KR20030087227A - Slurry for CMP of metal layer - Google Patents
Slurry for CMP of metal layer Download PDFInfo
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- KR20030087227A KR20030087227A KR1020020025199A KR20020025199A KR20030087227A KR 20030087227 A KR20030087227 A KR 20030087227A KR 1020020025199 A KR1020020025199 A KR 1020020025199A KR 20020025199 A KR20020025199 A KR 20020025199A KR 20030087227 A KR20030087227 A KR 20030087227A
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Abstract
Description
본 발명은 반도체 CMP 공정에 사용되는 슬러리에 관한 것으로, 특히 금속막에 대한 CMP 공정에 사용되는 슬러리에 관한 것이다.The present invention relates to a slurry used in a semiconductor CMP process, and more particularly to a slurry used in a CMP process for a metal film.
반도체 소자가 미세화, 고밀도화 및 다층 구조화 됨에 따라 보다 미세한 패턴 형성 기술이 사용되며 반도체 소자의 표면 구조가 복잡해지고 층간 절연막들의 단차도 커지고 있다. 따라서, 반도체 기판 상에 형성된 특정한 막에서의 단차를 제거하기 위한 평탄화 기술로서 대표적으로 화학적 기계적 연마(Chemical Mechanical Polishing, 이하 CMP라 함) 공정이 이용된다. 비아홀을 CVD 방법을 이용하여 텅스텐으로 채울 때, 텅스텐은 비아홀 내부 뿐만 아니라 주위의 절연층 위에도 적층된다. 후속 공정으로 절연층 위에 적층된 텅스텐을 건식 식각으로 제거하고자 할 때, 비아홀 내부에 적층된 텅스텐도 제거되며, 또한 건식 식각후에 텅스텐 막의 입자들이 반도체 기판 상에 남게 되면 치명적인 불량을 야기하는 단점이 있다. 따라서 이러한 단점을 제거하고자 최근에는 텅스텐 비아 형성 후, 절연층 위의 텅스텐을 제거하기 위하여 후속 공정으로 CMP 공정을 진행하기도 한다.As semiconductor devices are miniaturized, densified, and multilayered, finer pattern formation techniques are used, and the surface structure of the semiconductor devices is complicated and the level of interlayer insulating films is also increased. Accordingly, a chemical mechanical polishing (CMP) process is typically used as a planarization technique for removing a step in a specific film formed on a semiconductor substrate. When via holes are filled with tungsten using the CVD method, tungsten is deposited not only in the via holes but also on the surrounding insulating layer. When the tungsten deposited on the insulating layer is to be removed by dry etching in a subsequent process, the tungsten deposited inside the via hole is also removed, and when the particles of the tungsten film remain on the semiconductor substrate after the dry etching, a fatal defect is caused. . Therefore, in order to eliminate this disadvantage, recently, after the formation of tungsten vias, a CMP process may be performed in a subsequent process to remove tungsten on the insulating layer.
CMP 공정이란 웨이퍼 표면을 연마패드와 슬러리를 이용하여 평탄화 시키는방법으로서, 좀 더 구체적으로, 연마패드 및 웨이퍼를 접촉하여 연마패드와 웨이퍼를 회전 및 직선 운동을 혼합한 오비탈 운동을 실시하면서 연마제가 포함된 슬러리를 이용하여 연마하는 공정이다. CMP 공정에 사용되는 슬러리의 구성은 크게 물리적 작용을 하는 연마 입자와 화학적 작용을 하는 에천트(etchant)등의 화합물의 혼합물로 구성되어 있다.The CMP process is a method of planarizing a wafer surface using a polishing pad and a slurry. More specifically, the polishing agent includes an orbital motion in which the polishing pad and the wafer are in contact with each other to perform an orbital motion in which the polishing pad and the wafer are mixed with rotation and linear motion. It is a process of grinding | polishing using the prepared slurry. The slurry used in the CMP process is composed of a mixture of abrasive particles, which have a large physical action, and an etchant, which has a chemical action.
