KR20100067952A - Cmp slurry having improved polishing selectivity and dispersion stability - Google Patents
Cmp slurry having improved polishing selectivity and dispersion stability Download PDFInfo
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- KR20100067952A KR20100067952A KR1020080126563A KR20080126563A KR20100067952A KR 20100067952 A KR20100067952 A KR 20100067952A KR 1020080126563 A KR1020080126563 A KR 1020080126563A KR 20080126563 A KR20080126563 A KR 20080126563A KR 20100067952 A KR20100067952 A KR 20100067952A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/04—Aqueous dispersions
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30625—With simultaneous mechanical treatment, e.g. mechanico-chemical polishing
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/31051—Planarisation of the insulating layers
- H01L21/31053—Planarisation of the insulating layers involving a dielectric removal step
Abstract
Description
본 발명은 반도체 제조의 CMP(Chemical Mechanical Planarization)공정에 사용되는 연마용 슬러리에 관한 것으로서, 구체적으로는 반도체 제조공정 중 ILD(Interlayer Dielectric) 공정 및/또는 STI(Shallow Trench Isolation) 공정에서 산화규소(SiO2)막과 질화규소(Si3N4)막의 연마 선택비를 향상시킬 수 있고, 불안정한 분산에 의한 필터 막힘 문제를 해결할 수 있는 CMP 슬러리에 관한 것이다. BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a polishing slurry used in a chemical mechanical planarization (CMP) process of semiconductor manufacturing, and more particularly, to silicon oxide in an interlayer dielectric (ILD) process and / or a shallow trench isolation (STI) process during a semiconductor manufacturing process. The present invention relates to a CMP slurry capable of improving the polishing selectivity of the SiO 2 ) film and the silicon nitride (Si 3 N 4 ) film and solving the problem of filter clogging due to unstable dispersion.
CMP(Chemical Mechanical Planarization, 화학적 기계적 평탄화)는 화학적 연마 및 기계적 연마가 동시에 상호작용을 하여 반도체 웨이퍼를 평탄화시키는 연마공정이다. 최근 반도체 소자의 고집적화, 고성능화에 따라 패턴의 선폭은 더욱 미세해지고, 구조는 점점 다층화되는 추세이며, 포토리소그래피(photolithography)의 정밀도 향상을 위해서는 각 공정에서의 층간 평탄도가 매우 중요한 요소이다. 이러한 평탄화 기술로서, 현재 가장 각광받고 있는 것이 CMP이며, CMP는 연마 대상 물질에 따라, 산화막(oxide) CMP, 금속(metal) CMP, 폴리실리콘(poly -Si) CMP 등 으로 분류되기도 한다. Chemical Mechanical Planarization (CMP) is a polishing process in which chemical polishing and mechanical polishing simultaneously interact to planarize a semiconductor wafer. In recent years, the line width of the pattern becomes finer and the structure becomes more and more multilayered with high integration and high performance of semiconductor devices. In order to improve the precision of photolithography, the interlayer flatness in each process is an important factor. As such a planarization technique, CMP is currently attracting the most attention, and CMP may be classified into an oxide CMP, a metal CMP, a poly-Si CMP, and the like depending on the material to be polished.
이 중, 산화막을 연마하는 CMP가 적용되는 반도체 공정은 대표적으로 ILD (Interlayer Dielectric) 공정과 STI(Shallow Trench Isolation)을 들 수 있으며, ILD공정은 층간 절연을 위해 과량으로 성막된 실리콘 산화막(silicon oxide)을 제거하기 위한 공정이고, STI공정은 칩(Chip)간 절연을 위해 트렌치(trench)를 형성하여 소자 분리를 하는 공정이다. Among these, semiconductor processes to which CMP is applied to polish oxide films are typically an interlayer dielectric (ILD) process and shallow trench isolation (STI), and an ILD process is an excessively formed silicon oxide film (silicon oxide) for interlayer insulation. ), And the STI process is a process of forming a trench to insulate the devices to insulate the chips.
CMP가 평탄화에 적용된 초기에는 산화막 연마를 위하여 실리카(SiO2) 슬러리가 주로 사용되었으나, 디자인 룰(design rule)이 작아지고, 소자가 박막화되어 고평탄화가 필요하게 됨에 따라, 기존의 실리카 슬러리 뿐 만 아니라, 이종(異種)의 막 간에 연마 선택비가 높은 산화세륨(CeO2) 슬러리를 적용하게 되었다. 산화세륨 슬러리는 실리콘 산화막에 대한 연마속도는 높고, 실리콘 질화막(Silicon Nitride, Si3N4)에 대한 연마속도는 매우 낮아, 단차가 있는 실리콘 산화막과 실리콘 질화막의 동시 연마시, 실리콘 산화막이 먼저 연마되고, 실리콘 질화막에서는 연마가 종료되는 식각 종료 기능을 가지는 것이 특징이다. 따라서, 이러한 산화세륨 슬러리를 산화막 CMP에 적용함으로써, 광역 평탄화(global planarization) 및 연마두께의 정밀한 제어가 가능하게 되었다. In the early days when CMP was applied to planarization, silica (SiO 2 ) slurries were mainly used for oxide polishing. However, as the design rule becomes smaller and the device becomes thinner and needs higher planarization, only conventional silica slurries are used. Rather, cerium oxide (CeO 2 ) slurries with high polishing selectivities were applied between heterogeneous films. The cerium oxide slurry has a high polishing rate for the silicon oxide film and a very low polishing rate for the silicon nitride film (Silicon Nitride, Si 3 N 4 ), so that the silicon oxide film is first polished at the same time when the stepped silicon oxide film and the silicon nitride film are simultaneously polished. The silicon nitride film is characterized by having an etching termination function in which polishing is completed. Therefore, by applying such a cerium oxide slurry to the oxide film CMP, global planarization and precise control of the polishing thickness can be achieved.
