KR101391605B1 - A Composition for wet etching of silicon nitride or silicon oxide - Google Patents
A Composition for wet etching of silicon nitride or silicon oxide Download PDFInfo
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- KR101391605B1 KR101391605B1 KR1020100139731A KR20100139731A KR101391605B1 KR 101391605 B1 KR101391605 B1 KR 101391605B1 KR 1020100139731 A KR1020100139731 A KR 1020100139731A KR 20100139731 A KR20100139731 A KR 20100139731A KR 101391605 B1 KR101391605 B1 KR 101391605B1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/30—Acidic compositions for etching other metallic material
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- C09K13/00—Etching, surface-brightening or pickling compositions
- C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
Abstract
본 발명은 실리콘질화막의 습식 식각용 조성물에 관한 것으로 자세하게는 반도체 공정에서 실리콘질화막 또는 실리콘산화막을 식각함에 있어서, 장기간 사용시에도 실리콘질화막과 실리콘산화막의 선택비에 영향을 주지 않고 식각속도를 일정하게 유지할 수 있는 습식 식각용 조성물이며, 인화합물과 암모늄계화합물을 포함하는 습식 식각용 조성물에 관한 것이다.More particularly, the present invention relates to a composition for wet etching a silicon nitride film, and more particularly, to a method for etching a silicon nitride film or a silicon oxide film in a semiconductor process, wherein the etch rate is kept constant without affecting the selectivity between the silicon nitride film and the silicon oxide film The present invention relates to a wet etching composition comprising a phosphorus compound and an ammonium-based compound.
Description
본 발명은 실리콘질화막 또는 실리콘 산화막을 식각하여 제거함에 있어서, 장기간 사용에도 실리콘질화막과 실리콘산화막의 선택도에 영향을 주지 않고 식각 속도를 일정하게 유지할 수 있도록 하는 습식 식각용 조성물에 관한 것이다.The present invention relates to a wet etching composition capable of maintaining a constant etch rate without affecting the selectivity of a silicon nitride film and a silicon oxide film even after long-term use in etching and removing a silicon nitride film or a silicon oxide film.
일반적으로 실리콘질화막을 제거하기 위해서 인산(Phosphoric acid)을 사용하고 있으며, 사용 공정온도가 고온공정이고 초순수의 함량이 질화막과 산화막의 식각률에 영향을 미치기 때문에 인산에 초순수의 함량을 일정하게 유지하기 위하여 순수(Deionized Water)를 공급해야 한다. 또한 인산 자체가 강산이므로 부식성이 있어 취급하기가 까다롭다. Generally, phosphoric acid is used to remove silicon nitride film. In order to maintain the amount of ultrapure water in phosphoric acid because the process temperature is high temperature process and the content of ultrapure water affects the etching rate of nitride film and oxide film Deionized water should be supplied. Also, since phosphoric acid itself is a strong acid, it is corrosive and difficult to handle.
또한, 실리콘 질화막 및 실리콘 산화막의 식각에 있어서 인산계 식각액 조성물을 장기간 사용하는 경우 인산계 식각액의 실리콘 농도가 증가하면서 에칭 속도가 저하된다. 그러므로 실리콘 질화막과 실리콘산화막의 선택비가 급격히 변화하기 때문에 안정적인 공정유지가 어려우며, 장기간 사용하는 경우 인산계 식각액의 실리콘 농도가 포화되어 산화규소로 석출되기 때문에 장기간 사용이 바람직하지 못하다는 단점이 있다. 이를 해결하기 위한 방안으로 한국공개특허 2008-0079999호 에의하면 기존의 인화합물, 붕소화합물, 규소화합물, 불소화합물을 사용하여 산화규소의 석출 없이 장시간 사용이 가능하였으나 붕소화합물이나 규소화합물, 불소화합물의 함유에 따라 실리콘산화막의 식각속도가 다르게 나타나 인산계와 비슷한 실리콘 산화막의 식각속도를 유지하고자 하는 반도체 공정에 바람직하지 못한 문제점이 있다.Further, when the phosphoric acid etchant composition is used for a long time in the etching of the silicon nitride film and the silicon oxide film, the etching rate is lowered while the silicon concentration of the phosphoric acid etchant is increased. Therefore, it is difficult to maintain a stable process because the selectivity ratio between the silicon nitride film and the silicon oxide film changes abruptly, and when used for a long period of time, the silicon concentration of the phosphoric acid etchant is saturated and precipitates into silicon oxide. As a method for solving this problem, Korean Patent Laid-Open Publication No. 2008-0079999 discloses that a phosphorus compound, a boron compound, a silicon compound, and a fluorine compound can be used for a long time without precipitation of silicon oxide. However, The etching rate of the silicon oxide film is different depending on the content of the silicon oxide film, which is an undesirable problem in the semiconductor process for maintaining the etching rate of the silicon oxide film similar to the phosphoric acid system.
