal impurities taken into the etching solution of the present invention and the conventional etching solution.
Figures (a) and (b) are diagrams showing the results of atomic absorption spectrometry and measurement of the recombination lifetime of minority carriers, respectively.

あらかじめDHF処理によって清浄な面を露出さセfニ
ジI)コ>基板をAQ、 Fe、 Cr、 Ni、 C
uを各lppm添加したエツチング液中で10分間処理
した。処理後のシリコン基板は純水によって10分間リ
ンスを行った後、遠心乾燥法により乾燥した。乾燥後、
シリコン基板上に残留している金属不純物を原子吸光分
析及び少数キャリア再結合ライフタイム測定によって評
価した。少数キャリア再結合ライフタイム測定は、処理
後のシリコン基板に950℃の酸化性雰囲気中で熱処理
を施した後、μ波反射式非接触ライフタイム測定器にて
測定した。従来のエツチング液として、緩衝弗酸溶液(
B)IF)(HF : 6%、 NH4F : 30%
)を用い、本発明のエツチング液として弗酸を含む緩衝
弗酸溶液(BHF)中に、過酸化水素()1202)を
含むエツチング液(BHF/H2O2) (HF:6%
、 NH4F : 30%、 )(202: 1%)を
用いた。
The clean surface is exposed in advance by DHF treatment.
The samples were treated for 10 minutes in an etching solution containing 1ppm of U. The silicon substrate after the treatment was rinsed with pure water for 10 minutes, and then dried by a centrifugal drying method. After drying,
Metal impurities remaining on the silicon substrate were evaluated by atomic absorption spectrometry and minority carrier recombination lifetime measurements. Minority carrier recombination lifetime measurement was performed using a μ wave reflection type non-contact lifetime measurement device after heat-treating the silicon substrate after the treatment in an oxidizing atmosphere at 950°C. Buffered hydrofluoric acid solution (
B) IF) (HF: 6%, NH4F: 30%
), the etching solution of the present invention is an etching solution (BHF/H2O2) containing hydrogen peroxide (1202) in a buffered hydrofluoric acid solution (BHF) containing hydrofluoric acid (HF: 6%
, NH4F: 30%, ) (202: 1%) were used.

従来のBHFでは、Cuが多量に取り込まれている。Conventional BHF incorporates a large amount of Cu.

これに対して本発明のBHF/)(202では、従来B
HFで問題であったCuの取り込みがなく、いずれの金
属不純物に対しても、取り込み量は検出限界以下であっ
た。
On the other hand, in the BHF/) (202 of the present invention, the conventional BHF/) (202)
There was no uptake of Cu, which was a problem with HF, and the amount of uptake was below the detection limit for any metal impurity.

第1図(b)のライフタイム測定の結果は、この原子吸
光の結果をよく対応しており、Cuを多量に取り込んで
いるB)IPでは特にN型サブのライフタイムの劣化が
著しいのに対して、BHF/H2O2では、清浄基板の
ものと同程度てあり、BHF/H2O2処理のシリコン
基板表面が極めて清浄であることを示している。
The lifetime measurement results shown in Figure 1(b) correspond well to the atomic absorption results, and in B) IP that incorporates a large amount of Cu, the lifetime deterioration of the N-type sub is particularly significant. On the other hand, in the case of BHF/H2O2, the level is comparable to that of a clean substrate, indicating that the surface of the silicon substrate treated with BHF/H2O2 is extremely clean.

第2図は本発明及び従来のエツチング液による金属不純
物に対する除去効果を比較したものであり、第2図Ca
b、 (b)はそれぞれ原子吸光分析及び少数キャリア
の再結合ライフタイム測定の結果である。
Figure 2 compares the removal effects of metal impurities by the etching solution of the present invention and the conventional etching solution.
b and (b) are the results of atomic absorption spectrometry and minority carrier recombination lifetime measurement, respectively.

