WO1999067056A1 - Composition destinee au polissage chimio-mecanique de couches metalliques - Google Patents

Composition destinee au polissage chimio-mecanique de couches metalliques Download PDF

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Publication number
WO1999067056A1
WO1999067056A1 PCT/US1999/013709 US9913709W WO9967056A1 WO 1999067056 A1 WO1999067056 A1 WO 1999067056A1 US 9913709 W US9913709 W US 9913709W WO 9967056 A1 WO9967056 A1 WO 9967056A1
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WIPO (PCT)
Prior art keywords
composition
acid
fluoride
potassium
abrasive
Prior art date
Application number
PCT/US1999/013709
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English (en)
Inventor
Brian Mravic
Anthony Mark Pasqualoni
Deepak Mahulikar
Thomas P. Madelung
Original Assignee
Arch Specialty Chemicals, Inc.
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Arch Specialty Chemicals, Inc. filed Critical Arch Specialty Chemicals, Inc.
Publication of WO1999067056A1 publication Critical patent/WO1999067056A1/fr

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Classifications

    • 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
    • C09G1/02—Polishing compositions containing abrasives or grinding agents
    • 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
    • C23F3/00—Brightening metals by chemical means
    • 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 potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table 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
    • H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
    • H01L21/321—After treatment
    • H01L21/32115—Planarisation
    • H01L21/3212—Planarisation by chemical mechanical polishing [CMP]