일반적으로 CMP공정에 적용되는 슬러리는 수용성 용액으로 첨가되는 화합물은 연마대상인 금속층을 산화시키는 산화제와 pH 조절제를 첨가하고 필요시 CMP공정에서 요구되는 목적에 적합한 첨가제등을 추가 첨가 하여 제조한다.In general, the slurry used in the CMP process is prepared by adding an oxidizing agent and a pH adjusting agent for oxidizing the metal layer to be polished, and adding an additive suitable for the purpose required in the CMP process if necessary.
상기와 같은 CMP용 슬러리 중에 특히 텅스텐과 같은 금속막을 연마하기위한 슬러리는 금속 에천트로서 질산화 철(Fe(NO3)3)과 과산화 수소(H2O2)등을 함유한다. 하지만, 과산화수소는 슬러리 안의 철이온 같은 메탈 이온들과 반응을 하여 물(H2O)과 산소(O2)로 분해되는 과수분해반응이 진행되며, 슬러리 안의 과산화수소의 농도가 시간이 지남에 따라 감소하게 된다. 이러한 이유로, 금속막을 CMP 처리할 때마다, 매번 과산화수소를 슬러리에 첨가해야하는 번거로움이 있다.In such a slurry for CMP, a slurry for polishing a metal film such as tungsten contains iron nitride (Fe (NO 3 ) 3 ), hydrogen peroxide (H 2 O 2 ), or the like as a metal etchant. However, hydrogen peroxide reacts with metal ions such as iron ions in the slurry to decompose into water (H 2 O) and oxygen (O 2 ), and the concentration of hydrogen peroxide in the slurry decreases over time. Done. For this reason, it is troublesome to add hydrogen peroxide to the slurry every time the metal film is subjected to CMP treatment.
따라서, 상기 문제를 해결하기 위하여, 본 발명의 기술적 과제는 과산화수소를 함유하는 슬러리에서 과산화수소의 분해 반응을 억제할 수 있는 CMP용 슬러리를 제공하는데 있다.Accordingly, in order to solve the above problem, the technical problem of the present invention is to provide a slurry for CMP that can suppress the decomposition reaction of hydrogen peroxide in the slurry containing hydrogen peroxide.
상기 기술적 과제를 해결하기 위하여, 본 발명에 따른 과산화수소를 함유하는 슬러리에는 과수분해억제제가 첨가되는 것을 특징으로 한다.In order to solve the above technical problem, a perhydrolysis inhibitor is added to the slurry containing hydrogen peroxide according to the present invention.
과수분해억제제로서 인화합물을 사용하며, 본 발명의 일 실시예에 따르면, 무기 인화합물로는 H3PO4를 사용하며, 또 다른 실시예에 따르면, 유기 인화합물로는 아미노 트리(메틸렌-포스포닉 산)(Amino tri(metylene-phosphonic acid))을 사용한다.A phosphorus compound is used as a perhydrolysis inhibitor, and according to one embodiment of the present invention, H 3 PO 4 is used as the inorganic phosphorus compound, and according to another embodiment, amino tri (methylene-force) Phonic acid) (Amino tri (metylene-phosphonic acid)) is used.