清浄な半導体基板をAQ、 Fa、 Cr、 Ni、 
Cuによって定量汚染させ、定量汚染後、従来法のBH
Fと本発明のBHF/H2O2によって処理を行った。
A clean semiconductor substrate is coated with AQ, Fa, Cr, Ni,
Quantitative contamination with Cu, and after quantitative contamination, conventional method BH
The treatment was carried out with F and BHF/H2O2 of the present invention.

処理時間は10分、純水によるリンス時間は10分であ
った。
The treatment time was 10 minutes, and the rinsing time with pure water was 10 minutes.

汚染量はAQ、 Fe、 Cr、 Niに対しては表面
濃度が1013原子/cn!、Cuに対しては1Q12
原子/CTI!である。
The surface concentration of AQ, Fe, Cr, and Ni is 1013 atoms/cn! , 1Q12 for Cu
Atomic/CTI! It is.

従来のB)IPはCuに対する除去効果が低い。これに
対して本発明のBHF/H2O2では、いずれの金属も
検出限界以下であり、極めて除去効果が高いことが分か
る。
Conventional B) IP has a low removal effect on Cu. On the other hand, in the case of BHF/H2O2 of the present invention, all metals are below the detection limit, indicating that the removal effect is extremely high.

第3図は本発明のBHF/H2O2におけるHF濃度と
H2O2濃度を変化させた場合のエツチング液からの金
属不純物の取り込みを評価した結果である。Fe。
FIG. 3 shows the results of evaluating the uptake of metal impurities from the etching solution when the HF concentration and H2O2 concentration in BHF/H2O2 of the present invention were varied. Fe.

Cuを各lppm添加したエツチング液中でシリコン基
板を10分間処理した後純水によって10分間リンスを
行った。リンス後、遠心乾燥法により乾燥した。評価は
少数キャリアの再結合ライフタイム測定により行った。
The silicon substrate was treated for 10 minutes in an etching solution containing 1 ppm of Cu, and then rinsed with pure water for 10 minutes. After rinsing, it was dried by a centrifugal drying method. The evaluation was performed by measuring the recombination lifetime of minority carriers.

)IF(弗酸)濃度が0.1乃至10重量%及び)+2
02(過酸化水素)濃度が0.5乃至15重量%の範囲
内で不純物の取り込みはなく、ライフタイムは清浄なウ
ェーハの場合と同じであった。HF濃度、H2O2濃度
がこれ以下の場合には、液調合時における制御性が悪く
なる。一方、濃度がこれ以上高くなれば、経済性に劣る
。従って、HF?1度、H2O2濃度としてはこの範囲
が適当である。
) IF (fluoric acid) concentration is 0.1 to 10% by weight and ) +2
When the 02 (hydrogen peroxide) concentration ranged from 0.5 to 15% by weight, no impurities were taken in, and the lifetime was the same as for a clean wafer. If the HF concentration and H2O2 concentration are lower than these, the controllability during liquid preparation will be poor. On the other hand, if the concentration is higher than this, it will be less economical. Therefore, HF? This range is appropriate for the H2O2 concentration.

第4図は本発明のシリコン基板上に付着する微粒子の測
定結果を示す。
FIG. 4 shows the measurement results of fine particles adhering to the silicon substrate of the present invention.

シリコン基板をエツチング液中で10分間処理した後、
純水にて10分間リンスを行った。リンス後、遠心乾燥
法によって乾燥し、乾燥後、シリコン基板表面上に付着
した微粒子をレーザー散乱式微粒子カウンターにて計数
した。図中の値は、各エツチング液での処理前後の差を
微粒子付着数として示している。また、リファレンスと
して純水リンスのみの水準を用いた。
After processing the silicon substrate in an etching solution for 10 minutes,
Rinsing was performed with pure water for 10 minutes. After rinsing, it was dried by a centrifugal drying method, and after drying, the particles adhering to the surface of the silicon substrate were counted using a laser scattering particle counter. The values in the figure indicate the difference before and after treatment with each etching solution as the number of attached fine particles. In addition, the level of only pure water rinsing was used as a reference.