종래의 산화세륨 슬러리에 관해서는 보다 높은 연마 선택비를 갖도록 하기 위해 산화세륨 입자의 특성을 제어하거나, 첨가제를 추가하여 실리콘 질화막의 연마 속도를 현저히 낮춤으로 인해 실리콘 산화막과의 연마 선택비를 증진시키는 방 법을 사용한 예 들이 있으며, 한국등록특허 0366304호에서는 산화세륨 슬러리에 피리딘계 화합물을 첨가함으로써 연마성능을 향상시킨 예가 있다. As for the conventional cerium oxide slurry, it is possible to control the properties of the cerium oxide particles in order to have a higher polishing selectivity, or to add an additive to improve the polishing selectivity with the silicon oxide film by significantly lowering the polishing rate of the silicon nitride film. There are examples using the method, and in Korean Patent No. 0366304, there is an example in which polishing performance is improved by adding a pyridine compound to a cerium oxide slurry.
본 발명자들은 CMP 슬러리에 피리딘계 화합물을 첨가하는 경우, 슬러리 제조공정 중 불순물을 제거하기 위한 필터링 공정에서, 필터 후의 슬러리 내 연마입자 고형분의 함량이 급격히 줄어들게 되며, 반도체 웨이퍼의 연마 전에 실시하는 필터링 공정에서도 또 다시 연마입자 고형분의 함량이 줄어들어, 슬러리 제조시 손실이 발생함은 물론, 원하는 연마성능을 확보하지 못하는 문제점이 있음을 발견하였다. When the pyridine-based compound is added to the CMP slurry, the present inventors rapidly reduce the content of the solid particles in the slurry after the filter in the filtering process for removing impurities during the slurry manufacturing process, and performs the filtering process before polishing the semiconductor wafer. In addition, the content of the abrasive grains is reduced again, so that the loss occurs in the slurry production, as well as found that there is a problem that does not secure the desired polishing performance.
본 발명은 상기의 문제점을 해결하기 위한 것으로서, 피리딘계 화합물 및/또는 벤조산계 화합물이 포함된 산화세륨 슬러리에, 비이온성 화합물을 첨가함으로써, 필터 막힘 또는 필터를 통한 연마입자 고형분 손실을 방지함과 동시에, 우수한 연마선택비를 갖는 CMP 슬러리를 제공하고자 한다. The present invention is to solve the above problems, by adding a non-ionic compound to the cerium oxide slurry containing a pyridine-based compound and / or benzoic acid-based compound, to prevent the clogging of the filter or the loss of solid particles through the filter and At the same time, it is intended to provide a CMP slurry with good polishing selectivity.
본 발명은 물; 연마입자; 피리딘계 화합물 및 벤조산계 화합물로 구성된 군에서 선택된 1종 이상의 물질; 및 폴리옥시프로필렌에테르 및 폴리옥시에틸렌옥시프로필렌공중합체로 구성된 군에서 선택된 1종 이상의 비이온성 화합물을 포함하는 CMP 슬러리를 제공한다.The present invention is water; Abrasive particles; At least one substance selected from the group consisting of a pyridine compound and a benzoic acid compound; And at least one nonionic compound selected from the group consisting of polyoxypropylene ether and polyoxyethylene oxypropylene copolymer.
본 발명에 따라, CMP 슬러리에 피리딘계 화합물 및/또는 벤조산계 화합물과 함께, 폴리옥시프로필렌에테르 및/또는 폴리옥시에틸렌옥시프로필렌 공중합체의 비이온성 화합물을 첨가하는 경우, 실리콘 산화막의 연마속도를 향상시키고, 실리콘 산화막과 실리콘 질화막 간의 연마 선택비를 높일 수 있으며, 불순물 제거를 위한 필터링 공정에서 필터 막힘 및 연마입자 고형분 손실 문제를 해결할 수 있다. According to the present invention, when a nonionic compound of polyoxypropylene ether and / or polyoxyethylene oxypropylene copolymer is added to a CMP slurry together with a pyridine compound and / or a benzoic acid compound, the polishing rate of the silicon oxide film is improved. In addition, it is possible to increase the polishing selectivity between the silicon oxide film and the silicon nitride film, and solve the problem of filter clogging and loss of abrasive solids in the filtering process for removing impurities.
본 발명은 물; 연마입자; 피리딘계 화합물 및/또는 벤조산계 화합물을 포함하는 CMP 슬러리에 있어서, 폴리옥시프로필렌에테르 및/또는 폴리옥시에틸렌옥시프로필렌 공중합체의 비이온성 화합물을 포함하는 것을 특징으로 한다. The present invention is water; Abrasive particles; A CMP slurry comprising a pyridine compound and / or a benzoic acid compound is characterized by comprising a nonionic compound of a polyoxypropylene ether and / or a polyoxyethyleneoxypropylene copolymer.