좀 더 구체적으로, 본 발명은 탈이온수(Deionized water), 연마제, 과산화수소, 질산화철, 및 과수분해억제제로 이루어지는 슬러리를 제공한다. 여기서 과산화수소와 질산화철은 산화제로 쓰인다. 상기 슬러리에는 산화제로서 질산 또는 황산등이 더 첨가될 수 있다. 상기 연마제는 실리카, 알루미나, 세리아, 및 티타니아 중에서 하나 선택되는 물질로 이루어며 슬러리의 총 중량을 기준으로 3~25중량%의 양으로 첨가되며 바람직하게는 3~10중량%의 양으로 첨가된다. 상기 과수분해억제제는 인산(H3PO4)일 수 있으며, 전체 슬러리의 총 중량을 기준으로 10~5000ppm의 양으로 첨가될 수 있으며 바람직하게는 50~500ppm의 양으로 첨가될 수 있다. 또는 상기 과수분해억제제는 아미노 트리(메틸렌-포스포닉 산)(Amino tri(methylene-phosphonic acid))일 수 있으며, 전체 슬러리의 총 중량을 기준으로 10~5000ppm의 양으로 첨가될 수 있으며 바람직하게는 50~500ppm의 양으로 첨가될 수 있다. 또는 상기 과수분해억제제는 펜타소디움염(Pentasodium salt), 1-하이드록시에틸렌-1,1-디포스포닉(1-Hydroxyethylene 1,1-Diphosphonic) 산(acid) 또는 그것의 염(salt),에틸렌 디아민 테트라(메틸렌 포스포닉 산)(Ethylene diamine tetra(methylene phosphonic acid)) 또는 그것의 염, 헥사메틸렌디아민 테트라(메틸렌 포스포닉 산)(Hexamethylenediamine tetra(methylene phosphonic acid)) 또는 그것의 염, 디에틸렌트리아민 펜타(메틸렌 포스포닉 산)(Diethylenetriamine penta(methylene phosphonic acid)) 또는 그것의 염에서 하나 선택되는 물질로 이루어질 수 있다. 상기 슬러리에는 분산성(장기 저장 안정성)을 위해 폴리(포타슘 아크릴레이트)(Poly(potassium acrylate))가 더 첨가될 수 있다. 상기 슬러리에는 pH 조절제가 더 첨가될 수 있으며, 상기 pH 조절제로서 황산, 인산, 질산, 수산화칼륨, 암모니아수 중에서 하나 선택되는 물질이 사용될 수 있다. 상기 슬러리에는 과산화수소 안정을 위해, 구연산(Citric acid)이 더 첨가될 수 있다. 본 발명에 따른 슬러리는 금속막 CMP용으로써, 텅스텐, 구리, 및 알루미늄등의 금속막 연마에 사용된다.More specifically, the present invention provides a slurry consisting of deionized water, an abrasive, hydrogen peroxide, iron nitrate, and a perhydrolysis inhibitor. Hydrogen peroxide and iron nitrate are used as oxidants. Nitric acid or sulfuric acid may be further added to the slurry as an oxidizing agent. The abrasive is composed of a material selected from silica, alumina, ceria, and titania, and is added in an amount of 3 to 25% by weight based on the total weight of the slurry, and preferably in an amount of 3 to 10% by weight. The perhydrolysis inhibitor may be phosphoric acid (H 3 PO 4 ), may be added in an amount of 10 to 5000ppm based on the total weight of the total slurry, preferably in an amount of 50 to 500ppm. Alternatively, the perhydrolysis inhibitor may be amino tri (methylene-phosphonic acid), and may be added in an amount of 10 to 5000 ppm based on the total weight of the entire slurry, and preferably It may be added in an amount of 50 to 500 ppm. Or the perhydrolysis inhibitor is pentasodium salt, 1-hydroxyethylene-1,1-diphosphonic acid or salt thereof, ethylene Ethylene diamine tetra (methylene phosphonic acid) or salts thereof, hexamethylenediamine tetra (methylene phosphonic acid) or salts thereof, diethylene tree It can be made of a material selected from amine penta (methylene phosphonic acid) (diethylenetriamine penta (methylene phosphonic acid)) or a salt thereof. The slurry may be further added with poly (potassium acrylate) for dispersibility (long term storage stability). A pH regulator may be further added to the slurry, and a substance selected from sulfuric acid, phosphoric acid, nitric acid, potassium hydroxide, and ammonia water may be used as the pH regulator. Citric acid may be further added to the slurry to stabilize hydrogen peroxide. The slurry according to the present invention is for metal film CMP and is used for polishing metal films such as tungsten, copper, and aluminum.