상기의 문제점을 해결하고자 본 발명은 암모늄계 화합물을 포함하는 실리콘질화막 또는 실리콘 산화막의 식각에 있어서 산화 규소의 발생으로 인한 에칭 속도 저하 및 실리콘질화막 대 실리콘산화막의 선택도 변화가 발생하지 않고, 장기간 사용이 가능한 습식 식각용 조성물을 제공하는데 그 목적이 있다.In order to solve the above-described problems, the present invention provides a method of manufacturing a silicon nitride film or a silicon oxide film containing an ammonium-based compound, wherein the etching rate is lowered due to the generation of silicon oxide and the selectivity of the silicon nitride film to the silicon oxide film is not changed, The present invention has been made in view of the above problems.
상기 목적을 달성하기 위하여, 본 발명은 인산, 암모늄계화합물 및 물을 함유하는 실리콘 질화막 식각액 조성물을 제공한다.In order to achieve the above object, the present invention provides a silicon nitride film etchant composition containing phosphoric acid, an ammonium compound, and water.
또한, 본 발명의 식각액 조성물은 불소계 화합물을 더 포함할 수 있다.Further, the etching liquid composition of the present invention may further contain a fluorine-based compound.
본 발명에 따른 식각조성물로 식각 공정을 수행하였을 때, 장기간 사용에도 에칭 속도 저하 및 선택도 변화가 발생하지 않으며, 식각 속도를 일정하게 유지하는 효과가 있다.
When the etching process is performed with the etching composition according to the present invention, the etching rate is lowered and selectivity is not changed even after long-term use, and the etching rate is maintained constant.
이하 본 발명을 상세히 설명한다.Hereinafter, the present invention will be described in detail.
본 발명은 인산 60 내지 95중량%, 암모늄계화합물 0.01 내지 20%, 그리고 식각속도를 증가시키기 위해 선택적으로 불소계화합물 0.01 내지 1 중량%를 사용할 수 있으며, 전체 조성물의 총 중량이 100중량%가 되도록 물을 포함하는 실리콘 질화막 식각액 조성물을 제공한다.The present invention can use 60 to 95% by weight phosphoric acid, 0.01 to 20% ammonium compound, and 0.01 to 1% by weight of fluorine compound selectively to increase the etching rate, so that the total weight of the total composition is 100% And a water-containing silicon nitride film etchant composition.
본 발명에 의한 식각액 조성물은 상기 조성 및 함량 범위에서 혼합되었을 때 우수한 식각속도 및 식각량을 제공한다.The etchant compositions according to the present invention provide excellent etching rates and etch rates when mixed in the above composition and content ranges.
본 발명에서 상기 인산은 만족할만한 실리콘질화막의 식각율 및 식각속도를 확보하기 위하여 사용되는 것으로 60 내지 95중량%, 보다 특히 85중량%로 사용하는 것이 바람직하다. 상기 인산이 60 중량% 미만으로 첨가하는 경우 실리콘 질화막의 식각율이 현저하게 저하되며, 95 중량%을 초과하는 경우 실리콘질화막과 함께 실리콘산화막이 식각속도가 급격히 감소하는 단점이 있다.In the present invention, the phosphoric acid is used to secure a satisfactory etching rate and etching rate of the silicon nitride film, and it is preferably used in an amount of 60 to 95 wt%, more particularly 85 wt%. When the phosphoric acid is added in an amount of less than 60 wt%, the etching rate of the silicon nitride film is remarkably lowered. When the phosphoric acid is more than 95 wt%, the etching rate of the silicon oxide film is drastically decreased.