피리딘계 화합물 및/또는 벤조산계 화합물을 첨가제로 포함하는 CMP슬러리는 높은 연마속도를 가지며, 실리콘 산화막과 실리콘 질화막 간의 연마 선택비가 높다는 장점을 가지고 있으나, 피리딘계 화합물 및/또는 벤조산계 화합물과, 금속산화물 연마제 및 기타 첨가제를 혼합하여 필터링 공정을 거칠 때, 필터의 포어(pore)를 막는 현상이 나타난다. 따라서, 이러한 막힘 현상을 극복하기 위해서 반응성이 없고, 분산작용 및 윤활작용이 높은 폴리옥시프로필렌에테르 및/또는 폴리옥시에틸렌옥시프로필렌 공중합체와 같은 비이온성 화합물을 CMP 슬러리에 추가로 포함함으로써, 연마입자의 분산 안정성이 유지되면서 상기의 필터 막힘 및 연마입자 고형분 손실 문제를 해결할 수 있었다.CMP slurry containing a pyridine compound and / or a benzoic acid compound as an additive has a high polishing rate and a high polishing selectivity between the silicon oxide film and the silicon nitride film, but the pyridine compound and / or the benzoic acid compound and the metal When the oxide abrasive and the other additives are mixed and subjected to the filtering process, clogging of the filter pores occurs. Therefore, in order to overcome this clogging phenomenon, non-reactive, highly dispersive and highly lubricating compounds, such as polyoxypropylene ether and / or polyoxyethylene oxypropylene copolymer, by additionally including in the CMP slurry, abrasive particles While maintaining the dispersion stability of the filter clogging and the loss of the solid particles was able to solve the problem.
본 발명의 CMP 슬러리에 포함되는 비이온성 유기 화합물은 폴리옥시프로필렌에테르 및/또는 폴리옥시에틸렌옥시프로필렌 공중합체로서, 하기 화학식 1 및/또는 화학식 2로 표시되는 물질일 수 있다. The nonionic organic compound included in the CMP slurry of the present invention may be a polyoxypropylene ether and / or a polyoxyethylene oxypropylene copolymer, and a material represented by the following Chemical Formula 1 and / or Chemical Formula 2.
[화학식1][Formula 1]
R(OCHCH3CH2)n-OR'R (OCHCH 3 CH 2 ) n -OR '
(R 및 R'는 H 또는 탄소수 1~18인 알킬기이며, n은 3 ~ 10인 정수)(R and R 'is H or an alkyl group having 1 to 18 carbon atoms, n is an integer of 3 to 10)
[화학식2](2)
RO(CH2CH2O)x(CH(CH3)CH2O)y(CH2CH2O)z-OR' RO (CH 2 CH 2 O) x (CH (CH 3 ) CH 2 O) y (CH 2 CH 2 O) z -OR '
((R 및 R'는 H 또는 탄소수 1~18인 알킬기이며, x, y 및 z은 3 ~ 10인 정수)(R and R 'are H or an alkyl group having 1 to 18 carbon atoms, and x, y and z are integers of 3 to 10)
본 발명의 CMP 슬러리에 포함되는 비이온성 화합물의 분자량 범위는 특별히 제한되지는 않으나, 바람직하게는 분자량 192 내지 10,000범위의 것일 수 있고, 더욱 바람직하게는 분자량 400 내지 3,100범위의 것일 수 있다. The molecular weight range of the nonionic compound included in the CMP slurry of the present invention is not particularly limited, but may preferably be in the range of 192 to 10,000 molecular weight, more preferably in the range of 400 to 3,100 molecular weight.
본 발명의 CMP 슬러리에 포함되는 비이온성 화합물의 함량은 바람직하게는 전체 슬러리 100중량부 대비 0.005중량부 내지 1중량부 범위일 수 있다. 비이온성 화합물 함량이 상기 범위인 경우에 필터 막힘 현상을 해결함과 동시에, 우수한 연마성능도 확보할 수 있는 장점이 있다.The content of the nonionic compound included in the CMP slurry of the present invention may preferably range from 0.005 parts by weight to 1 part by weight based on 100 parts by weight of the total slurry. When the nonionic compound content is within the above range, there is an advantage in that the filter clogging phenomenon is solved and an excellent polishing performance is also ensured.
본 발명의 CMP 슬러리는 피리딘계 화합물 및/또는 벤조산계 화합물을 포함하는 것으로서, 상기 피리딘계 화합물은 당업자에게 알려진 것이면 특별히 제한되지 않으며, 그 비제한적인 예로는 피리딘-2-카르복실산, 피리딘-3-카르복실산, 피리딘-4-카르복실산, 피리딘-2-아민, 피리딘-2,3-카르복실산, 피리딘-2-카르복스알데히드, 피리딘-3-카르복스알데히드, 3-히드록시 피리딘 및 2-히드록시 피리딘 등이 있고, 상기 물질들은 단독으로 사용하거나 또는 2종이상 혼합하여 사용할 수 있다. The CMP slurry of the present invention includes a pyridine-based compound and / or a benzoic acid-based compound, and the pyridine-based compound is not particularly limited as long as it is known to those skilled in the art, and non-limiting examples thereof include pyridine-2-carboxylic acid and pyridine-. 3-carboxylic acid, pyridine-4-carboxylic acid, pyridine-2-amine, pyridine-2,3-carboxylic acid, pyridine-2-carboxaldehyde, pyridine-3-carboxaldehyde, 3-hydroxy Pyridine, 2-hydroxy pyridine and the like, and the above materials may be used alone or in combination of two or more thereof.