본 발명에 관한 보다 상세한 내용은 다음의 구체적인 실험예를 통하여 설명하되, 여기에 기재되지 않은 내용은 이 기술분야에서 숙련된 자이면 충분히 기술적으로 유추할 수 있는 것이므로 설명을 생략한다. 하기 실험예들은 예시적 의미를 지니며 본 발명의 보호 범위를 제한한 것은 아니다.More detailed information about the present invention will be described through the following specific experimental examples, but the information not described herein will be omitted because it is sufficiently technically inferred by those skilled in the art. The following examples have exemplary meanings and do not limit the protection scope of the present invention.
<실험예1>Experimental Example 1
슬러리에 첨가되는 과수분해억제제인 인화합물중 무기화합물인 인산(H3PO4)의 첨가량에 따른 슬러리의 특성 변화를 평가하기 위하여 4개의 샘플 슬러리를 제조하였다. 슬러리는 탈이온수(Deionized water), 질산화철, 구연산 및 pH조절제등을 연마제와 혼합하고 2중량%의 과산화수소를 첨가하였다. 과수분해억제제로 인산을 첨가하는데, 전체 중량을 기준으로 0, 10, 100, 및 500ppm으로 첨하하여 슬러리 샘플 4개를 만들었다. 시료 웨이퍼는 텅스텐 피복 웨이퍼로 폴리실리콘 기판 상에 HTO막를 1000Å으로 데포하고 그 위에 Ti/TiN막들을 각각 100/400Å으로 데포한 후, 텅스텐을 4000Å으로 증착하여 제조하였다. 연마 조건은 하중 압력은 6psi, 테이블 회전 속도 45rpm, 스핀들 속도는 35rpm, 슬러리 유량은 250ml/min로 하였다. 각 슬러리별 평가 결과는 하기의 표1에 나타내었다.Four sample slurries were prepared to evaluate the change in the properties of the slurry according to the amount of the phosphoric acid (H 3 PO 4 ), which is an inorganic compound, of the phosphorus compound which is a hydrolysis inhibitor added to the slurry. The slurry was mixed with deionized water, iron nitrate, citric acid, pH adjuster and the like, and 2% by weight of hydrogen peroxide was added. Phosphoric acid was added as a perhydrolysis inhibitor, added to 0, 10, 100, and 500 ppm based on the total weight to make four slurry samples. The sample wafer was prepared by depositing a HTO film at 1000 mW on a polysilicon substrate with a tungsten coated wafer, Ti / TiN films at 100/400 mW respectively, and depositing tungsten at 4000 mW. The polishing conditions were load pressure of 6 psi, table rotational speed of 45 rpm, spindle speed of 35 rpm, and slurry flow rate of 250 ml / min. Evaluation results for each slurry are shown in Table 1 below.
상기 표1의 결과에서와 같이 인산의 첨가 농도에 따른 특성 평가를 진행한 결과, 제조직후에는 인산 첨가 농도가 증가할수록 텅스텐 막의 연마속도는 감소하였지만, 3일 후에는 증가된 것을 알 수 있다. 이는 첨가된 인산의 양이 증가할 수록 과산화수소의 과수분해 반응이 억제됨을 알 수 있다. 슬러리의 연마속도의 감소율은 인산을 500ppm첨가시, 인산을 전혀 첨가하지 않은 샘플에 비해, 82%에서 45%로로 크게 감소되는 결과를 보였다. 따라서, 슬러리의 연마속도의 재현성이 현저히 개선됨을 알 수 있다.As a result of evaluating the characteristics according to the concentration of phosphoric acid as shown in the results of Table 1, it was found that the polishing rate of the tungsten film was decreased as the concentration of phosphoric acid was added immediately after manufacture, but increased after 3 days. It can be seen that as the amount of added phosphoric acid increases, the perhydrolysis reaction of hydrogen peroxide is suppressed. The reduction rate of the slurry was greatly reduced from 82% to 45% when 500 ppm of phosphoric acid was added, compared to the sample without adding any phosphoric acid. Thus, it can be seen that the reproducibility of the polishing rate of the slurry is significantly improved.