従来法のBHFにおいてはバラツキが大きく、100個
程度の微粒子が付着している。これに対して本発明のB
l(F/H2O2では、Bl(Fと比較して微粒子の付
着が極めて少なくなっており、リファレンスとほぼ同程
度であ、る。また、液の組成を変えてもバラツキが少な
く、微粒子の付着数は非常に安定している。
In the conventional BHF method, there is a large variation, and about 100 fine particles are attached. In contrast, B of the present invention
With l(F/H2O2, the adhesion of fine particles is extremely reduced compared to Bl(F), and is almost the same as the reference.Also, even if the liquid composition is changed, there is little variation, and the adhesion of fine particles is The numbers are very stable.

このように、BHF / H202においては、従来1
3+(Fで問題となっていた微粒子の付着も抑えること
ができる。
In this way, in BHF/H202, conventional 1
The adhesion of fine particles, which was a problem with 3+ (F), can also be suppressed.

(実施例2) 第5図は本発明の実施例2を示すもので、本発明のBH
F/H2O2におけるH2O2濃度を変化させたときの
エッチレートの測定結果を示す図である。
(Example 2) FIG. 5 shows Example 2 of the present invention.
FIG. 3 is a diagram showing the measurement results of etch rate when changing the H2O2 concentration in F/H2O2.

あらかじめDHF処理によって清浄な面を露出させたシ
リコン基板表面に熱酸化膜を6000人形成し、従来の
BHFと、本発明のBHF/H2O2とで所定時間エツ
チングを行った。
A thermal oxide film was formed by 6000 people on the surface of a silicon substrate whose clean surface had been exposed by DHF treatment in advance, and etching was performed for a predetermined time using conventional BHF and BHF/H2O2 of the present invention.

本発明のBHF/H2O2は、従来のBHFとほぼ同様
のエッチレートが得られた。これは、H2O2濃度を変
化させても変わらなかった。従って、本発明のエツチン
グ液BHF/H2O2は、従来のBHFと同じ処理方法
で使用できるという利点を持っている。
With BHF/H2O2 of the present invention, an etch rate almost the same as that of conventional BHF was obtained. This did not change even if the H2O2 concentration was changed. Therefore, the etching solution BHF/H2O2 of the present invention has the advantage that it can be used in the same processing method as conventional BHF.

[発明の効果] 以上説明したように本発明のエツチング液は、0.1乃
至10重量%の弗酸を含むBHF中に、0.5乃至15
重量%のH2O2を添加することにより、シリコン酸化
膜のエツチングを行うと同時に、新たに清浄な薄い自然
酸化膜が形成されるために、活性なシリコン単結晶面が
露出することがない。この新たに形成される清浄な薄い
自然酸化膜は、数Å以下と非常に薄いため、次の工程に
影響はない。そのため、薬液中からの金属不純物の取り
込みが少なく、且つ金属不純物の除去能力に優れている
上に、微粒子の付着が極めて少ないエツチング液となる
[Effects of the Invention] As explained above, the etching solution of the present invention contains 0.5 to 15% by weight of BHF containing 0.1 to 10% by weight of hydrofluoric acid.
By adding % by weight of H2O2, a new clean thin natural oxide film is formed at the same time as the silicon oxide film is etched, so that active silicon single crystal planes are not exposed. This newly formed, clean, thin native oxide film is very thin, several angstroms or less, so it does not affect the next process. Therefore, the etching solution is one in which less metal impurities are taken in from the chemical solution, which has an excellent ability to remove metal impurities, and which has extremely little adhesion of fine particles.