또한, 상기 벤조산계 화합물 역시 당업자에게 알려진 것이면 특별히 제한되 지 않으며, 그 비제한적인 예는 3-히드록시벤조산, 4-히드록시벤조산, 3-아미노벤조산 및 4-아미노벤조산 등이 있고, 상기 물질들은 단독으로 사용하거나 또는 2종이상 혼합하여 사용할 수 있다. In addition, the benzoic acid-based compound is not particularly limited as long as it is known to those skilled in the art, and non-limiting examples thereof include 3-hydroxybenzoic acid, 4-hydroxybenzoic acid, 3-aminobenzoic acid and 4-aminobenzoic acid, and the like. These may be used alone or in combination of two or more thereof.
상기 피리딘계 화합물 및/또는 벤조산계 화합물은 CMP 슬러리에 첨가되어 질화규소막(Si3N4)를 선택적으로 패시베이션(Passivation)하여 연마가 되지 않게 한다. 따라서 산화규소막(SiO2)과 질화규소막 간의 연마를 선택적으로 이루어지게 하는 것이다. The pyridine-based compound and / or benzoic acid-based compound are added to the CMP slurry to selectively passivate the silicon nitride film (Si 3 N 4 ) to prevent polishing. Therefore, the polishing between the silicon oxide film (SiO 2 ) and the silicon nitride film is selectively performed.
특히 바람직하게는, 상기 피리딘계 화합물 및/또는 벤조산계 화합물에서 선택된 단독 또는 2종 이상을 혼합하여 사용할 수 있다.Especially preferably, it can be used individually or in mixture of 2 or more types chosen from the said pyridine type compound and / or a benzoic acid type compound.
본 발명의 CMP 슬러리에 포함되는 상기 피리딘계 화합물 및/또는 벤조산계 화합물의 함량은 전체 슬러리 100 중량부 대비 0.1 중량부 내지 1 중량부 범위일 수 있다. 피리딘계 화합물 및/또는 벤조산계 화합물의 함량이 상기 범위인 경우에 우수한 연마속도와 함께 높은 선택비를 구현할 수 있고, 분산안정성 역시 확보할 수 있는 장점이 있다. The content of the pyridine-based compound and / or benzoic acid-based compound included in the CMP slurry of the present invention may range from 0.1 part by weight to 1 part by weight based on 100 parts by weight of the total slurry. When the content of the pyridine-based compound and / or benzoic acid-based compound is within the above range, it is possible to realize a high selectivity with excellent polishing rate and to secure dispersion stability.
본 발명의 CMP 슬러리에 포함되는 연마입자는 통상적인 CMP 슬러리에 사용되는 금속산화물 입자이면 특별히 제한되지 않으며, 그 비제한적인 예로는 산화세륨(CeO2), 실리카(SiO2), 알루미나(Al2O3), 지르코니아(ZrO2) 및 티타니아(TiO2) 등이 있고, 상기 연마입자는 단독으로 사용하거나 또는 2종이상 혼합하여 사용할 수 있다. The abrasive particles included in the CMP slurry of the present invention are not particularly limited as long as they are metal oxide particles used in a conventional CMP slurry, and non-limiting examples thereof include cerium oxide (CeO 2 ), silica (SiO 2 ), and alumina (Al 2). O 3 ), zirconia (ZrO 2 ), titania (TiO 2 ), and the like, and the abrasive particles may be used alone or in combination of two or more thereof.
바람직하게는 본 발명의 CMP 슬러리에 포함되는 연마입자는 산화세륨(CeO2)일 수 있다. 이러한 산화세륨 연마입자의 제조방법은 금속산화물의 제조방법으로서 당업자에게 알려진 것이면 특별히 제한되지 않으며, 그 비제한적인 예로는 고상법, 기상법 및 액상법 등이 있고, 예를 들어 탄산세륨을 600 내지 1000 ℃ 온도에서 수 분 내지 수십 시간 동안 열처리하여 제조할 수 있다. Preferably, the abrasive particles included in the CMP slurry of the present invention may be cerium oxide (CeO 2 ). The method for producing cerium oxide abrasive particles is not particularly limited as long as it is known to those skilled in the art as a method for producing a metal oxide, and the non-limiting examples thereof include a solid phase method, a gas phase method and a liquid phase method. It may be prepared by heat treatment at a temperature for several minutes to several tens of hours.
본 발명의 CMP 슬러리에 포함되는 연마입자로서 산화세륨이 사용될 경우에는, 상기 산화세륨의 결정립(crystallite) 크기는 15nm 내지 100nm 범위일 수 있다. 산화세륨의 결정립 크기가 상기 범위인 경우에 높은 연마속도를 구현할 수 있으며, 웨이퍼 표면에 발생하는 마이크로 스크래치도 최소화할 수 있는 장점이 있다. When cerium oxide is used as the abrasive particles included in the CMP slurry of the present invention, the crystallite size of the cerium oxide may range from 15 nm to 100 nm. When the grain size of cerium oxide is within the above range, it is possible to realize a high polishing rate and to minimize the micro scratches occurring on the wafer surface.