<실험예 2>Experimental Example 2
슬러리에 첨가되는 과수분해억제제인 인화합물중 무기화합물인 인산(H3PO4)의 첨가량에 따른 슬러리의 특성 변화를 평가하기 위하여 4개의 샘플 슬러리를 제조하였다. 슬러리는 탈이온수(Deionized water), 질산화철, 구연산 및 pH조절제등을 연마제와 혼합하고 2중량%의 과산화수소를 첨가하였다. 과수분해억제제로 아미노 트리(메틸렌 포스포닉 산)을 첨가하는데, 전체 중량을 기준으로 0, 10, 100, 및 500ppm으로 첨하하여 슬러리 샘플 4개를 만들었다. 시료 웨이퍼는 텅스텐 피복 웨이퍼로 실리콘 기판 상에 HTO막를 1000Å으로 데포하고 그 위에 Ti/TiN막들을 각각 100/400Å으로 데포한 후, 텅스텐을 4000Å으로 증착하여 제조하였다. 연마 조건은 하중 압력은 6psi, 테이블 회전 속도 45rpm, 스핀들 속도는 35rpm, 슬러리 유량은 250ml/min로 하였다. 각 슬러리별 평가 결과는 하기의 표2에 나타내었다.Four sample slurries were prepared to evaluate the change in the properties of the slurry according to the amount of the phosphoric acid (H 3 PO 4 ), which is an inorganic compound, of the phosphorus compound which is a hydrolysis inhibitor added to the slurry. The slurry was mixed with deionized water, iron nitrate, citric acid, pH adjuster and the like, and 2% by weight of hydrogen peroxide was added. Amino tri (methylene phosphonic acid) was added as a perhydrolysis inhibitor, adding 4, 0, 10, 100, and 500 ppm based on the total weight to make 4 slurry samples. The sample wafer was prepared by depositing a HTO film at 1000 mW on a silicon substrate with a tungsten coated wafer and Ti / TiN films at 100/400 mW respectively, and depositing tungsten at 4000 mW. The polishing conditions were load pressure of 6 psi, table rotational speed of 45 rpm, spindle speed of 35 rpm, and slurry flow rate of 250 ml / min. Evaluation results for each slurry are shown in Table 2 below.
상기 표2의 결과에서와 같이 아미노 트리(메틸렌 포스포닉 산)의 첨가 농도에 따른 특성 평가를 진행한 결과, 인산을 첨가했을 때보다 연마속도의 재현성이 크게 개선됨을 알 수 있다. 즉, 슬러리의 연마속도의 감소율은 아미노 트리(메틸렌 포스포닉 산)을 500ppm첨가시, 전혀 첨가하지 않은 샘플에 비해, 82%에서 16%로로 더욱 크게 감소되는 결과를 보였다. 따라서, 슬러리의 연마속도의 재현성이 현저히개선됨을 알 수 있다.As a result of Table 2, as a result of the evaluation of the properties according to the addition concentration of amino tri (methylene phosphonic acid), it can be seen that the reproducibility of the polishing rate is significantly improved than when adding the phosphoric acid. That is, the rate of reduction of the polishing rate of the slurry was further reduced from 82% to 16% compared to the sample without adding any amino tri (methylene phosphonic acid) at 500 ppm. Therefore, it can be seen that the reproducibility of the polishing rate of the slurry is significantly improved.
이상에서 설명한 본 발명은 상술한 실험예에 의해 한정되는 것이 아니고, 본 발명의 기술적 사상을 벗어나지 않는 범위 내에서 여러 가지 치환, 변형 및 변경이 가능하다는 것이 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자에게 있어 명백할 것이다.The present invention described above is not limited to the above-described experimental example, and various substitutions, modifications, and changes can be made without departing from the technical spirit of the present invention. It will be clear to those who have it.