본 발명에서 상기 암모늄계화합물은 암모니아수, 암모늄클로라이드, 암모늄아세트산, 암모늄인산염, 암모늄과옥시이황산염, 암모늄황산염, 암모늄불산염에서 선택되는 어느 하나 또는 둘 이상의 혼합물인 것을 사용할 수 있다. 또한 암모늄계화합물은 상기 화합물에 한정되는 것은 아니고 암모늄이온을 갖고 있는 모든 화합물을 포함한다. 상기 암모늄계화합물이 0.01중량% 미만으로 첨가되는 경우 장기간 사용시 선택도를 유지하는 효과가 감소하고, 20중량% 초과로 첨가되는 경우 실리콘질화막과 실리콘 산화막의 식각 속도가 변화하게 되어 선택도가 변화하게 된다.
In the present invention, the ammonium compound may be any one or a mixture of two or more selected from ammonia water, ammonium chloride, ammonium acetic acid, ammonium phosphate, ammonium and oxysulfate, ammonium sulfate and ammonium fluorate. The ammonium-based compound is not limited to the above-mentioned compounds but includes all compounds having an ammonium ion. When the ammonium-based compound is added in an amount of less than 0.01% by weight, the effect of maintaining the selectivity for a long period of time is decreased. When the ammonium-based compound is added in an amount exceeding 20% by weight, the etching rate of the silicon nitride film and the silicon oxide film is changed, do.
본 발명에서 상기 불소계화합물은 불화수소, 불화암모늄, 불화수소암모늄에서 선택되는 어느 하나 또는 둘이상의 혼합물인 것을 사용할 수 있다. 보다 바람직하게는 불화수소암모늄을 사용하는 것이 장기간 사용시 선택도 유지하기 때문에 좋다. 상기 불소계화합물이 0.01중량% 미만으로 첨가되는 경우 질화막의 식각속도가 작아져 질화막 제거가 용이하지 않을 수 있으며, 1중량%을 초과하는 경우 실리콘질화막의 식각 속도가 크게 향상되지만, 실리콘산화막 또한 식각되는 단점이 있다.In the present invention, the fluorine-based compound may be any one or a mixture of two or more selected from hydrogen fluoride, ammonium fluoride, and ammonium hydrogen fluoride. More preferably, the use of ammonium hydrogen fluoride is preferable because it maintains the selectivity during long-term use. When the fluorine-based compound is added in an amount of less than 0.01% by weight, the etching rate of the nitrided film is decreased and the removal of the nitride film may not be easy. When the fluorinated compound is added in an amount exceeding 1% by weight, the etching rate of the silicon nitride film is greatly improved. There are disadvantages.
본 발명의 상기 실리콘질화막 습식 식각용 조성물은 식각하고자 하는 실리콘질화막에 도포하기전에 가열하여 사용하는 것이 보다 효과적인 식각 성능을 얻을 수 있으며 구체적으로는 100 내지 180℃로 예열하여 이용하는 것이 좋다.The silicon nitride film wet etching composition of the present invention may be heated and used before being applied to the silicon nitride film to be etched to obtain a more effective etching performance. Specifically, it may be preheated to 100 to 180 占 폚.
본 발명에 의한 식각조성물은 실리콘질화막 또는 실리콘 산화막을 식각하여 제거함에 있어서, 장기간 사용에도 에칭 속도 저하 및 선택비 변화가 발생하지 않으며, 식각 속도를 일정하게 유지하는 효과가 있다.The etching composition according to the present invention has an effect of maintaining the etching rate constant even when the silicon nitride film or the silicon oxide film is etched and removed, without any lowering of the etching rate and change of the selection ratio even after long-term use.
이하, 실시예에 의해 본 발명을 보다 상세히 설명하나, 이는 발명의 구성 및 효과를 이해시키기 위한 것일 뿐, 본 발명의 범위를 제한하고자 하는 것은 아니다.