상기 결정립의 크기는 XRD(X-ray Diffraction)를 이용하여 측정할 수 있으며, 예를 들어 산화세륨 메인 피크의 반치폭으로부터 계산할 수 있다. The grain size may be measured using XRD (X-ray Diffraction), for example, it may be calculated from the half width of the cerium oxide main peak.
본 발명의 CMP 슬러리에 포함되는 연마입자의 함량은 특별히 제한되지는 않으나, 바람직하게는 전체 슬러리 100 중량부 대비 0.1 중량부 내지 1 중량부 범위일 수 있다. 연마입자 함량이 상기 범위인 경우에 반도체 웨이퍼 연마시 높은 연마속도를 구현할 수 있으며, 웨이퍼 표면에 발생하는 마이크로 스크래치도 최소화할 수 있는 장점이 있다. The content of the abrasive particles included in the CMP slurry of the present invention is not particularly limited, but may preferably range from 0.1 part by weight to 1 part by weight based on 100 parts by weight of the total slurry. When the abrasive particle content is in the above range, it is possible to implement a high polishing rate when polishing a semiconductor wafer, and there is an advantage of minimizing the micro scratches generated on the wafer surface.
본 발명의 CMP 슬러리의 pH는 특별히 제한되지 않으나, 바람직하게는 pH 4 내지 6 범위일 수 있다. 슬러리의 pH가 상기 범위인 경우에 실리콘 산화막에 대한 연마속도를 높게 유지할 수 있고, 연마입자의 침전없이 우수한 분산안정성을 확보할 수 있는 장점이 있다. The pH of the CMP slurry of the present invention is not particularly limited, but may preferably be in the range of pH 4-6. When the pH of the slurry is within the above range, it is possible to maintain a high polishing rate for the silicon oxide film and to secure excellent dispersion stability without precipitation of the abrasive particles.
따라서, 본 발명의 CMP 슬러리는 적절한 pH범위를 유지하기 위하여, 상기의 함유물 이외에 pH 조절제를 더 포함할 수 있다. pH 조절제는 통상의 CMP 슬러리에서 pH를 조절하기 위하여 사용하는 산성 또는 염기성의 물질로서 당업자에게 알려진 것이라면 특별히 제한되지 않으며, 그 비제한적인 예로 염기성 물질로서는, 트리메탄올아민(Trimetanolamine), 트리에탄올아민(Trietanolamine), 트리메틸암모늄하이드록사이드(Trimethylammonium hydroxide), 트리에틸암모늄하이드록사이드(Triethylammonium hydroxide), 디메틸벤질아민(Dimethylbenzylamine), 에톡시벤질아민(Ethoxybenzyl amine) 및 수산화 칼륨(Potassium hydroxide) 등이 있으며, 산성 물질로서는, 염산(hydrochloric acid), 황산(sulfuric acid) 및 질산(nitric acid) 등이 있고, 상기 물질들은 단독으로 사용하거나 또는 2종이상 혼합하여 사용할 수 있다. Accordingly, the CMP slurry of the present invention may further include a pH adjusting agent in addition to the above-mentioned contents in order to maintain an appropriate pH range. The pH adjusting agent is not particularly limited as long as it is known to those skilled in the art as an acidic or basic substance used to control pH in a conventional CMP slurry. ), Trimethylammonium hydroxide, triethylammonium hydroxide, dimethylbenzylamine, ethoxybenzyl amine and potassium hydroxide. Examples of the substance include hydrochloric acid, sulfuric acid, nitric acid, and the like, which may be used alone or in combination of two or more thereof.
본 발명에 의한 CMP 슬러리는 탁월한 분산 안정성으로 인하여 일액형 형태로 사용이 가능한 장점이 있다. 상용의 CMP 슬러리는 연마 성능을 향상시키기 위하여 별도의 첨가제를 포함하는 경우가 많으나, 이로 인하여 분산 안정성이 심각하게 저해되어 슬러리 제조 후 반도체 웨이퍼 연마에 적용하기까지의 시간 동안 연마입자 고형분의 응집 및 침전 현상이 심하게 일어나는 문제점이 있다. 따라서, 상용의 CMP 슬러리는 연마입자를 포함하는 슬러리와 연마성능 향상 첨가제를 포함하는 슬러리를 따로 제조한 후, 연마 공정에 적용하기 직전에 혼합하여 사용하는 이액형 형태를 가지는 경우가 대부분이다. 그러나, 본 발명에 의한 CMP 슬러리는 일액형 형태로 사용하더라도 연마입자 고형분의 응집 및 침전 현상이 일어나지 않고, 장시간 동안 우수한 분산 안정성을 보이는 장점이 있으며, 일액형 형태로서 연마공정에의 적용이 편리하고, 슬러리 물성 제어가 용이하며, 별도의 혼합으로 인한 반도체 연마공정에서의 슬러리 물성 편차를 줄일 수 있는 장점이 있다. CMP slurry according to the present invention has the advantage that can be used in one-component form due to excellent dispersion stability. Commercially available CMP slurries often contain separate additives to improve polishing performance.Because of this, the dispersion stability is severely impaired, which leads to agglomeration and precipitation of the abrasive grain solids during the time from the slurry preparation to application to semiconductor wafer polishing. There is a problem that occurs badly. Therefore, commercially available CMP slurries generally have a two-part form in which a slurry containing abrasive particles and a slurry containing abrasive performance improving additives are separately prepared and then mixed and used immediately before being applied to a polishing process. However, the CMP slurry according to the present invention has the advantage of exhibiting excellent dispersion stability for a long time without agglomeration and sedimentation of the solid particles of abrasive particles even when used in a one-component form, and is convenient to apply to the polishing process as a one-component form. In addition, it is easy to control the properties of the slurry, there is an advantage that can reduce the variation of the slurry properties in the semiconductor polishing process due to the separate mixing.