본 발명에 따르면, 금속막을 연마하기 위한 CMP 슬러리에 과산화수소를 첨가할 때, 인화합물 계통의 과수분해억제제를 첨가하여, 과산화수소의 과수분해 반응을 억제할 수 있으며, 그에 따라, 과산화수소의 농도를 일정시간 유지시킴으로써 지속적인 연마속도를 갖는 슬러리를 제조할 수 있다.According to the present invention, when the hydrogen peroxide is added to the CMP slurry for polishing the metal film, the perhydrolysis inhibitor of the phosphorus compound system can be added to suppress the perhydrolysis reaction of the hydrogen peroxide, whereby the concentration of the hydrogen peroxide is constant for a certain time. By maintaining it, a slurry having a sustained polishing rate can be produced.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2007048314A1 (en) * | 2005-10-28 | 2007-05-03 | Anji Microelectronics (Shanghai) Co., Ltd | A chemical mechanical polishing paste for copper |
| WO2007048313A1 (en) * | 2005-10-28 | 2007-05-03 | Anji Microelectronics (Shanghai) Co., Ltd | A chemical mechanical polishing paste for barrier layer |
| KR100725550B1 (en) * | 2005-01-20 | 2007-06-08 | 제일모직주식회사 | Slurry composition for copper wiring polishing and metal wiring polishing method using the same |
| KR101539765B1 (en) * | 2008-09-02 | 2015-07-28 | 동우 화인켐 주식회사 | Method for manufacturing array substrate for liquid crystal display |
| KR101723981B1 (en) | 2016-06-21 | 2017-04-07 | (주)세미로드 | Apparatus for measuring and adjusting concentration of the slurry solution |
| KR101868771B1 (en) | 2018-03-22 | 2018-07-17 | 성락규 | Solution for Detecting Concentration of CMP Slurry and Preparation thereof |
| KR20180091945A (en) * | 2016-01-06 | 2018-08-16 | 캐보트 마이크로일렉트로닉스 코포레이션 | Tungsten-treated slurry containing catalyst |
| KR20210047082A (en) | 2019-10-21 | 2021-04-29 | 성락규 | Standard solution for detecting hydrogen peroxide, detection method for measuring the concentration of hydrogen peroxide using it and automatic control method of concentration of hydrogen peroxide |
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2002
- 2002-05-08 KR KR1020020025199A patent/KR20030087227A/en not_active Withdrawn
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100725550B1 (en) * | 2005-01-20 | 2007-06-08 | 제일모직주식회사 | Slurry composition for copper wiring polishing and metal wiring polishing method using the same |
| WO2007048314A1 (en) * | 2005-10-28 | 2007-05-03 | Anji Microelectronics (Shanghai) Co., Ltd | A chemical mechanical polishing paste for copper |
| WO2007048313A1 (en) * | 2005-10-28 | 2007-05-03 | Anji Microelectronics (Shanghai) Co., Ltd | A chemical mechanical polishing paste for barrier layer |
| CN1955212B (en) * | 2005-10-28 | 2011-08-03 | 安集微电子（上海）有限公司 | Chemical mechanical polishing material for barrier layer |
| KR101539765B1 (en) * | 2008-09-02 | 2015-07-28 | 동우 화인켐 주식회사 | Method for manufacturing array substrate for liquid crystal display |
| KR20180091945A (en) * | 2016-01-06 | 2018-08-16 | 캐보트 마이크로일렉트로닉스 코포레이션 | Tungsten-treated slurry containing catalyst |
| JP2019508525A (en) * | 2016-01-06 | 2019-03-28 | 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 | Tungsten-treated slurry containing catalyst |
| EP3400267A4 (en) * | 2016-01-06 | 2019-09-25 | Cabot Microelectronics Corporation | TUNGSTEN TREATMENT SLURRY CONTAINING A CATALYST |
| KR101723981B1 (en) | 2016-06-21 | 2017-04-07 | (주)세미로드 | Apparatus for measuring and adjusting concentration of the slurry solution |
| KR101868771B1 (en) | 2018-03-22 | 2018-07-17 | 성락규 | Solution for Detecting Concentration of CMP Slurry and Preparation thereof |
| KR20210047082A (en) | 2019-10-21 | 2021-04-29 | 성락규 | Standard solution for detecting hydrogen peroxide, detection method for measuring the concentration of hydrogen peroxide using it and automatic control method of concentration of hydrogen peroxide |
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