Hereinafter, the present invention will be described in more detail with reference to Examples. However, the present invention is not intended to limit the scope of the present invention.
[실시예 1] [Example 1]
인산 85중량%, 암모늄클로라이드 0.2중량% 및 14.8중량%의 탈이온수를 혼합하여 실리콘 질화막 습식 식각조성물을 제조하였다. 제조한 조성물을 비이커에 투입하고 157℃ 온도에 도달했을 때 실리콘산화막(SiO2)이 형성된 기판과 실리콘 질화막이 형성된 기판을 각각 10분간 침지하여 식각을 실시하였으며 산화막 식각속도를 측정하였다. 이를 1배취로 해서 이후 30분 단위로 연속적으로 반복 측정하였다.85 wt% phosphoric acid, 0.2 wt% ammonium chloride, and 14.8 wt% deionized water were mixed to prepare a silicon nitride film wet etching composition. The prepared composition was put into a beaker, and when the temperature reached 157 ° C, the substrate on which the silicon oxide film (SiO 2 ) was formed and the substrate on which the silicon nitride film was formed were immersed for 10 minutes, and the etching rate was measured. This was repeated one time and then repeatedly measured every 30 minutes.
상기 식각조성물의 구성성분과 함량은 하기 표 1에 나타내었다.The composition and content of the etching composition are shown in Table 1 below.
[실시예 2][Example 2]
암모늄클로라이드 대신에 암모늄황산염을 첨가한 것을 제외하고는 상기 실시예 1과 동일하게 실시하였다. The procedure of Example 1 was repeated, except that ammonium sulfate was added instead of ammonium chloride.
[실시예 3][Example 3]
암모늄클로라이드 대신에 암모늄인산염을 첨가한 것을 제외하고는 상기 실시예 1과 동일하게 실시하였다. The procedure of Example 1 was repeated except that ammonium phosphate was added instead of ammonium chloride.
[실시예 4][Example 4]
불화수소암모늄 0.01중량%을 더 첨가한 것을 제외하고는 상기 실시예 1과 동일하게 실시하였다.Except that 0.01 wt% of ammonium hydrogen fluoride was further added.
[비교예 1][Comparative Example 1]
상기 실시예 1과 동일하게 실시하되, 하기 표 1에 나타난 구성성분과 함량으로 혼합하여 제조하였다.The same procedure as in Example 1 was carried out except that the ingredients and the contents shown in Table 1 were mixed.
[비교예 2][Comparative Example 2]
불화수소암모늄 0.01중량%을 더 첨가한 것을 제외하고는 상기 비교예 1과 동일하게 실시하였다.
Comparative Example 1 was repeated except that 0.01 wt% of ammonium hydrogen fluoride was further added.
[물성측정][Measurement of physical properties]
식각속도는 엘립소미트리(Nano-View, SE-MG-1000; Ellipsometery)를 이용하여 실리콘 질화막의 두께를 측정함으로써 결정하였다The etching rate was determined by measuring the thickness of the silicon nitride film using a Nano-View (SE-MG-1000; Ellipsometry)
<식각속도감소율><Reduction rate of etching rate>
식각속도감소율을 결정하는 수식은 다음과 같다..The formula for determining the etch rate reduction is:
상기 식에서,In this formula,
A는 초기 막 에칭속도;A is the initial film etch rate;
B는 가열시간에 대한 막 에칭속도;B is the film etching rate with respect to the heating time;
C는 식각속도 감소율(%) 이다.C is the etching rate reduction rate (%).