이하, 실시예 및 비교예를 들어 본 발명을 보다 자세히 설명할 것이다. 그러나 본 발명이 이로써 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to Examples and Comparative Examples. However, the present invention is not limited thereto.
[실시예1] 피리딘계 화합물과 폴리옥시프로필렌에테르를 첨가한 슬러리 제조 Example 1 Slurry Preparation of Pyridine Compound and Polyoxypropylene Ether
탈이온수 2981.7g에, 평균입경 100nm의 산화세륨 분말 15.0g을 분산시킨 후, 피리딘-2-카르복실산 3g과, 분자량 400의 폴리프로필렌글리콜(PPG) 0.3g을 첨가하여 균일하게 혼합되도록 교반하였다. 그리고, 수산화 칼륨 수용액을 사용하여 슬러리의 pH가 5.5로 되도록 조절하여 CMP슬러리를 제조하였다.After dispersing 15.0 g of cerium oxide powder having an average particle diameter of 100 nm in 2981.7 g of deionized water, 3 g of pyridine-2-carboxylic acid and 0.3 g of polypropylene glycol (PPG) having a molecular weight of 400 were added and stirred to uniformly mix. . Then, the pH of the slurry was adjusted to 5.5 using an aqueous potassium hydroxide solution to prepare a CMP slurry.
[실시예2] 벤조산계 화합물과 폴리옥시프로필렌에테르를 첨가한 슬러리 제조 Example 2 Preparation of Slurry with Addition of a Benzoic Acid Compound and Polyoxypropylene Ether
피리딘-2-카르복실산 3g을 첨가하는 대신에, 3-아미노벤조산 3g을 첨가한 것을 제외하고는 상기 실시예 1과 동일한 방법으로 CMP 슬러리를 제조하였다. A CMP slurry was prepared in the same manner as in Example 1, except that 3 g of 3-aminobenzoic acid was added instead of 3 g of pyridine-2-carboxylic acid.
[실시예 3] 벤조산계 화합물과 폴리옥시프로필렌에테르를 첨가한 슬러리 제조 Example 3 Slurry Preparation with Addition of a Benzoic Acid Compound and Polyoxypropylene Ether
피리딘-2-카르복실산 3g을 첨가하는 대신에, 4-아미노벤조산 3g을 첨가한 것을 제외하고는 상기 실시예 1과 동일한 방법으로 CMP 슬러리를 제조하였다. A CMP slurry was prepared in the same manner as in Example 1, except that 3 g of 4-aminobenzoic acid was added instead of 3 g of pyridine-2-carboxylic acid.
[실시예4] 피리딘계 화합물과 폴리옥시프로필렌에테르를 첨가한 슬러리 제조 Example 4 Slurry Preparation of Pyridine Compound and Polyoxypropylene Ether
분자량 400의 폴리프로필렌글리콜 0.3g을 첨가하는 대신에, 분자량 3000의 폴리프로필렌 글리콜 0.3g을 첨가한 것을 제외하고는 상기 실시예1과 동일한 방법으로 CMP 슬러리를 제조하였다. Instead of adding 0.3 g of polypropylene glycol having a molecular weight of 400, a CMP slurry was prepared in the same manner as in Example 1 except that 0.3 g of polypropylene glycol having a molecular weight of 3000 was added.
[실시예5] 피리딘계 화합물과 폴리옥시에틸렌옥시프로필렌 공중합체를 첨가한 슬러리 제조 Example 5 Slurry Preparation with Pyridine Compound and Polyoxyethyleneoxypropylene Copolymer
분자량 400의 폴리프로필렌글리콜 0.3g을 첨가하는 대신에, 분자량 3100인 폴리옥시에틸렌옥시프로필렌 공중합체 0.3g을 첨가한 것을 제외하고는 상기 실시예1과 동일한 방법으로 CMP 슬러리를 제조하였다. Instead of adding 0.3 g of polypropylene glycol having a molecular weight of 400, a CMP slurry was prepared in the same manner as in Example 1 except that 0.3 g of a polyoxyethylene oxypropylene copolymer having a molecular weight of 3100 was added.
[비교예1] 피리딘계 화합물만 첨가하고 슬러리 제조 Comparative Example 1 Slurry Preparation with Pyridine Compound
분자량 400의 폴리프로필렌글리콜 0.3g을 첨가하지 않은 것을 제외하고는 상기 실시예 1과 동일한 방법으로 CMP 슬러리를 제조하였다. A CMP slurry was prepared in the same manner as in Example 1, except that 0.3 g of polypropylene glycol having a molecular weight of 400 was not added.