従って、本発明のエツチング液を用いることによって、
高品質・高歩留りの半導体装置を製造することができる
効果がある。
Therefore, by using the etching solution of the present invention,
This has the effect of making it possible to manufacture semiconductor devices of high quality and high yield.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図(a)、 (b)は本発明の実施例1及び従来の
エツチング液中からの金属不純物の取り込みを示す原子
吸光分析及び少数キャリアの再結合ライフタイム測定の
結果を示す図、第2図(a)、 (b)は本発明の実施
例2及び従来のエツチング液による金属不純物に対する
除去効果を示す原子吸光分析及び少数キャリアの再結合
ライフタイム測定の結果を示す図、第3図は本発明のB
HF/H2O2におけるエツチング液中からの金属不純
物の取り込みの組成比依存性を示す少数キャリアの再結
合ライフタイム測定の結果を示す図、第4図はシリコン
基板表面上に付着する微粒子の測定結果を示す図、第5
図は単位時間当たりのエツチング量の測定結果を示す図
である。 特許出願人  日本電気株式会社 )べ 代 理 人  弁理士 菅 野   中、:3−匹R 第 図 第 図 第 図 第 図
FIGS. 1(a) and 1(b) are diagrams showing the results of atomic absorption spectrometry and minority carrier recombination lifetime measurement showing the incorporation of metal impurities from the etching solution of Example 1 of the present invention and the conventional etching solution. Figures 2 (a) and (b) are diagrams showing the results of atomic absorption spectrometry and minority carrier recombination lifetime measurement showing the removal effect on metal impurities by Example 2 of the present invention and the conventional etching solution, and Figure 3. is B of the present invention
Figure 4 shows the results of minority carrier recombination lifetime measurement showing the composition ratio dependence of metal impurity uptake from the etching solution in HF/H2O2. Figure 4 shows the measurement results of fine particles adhering to the silicon substrate surface. Figure 5
The figure shows the measurement results of the amount of etching per unit time. Patent applicant: NEC Corporation) Patent attorney: Naka Kanno: 3-R Figure Figure Figure Figure Figure

Claims (3)

【特許請求の範囲】[Claims] (1)緩衝弗酸溶液中にシリコン基板を浸漬し、シリコ
ン酸化膜をエッチング処理するエッチング液であって、 弗酸を含む緩衝弗酸溶液中に、過酸化水素を含むことを
特徴とするシリコン酸化膜のエッチング液。
(1) An etching solution for etching a silicon oxide film by immersing a silicon substrate in a buffered hydrofluoric acid solution, characterized in that the buffered hydrofluoric acid solution contains hydrogen peroxide. Etching solution for oxide film.
(2)前記緩衝弗酸溶液中に含まれる弗酸の濃度は、0
.1乃至10重量%の範囲であることを特徴とする請求
項第(1)項記載のシリコン酸化膜のエッチング液。
(2) The concentration of hydrofluoric acid contained in the buffered hydrofluoric acid solution is 0.
.. The silicon oxide film etching solution according to claim 1, wherein the etching solution is in the range of 1 to 10% by weight.
(3)前記過酸化水素の濃度は、0.5乃至15重量%
の範囲であることを特徴とする請求項第(1)項記載の
シリコン酸化膜のエッチング液。
(3) The concentration of hydrogen peroxide is 0.5 to 15% by weight.
The silicon oxide film etching solution according to claim 1, wherein the etching solution is within the range of .
JP02154698A 1990-06-13 1990-06-13 Etching solution for silicon oxide film and method for etching silicon oxide film Expired - Fee Related JP3109083B2 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003101055A (en) * 2001-09-27 2003-04-04 Mitsubishi Electric Corp Method for manufacturing solar battery
JP2011003759A (en) * 2009-06-19 2011-01-06 Nikon Corp Cleaning method of member, exposure method, device manufacturing method, and cleaning liquid

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0577733U (en) * 1992-03-25 1993-10-22 スタンレー電気株式会社 Solar sensor
DE102015004101A1 (en) * 2015-03-25 2016-09-29 Condias Gmbh Process for the preparation of dilute hydrofluoric acid

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003101055A (en) * 2001-09-27 2003-04-04 Mitsubishi Electric Corp Method for manufacturing solar battery
JP2011003759A (en) * 2009-06-19 2011-01-06 Nikon Corp Cleaning method of member, exposure method, device manufacturing method, and cleaning liquid

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