구 분
division
조성물
Composition
(℃)Process temperature
(° C)
식각속도
(Å/min)Nitride film
Etching rate
(Å / min)
식각속도
(Å/min)Oxide film
Etching rate
(Å / min)
식각속도
감소율(%)Oxide film
Etching rate
Decrease (%)
실시예 1
Example 1
+ 암모늄클로라이드(0.2중량%)Phosphoric acid (85 wt% aqueous solution)
+ Ammonium chloride (0.2% by weight)
157
157
실시예 2
Example 2
+ 암모늄황산염(0.2중량%)Phosphoric acid (85 wt% aqueous solution)
+ Ammonium sulfate (0.2% by weight)
157
157
실시예 3
Example 3
+ 암모늄인산염(0.2중량%)Phosphoric acid (85 wt% aqueous solution)
+ Ammonium phosphate (0.2% by weight)
157
157
실시예 4
Example 4
+ 암모늄클로라이드(0.2중량%)
+ 불화수소암모늄(0.01중량%)Phosphoric acid (85 wt% aqueous solution)
+ Ammonium chloride (0.2% by weight)
+ Ammonium hydrogen fluoride (0.01% by weight)
157
157
비교예 1
Comparative Example 1
인산(85중량% 수용액)
Phosphoric acid (85 wt% aqueous solution)
157
157
비교예 2
Comparative Example 2
+ 불화수소암모늄(0.01중량%)Phosphoric acid (85 wt% aqueous solution)
+ Ammonium hydrogen fluoride (0.01% by weight)
157
157
상기 [표 1]에 나타낸 바와 같이 본 발명의 실리콘질화막 습식 식각용 조성물은 기판을 침지한 결과, 인산 및 암모늄계화합물을 함유하는 실리콘 산화막의 식각속도가 5내지 6(Å/min)으로 나타났고, 이때의 산화막 식각속도 감소율이 2% 이하였다. 비교예 2의 결과를 보면 초기대비 60분 후의 산화막 식각속도 감소율이 55%인 것으로 나타났는데 이와 비교해 보면 본 발명의 효과를 확인할 수가 있다. As shown in Table 1, the silicon nitride film wet etching composition of the present invention was found to have an etching rate of 5 to 6 (Å / min) for a silicon oxide film containing phosphoric acid and ammonium compounds as a result of immersing the substrate , And the reduction rate of the oxide film etching rate at this time was 2% or less. The results of Comparative Example 2 show that the reduction rate of the oxide film etching rate after 60 minutes from the initial value is 55%, which is comparable to that of the present invention.
또한 인산, 암모늄클로라이드 및 불화암모늄을 함유하는 실리콘산화막의 식각속도는 7.35내지 6.10(Å/min)으로 나타났고, 이때의 산화막 식각속도 감소율은 비교예2와 비교하여 현저히 적은 놀라운 효과를 확인하였다.In addition, the etching rate of the silicon oxide film containing phosphoric acid, ammonium chloride and ammonium fluoride was found to be 7.35 to 6.10 (Å / min), and the etching rate reduction rate at this time was remarkably small as compared with Comparative Example 2.
본 발명에 따르면 암모늄화합물을 함유하는 조성물을 사용함으로서 산화막의식각속도를 유지하는데 이점이 있다.According to the present invention, the use of a composition containing an ammonium compound is advantageous in maintaining the oxide film consciousness angular speed.
Claims (6)
Phosphoric acid, and water of at least one acid selected from sulfuric acid, phosphoric acid, and hydrochloric acid.
상기 식각액 조성물은 인산 60 내지 95중량%, 암모늄염 0.01 내지 20중량% 및 잔여량의 물을 포함하는 실리콘 질화막 식각액 조성물.
The method according to claim 1,
Wherein the etchant composition comprises 60 to 95 wt% phosphoric acid, 0.01 to 20 wt% ammonium salt, and a balance of water.
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KR20180084210A (en) | 2017-01-16 | 2018-07-25 | 동우 화인켐 주식회사 | Non-phosphoric acid based composition for etching silicon nitride layer |
US10242880B2 (en) | 2016-10-07 | 2019-03-26 | Samsung Electronics Co., Ltd. | Method of wet etching and method of fabricating semiconductor device using the same |
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KR101380487B1 (en) * | 2012-05-09 | 2014-04-01 | 오씨아이 주식회사 | Etching solution for silicon nitride layer |
US9868902B2 (en) | 2014-07-17 | 2018-01-16 | Soulbrain Co., Ltd. | Composition for etching |
KR102398593B1 (en) | 2017-05-02 | 2022-05-17 | 주식회사 이엔에프테크놀로지 | Etching composition for silicon nitride film |
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