[비교예2] 벤조산계 화합물만 첨가하고 슬러리 제조 [Comparative Example 2] Slurry Preparation with Only Benzoic Acid Compound
분자량 400의 폴리프로필렌글리콜 0.3g을 첨가하지 않은 것을 제외하고는 상기 실시예 2와 동일한 방법으로 CMP 슬러리를 제조하였다. A CMP slurry was prepared in the same manner as in Example 2, except that 0.3 g of polypropylene glycol having a molecular weight of 400 was not added.
[비교예3] 벤조산계 화합물만 첨가하고 슬러리 제조 [Comparative Example 3] Slurry Preparation with Only Benzoic Acid Compound
분자량 400의 폴리프로필렌글리콜 0.3g을 첨가하지 않은 것을 제외하고는 상기 실시예 3과 동일한 방법으로 CMP 슬러리를 제조하였다. A CMP slurry was prepared in the same manner as in Example 3, except that 0.3 g of polypropylene glycol having a molecular weight of 400 was not added.
[비교예4] 피리딘계 화합물과 폴리옥시에틸렌옥시프로필렌 공중합체를 첨가한 슬러리 제조 Comparative Example 4 Slurry Preparation of Pyridine Compound and Polyoxyethyleneoxypropylene Copolymer
분자량 400의 폴리프로필렌글리콜 0.3g을 첨가하는 대신에, 분자량 6400인 폴리옥시에틸렌옥시프로필렌 공중합체 0.3g을 첨가한 것을 제외하고는 상기 실시예1과 동일한 방법으로 CMP 슬러리를 제조하였다. Instead of adding 0.3 g of polypropylene glycol having a molecular weight of 400, a CMP slurry was prepared in the same manner as in Example 1 except that 0.3 g of a polyoxyethyleneoxypropylene copolymer having a molecular weight of 6400 was added.
[비교예5] 피리딘계 화합물과 폴리옥시에틸렌알킬에테르를 첨가한 슬러리 제조 Comparative Example 5 Slurry Preparation of Pyridine Compound and Polyoxyethylene Alkyl Ether
분자량 400의 폴리프로필렌글리콜 0.3g을 첨가하는 대신에, 분자량 400인 폴리에틸렌글리콜(PEG) 0.3g을 첨가한 것을 제외하고는 상기 실시예1과 동일한 방법으로 CMP 슬러리를 제조하였다. Instead of adding 0.3 g of polypropylene glycol having a molecular weight of 400, a CMP slurry was prepared in the same manner as in Example 1 except that 0.3 g of polyethylene glycol (PEG) having a molecular weight of 400 was added.
[비교예6] 실리카 슬러리 Comparative Example 6 Silica Slurry
상용의 CMP용 실리카 슬러리(SP4000, 제일모직사)를 준비하였다. A commercially available CMP silica slurry (SP4000, Cheil Industries) was prepared.
[실험예1] 연마성능 및 필터링성능 평가Experimental Example 1 Evaluation of Polishing and Filtering Performance
상기 실시예 및 비교예에서 제조된 CMP슬러리를 이용하여 하기 연마조건에서 1분간 연마하였다. 연마에 의해 제거된 웨이퍼의 두께 변화를 측정하여 연마속도를 산출하였고, 옵티프로브(Optiprobe) 장비를 사용하여 3mm 에지를 제외한 98포인트 분석으로 웨이퍼 연마균일도(Within Wafer Non Uniformity)를 평가하였다. The CMP slurry prepared in Examples and Comparative Examples was used to polish for 1 minute under the following polishing conditions. The polishing rate was calculated by measuring the change in thickness of the wafer removed by polishing, and the wafer wafer uniformity was evaluated by an 98-point analysis excluding 3mm edge using an Optitiprobe device.
<연마조건><Polishing condition>
- 연마기 : AMAT Mirra (AMAT社)-Polishing machine: AMAT Mirra (AMAT Co.)
- 패드 : IC1000 k-groove(Roddel社)-Pad: IC1000 k-groove (Roddel)
- Polishing time : 30 sec.Polishing time: 30 sec.
- Platen rpm : 103 rpmPlaten rpm: 103 rpm
- Head rpm : 97 rpmHead rpm: 97 rpm
- Flow rate : 200 ml/min.Flow rate: 200 ml / min.
- Used wafer: 8인치 SiO2 평탄 웨이퍼(PE-TEOS)-Used wafer: 8 inch SiO 2 flat wafer (PE-TEOS)
- Pressure : 3 psiPressure: 3 psi
또한, 상기 실시예 및 비교예에서 제조된 슬러리를 Pall 사의 0.5㎛ 필터를 사용하여 필터링하였으며, 필터링 전 후의 CMP슬러리 내의 고체함량을 측정하여 다음 식과 같이 필터효율을 산출하였다. 그리고 필터가 시행된 슬러리를 이용하여 연마성능을 평가 하였다.In addition, the slurry prepared in Examples and Comparative Examples was filtered using a 0.5 μm filter manufactured by Pall, and the filter efficiency was calculated by measuring the solids content in the CMP slurry before and after filtering. And the polishing performance was evaluated using the slurry applied filter.
[일반식1][Formula 1]
필터효율 = (필터 후 고체함량) / (필터 전 고체함량)×100 (%) Filter efficiency = (solid content after filter) / (solid content before filter) × 100 (%)
상기 연마성능 시험 및 필터효율 시험 결과를 하기 표1에 나타내었다. The polishing performance test and filter efficiency test results are shown in Table 1 below.
[표 1]TABLE 1
(Å/min.)Silicon Oxide Film Polishing Rate
(Å / min.)
(Å/min.)Silicon Nitride Film Polishing Rate
(Å / min.)
(Mw 400)PPG 0.3g
(Mw 400)
3.0g3-aminobenzoic acid
3.0 g
(Mw 400)PPG 0.3g
(Mw 400)
3.0g4-aminobenzoic acid
3.0 g
(Mw 400)PPG 0.3g
(Mw 400)
(Mw 3000)PPG 0.3g
(Mw 3000)
(Mw 3100)0.3 g of copolymer
(Mw 3100)
3.0g3-aminobenzoic acid
3.0 g
3.0g4-aminobenzoic acid
3.0 g
(Mw 6400)0.3 g of copolymer
(Mw 6400)
(MW 400)PEG 0.3g
(MW 400)
상기 표1에서 나타나듯이, 비교예6(상용의 실리카 슬러리)와 비교하여 실시예1 내지5 및 비교예1 내지5(산화세륨 슬러리)는 모두 산화규소막의 연마속도가 높고, 질화규소막의 연마속도가 낮아 높은 연마선택비를 구현할 수 있음을 알 수 있다.As shown in Table 1, in comparison with Comparative Example 6 (commercial silica slurry), Examples 1 to 5 and Comparative Examples 1 to 5 (cerium oxide slurry) were both high in polishing rate of silicon oxide film and high in polishing rate of silicon nitride film. It can be seen that low polishing selectivity can be achieved.
그러나, 비교예 1 내지 5는 불순물 제거를 위한 필터링 공정시 많은 양의 고형분이 필터를 통과하지 못하여 낮은 필터 효율을 알 수 있다. 이는 산화세륨계 슬러리에서 높은 연마선택비를 구현하기 위하여 첨가하는 피리딘계 화합물 또는 벤조산계 화합물이 슬러리의 분산 안정성을 심각하게 저해하여 연마입자의 응집이 발생시키거나, 피리딘계 화합물 또는 벤조산계 화합물과 금속산화물이 필터의 포어(pore)를 막아서 필터 막힘 현상을 나타내게 하는 것으로 생각된다. However, in Comparative Examples 1 to 5, a large amount of solids did not pass through the filter in the filtering process for removing impurities, thereby indicating low filter efficiency. This is because the pyridine compound or benzoic acid compound added in order to achieve high polishing selectivity in the cerium oxide slurry seriously inhibits the dispersion stability of the slurry, causing agglomeration of abrasive particles, or the pyridine compound or benzoic acid compound. It is believed that the metal oxides block the pores of the filter and cause the filter to become clogged.
이에 반하여, 산화세륨계 슬러리에 피리딘계 화합물 또는 벤조산계 화합물을 첨가하고, 비이온성 화합물로서 폴리옥시프로필렌에테르 또는 폴리옥시에틸렌옥시프로필렌 공중합체를 첨가한 실시예 1 내지 5는 높은 연마선택비를 그대로 유지한 상태에서, 필터 효율을 증가시킴을 알 수 있다. 특히, 실시예 1과 실시예4를 비교하고, 실시예 5와 비교예4를 비교해 보면 분자량이 증가할수록 연마량 및 필터효율이 감소함을 알 수가 있다. In contrast, Examples 1 to 5 in which a pyridine compound or a benzoic acid compound were added to a cerium oxide slurry and a polyoxypropylene ether or a polyoxyethyleneoxypropylene copolymer were added as a nonionic compound had high polishing selectivity. In the maintained state, it can be seen that the filter efficiency is increased. In particular, when Example 1 and Example 4 are compared, and Example 5 and Comparative Example 4 are compared, it can be seen that as the molecular weight increases, the polishing amount and the filter efficiency decrease.
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| KR101406759B1 (en) * | 2012-11-07 | 2014-06-19 | 주식회사 케이씨텍 | Polishing slurry and substrate or wafer polishing method using the same |
| JP2015528036A (en) * | 2012-07-11 | 2015-09-24 | キャボット マイクロエレクトロニクス コーポレイション | Compositions and methods for selective polishing of silicon nitride materials |
| CN109251677A (en) * | 2017-07-13 | 2019-01-22 | 安集微电子科技（上海）股份有限公司 | A kind of chemical mechanical polishing liquid |
| WO2021131434A1 (en) * | 2019-12-24 | 2021-07-01 | ニッタ・デュポン株式会社 | Polishing composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2015528036A (en) * | 2012-07-11 | 2015-09-24 | キャボット マイクロエレクトロニクス コーポレイション | Compositions and methods for selective polishing of silicon nitride materials |
| KR101406759B1 (en) * | 2012-11-07 | 2014-06-19 | 주식회사 케이씨텍 | Polishing slurry and substrate or wafer polishing method using the same |
| CN109251677A (en) * | 2017-07-13 | 2019-01-22 | 安集微电子科技（上海）股份有限公司 | A kind of chemical mechanical polishing liquid |
| CN109251677B (en) * | 2017-07-13 | 2021-08-13 | 安集微电子科技（上海）股份有限公司 | Chemical mechanical polishing solution |
| WO2021131434A1 (en) * | 2019-12-24 | 2021-07-01 | ニッタ・デュポン株式会社 | Polishing composition |
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