Definitions

  • the present invention relates to the field of semiconductor integrated circuit manufacturing, and more particular to improved compositions for chemical mechanical polishing (CMP).
  • CMP chemical mechanical polishing
  • barrier layers are interposed between the copper and the underlying silicon or the underlying dielectric which is often silicon oxide.
  • a favored barrier material in the industry is tantalum or tantalum nitride.
  • alternating layers of metal and dielectric are put on the silicon wafer by a variety of processes. After each layer is applied, a means is used to remove excess amounts of the layer and to assure both local and global planarity of the surface in preparation for the application of the next layer.
  • CMP chemical mechanical planarization or chemical mechanical polishing
  • the chemical action is generally considered to take one of two forms.
  • the chemicals in the solution react with the metal layer to continuously form an oxide layer on the surface of the metal.
  • This generally requires the addition of an oxidizer to the solution such as hydrogen peroxide, ferric nitrate, etc.
  • an oxidizer to the solution such as hydrogen peroxide, ferric nitrate, etc.
  • the mechanical abrasive action of the particles continuously and simultaneously removes this oxide layer.
  • Optimum results in terms of removal rate and polished surface quality are obtained by a judicious balance of these two processes.
  • Typical copper CMP slurries contain one or more carboxylic acids to lower the pH to below 7, and the abrasive particles used are typically alumina, silica, ceria or mixtures thereof.
  • both the metal layer itself and its associated barrier layer or layers must be removed, leaving only the desired horizontal and vertical metal interconnects.
  • typical copper polishing slurries do not effectively remove the tantalum barrier layer at an acceptable rate.
  • the Ta barrier layer it typically many times thinner than the copper layer, in order for it to be removed in an economically viable polishing time, the removal rate of the polishing system for the barrier layer need only be a fraction of that of the removal rate of the copper layer. The economically viable rate is defined by the fabricator of the wafers.
  • tantalum exhibits the most stable passivity among known metals. This means that it is quite difficult to find a polishing solution that will overcome this passivity, which is due to the formation of a protective tantalum oxide film on the surface.
  • tantalum is resistant to attack by oxidizing metal chlorides, caustic alkali solutions, all the common inorganic acids and mixtures thereof such as aqua regia, as well as carboxylic acids which are used in copper polishing slurries (see, for example, H.H. Uhlig, "Corrosion and Corrosion Control", John Wiley & Sons, 1967, pp 327-328 and M. Pourbaix, "Atlas of Electrochemical Equilibria in Aqueous Solutions", Pergamon Press, 1966, pp 251- 255).
  • the reference by Uhlig indicates that Ta is attacked by hydrofluoric acid and fluorides in trace amounts.
  • the reference by Pourbaix indicates that tantalum pentoxide (the passivating oxide) can be attacked by concentrated hydrofluoric acid.
  • a polishing solution In order for a polishing solution to be commercially viable, however, it must not corrosively attack the polishing equipment which includes polishing machine parts and polishing pad. This essentially eliminates the possibility of using concentrated hydrofluoric acid as a CMP solution for tantalum.
  • the present invention describes a slurry composition for CMP and a method for using the same.
  • the chemical mechanical polishing slurry composition comprises:
  • a fluorine-containing compound e.g., fluoride-ion containing compound
  • an oxidizer and a carboxylic acid can be used as additives in the slurry composition.
  • the resulting slurry is especially useful for the polishing of tantalum and copper layers on a substrate.
  • Fig. 1 is a graph plotting Ta CMP removal rate versus NH 4 F concentration
  • Fig. 2 is a graph plotting the effect of ammonium fluoride on copper CMP. DETAILED DESCRIPTION OF THE INVENTION
  • the present invention consists of adding fluoride ions to a polishing solution to enhance the removal rate of metal layers on integrated circuit silicon wafers during CMP.
  • One advantage of this approach is that it is effective at pH values above 2 where corrosive attack of the polishing equipment is not a problem. All of the examples below used ammonium fluoride as the source of fluoride ions, but other fluorides could be used as well.
  • An advantage of the present invention is that the addition of fluoride ions to certain copper polishing solutions does not seriously degrade the copper polishing performance of the solution. Therefore, the potential exists of having one polishing solution, either a slurry containing suspended abrasive particles or a solution for use with a pad which has the abrasive particles incorporated within it, that would effectively polish both the copper layer and its underlying tantalum barrier layer.
  • the present invention is particularly directed to a chemical mechanical polishing slurry composition
  • a chemical mechanical polishing slurry composition comprising: (a) a fluorine-containing compound; (b) an abrasive; and (c) water.
  • the fluorine-containing compound is at least one compound selected from the group consisting of: an acid fluoride; a fluorinated salt; and a polyammonium fluoride salt.
  • the fluorine-containing compound is at least one compound selected from the group consisting of: hydrogen fluoride, perfluoric acid, alkali metal fluoride salt, alkaline earth metal fluoride salt, ammonium fluoride, tetramethylammonium fluoride, ammonium bifluoride, ethylenediammonium difluoride diethylenetriammonium trifluoride and mixtures thereof.
  • the fluorine-containing compound is ammonium fluoride.
  • composition according to the present invention may further comprise a carboxylic acid.
  • suitable carboxylic acids are: formic acid, acetic acid, propanoic acid, butanoic acid, pentanoic acid, hexanoic acid, heptanoic acid, octanoic acid, nonanoic acid and mixtures thereof.
  • the composition may also include an oxidizer.
  • oxidizers are hydrogen peroxide, potassium ferricyanide, potassium dichromate, potassium iodate, potassium bromate, vanadium trioxide, hypochlorous acid, sodium hypochlorite, potassium hypochlorite, calcium hypochlorite, magnesium hypochlorite, ferric nitrate, and mixtures thereof.
  • Suitable oxidizers are ammonium persulfate, ammonium nitrate, potassium nitrate, potassium permanganate, ammonium hydroxide and mixtures thereof.
  • the pH of the composition is preferably between about 2 to 9, more preferably 2 to 7, and most preferably 3 to 4.
  • the composition typically comprises between 0.01 to 2.0 molar fluoride ions, more preferably 0.14 to 0.41 molar fluoride ions, and most preferably 0.20 to 0.35 molar fluoride ions.
  • the abrasive is typically at least one abrasive selected from the group consisting of: silica, alumina, silicon carbide, silicon nitride, iron oxide, ceria and mixtures thereof.
  • the composition typically comprises about 0.1 to 25% abrasive by weight.
  • the present invention also comprises a method for polishing which includes the steps of:
  • composition comprises a fluorine-containing compound, an abrasive and water to a substrate;
  • the abrasive is incorporated directly into the polishing pad.
  • Example 1 shows the effectiveness of fluoride ions in the CMP of tantalum. The results are summarized in Table 1 and Fig. 1. Aqueous solutions with different concentrations of ammonium fluoride were used to polish tantalum wafers with a diameter of 4 inches using a Struers RotoPol-3 laboratory polishing machine, a Rodel IC 1000 perforated pad, a pressure of 3.8 psi, a relative velocity between the pad and wafer of 236 feet per minute, and a solution flow rate of 40 ml/min. The abrasive particles were Ludox AM colloidal silica at a concentration of 5 weight percent. No oxidizer was used in the slurry. Small amounts of propanoic acid were added to assure that the pH remained in the range of 6.8-7.2.
  • this slurry is effective for tantalum in a concentration range of about 0.5 weight percent to at least 1.25 weight percent ammonium fluoride. This corresponds to a molar concentration of fluoride ions of from 0.14 to 0.38 moles per liter. The optimum is about 1 wt.% or 0.27 molar fluoride ion concentration.
  • the solution with 1 weight percent ammonium fluoride was used for polishing with no abrasive particles present.
  • the removal rate due to chemical action alone was 8 nm/min.
  • the first data point in Table 1 shows that mechanical action without the presence of ammonium fluoride results in a removal rate of essentially zero.
  • the removal rate was 112 nm/min.
  • Example 3 shows that this basic chemistry provides an acceptable tantalum removal rate when the abrasive particles are incorporated into the polishing pad rather than suspended in the solution as in the following.
  • the abrasive particles in this case were alumina rather than the colloidal silica particles in the examples previously cited.
  • a 1 weight percent ammonium fluoride aqueous solution with a pH of 7.1 was used to polish a tantalum wafer at a pressure of 8.9 psi. and a relative velocity of 236 ft/min.
  • the average removal rate was 70 nm min. This is somewhat less than the 112 nm/min. obtained at the same NH 4 F concentration in Table 1 and required a higher pressure.
  • polishing performance of the abrasive-impregnated pad has been found to be highly dependent on the resilience of the backing used for the pad. Therefore, this example merely shows that the same basic chemistry works effectively regardless of whether the particles are suspended in the solution or embedded in the polishing pad.
  • Example 4 shows the effectiveness of the basic chemistry used to polish copper wafers. The results are shown in Table 3 and Fig. 2. The polishing pressures and relative velocities were the same as in Table 1. However, in the present slurries, the concentration of colloidal silica was only 2.5 weight percent instead of 5 weight percent. In addition, an oxidizer content of 6.5 volume percent hydrogen peroxide was used to enhance the copper polishing rate.
  • Table 3 and Fig. 2 show that the addition of ammonium fluoride to a slurry does not significantly degrade the polishing rate of copper. In fact, the polishing rate is enhanced by ammonium fluoride additions. This is similar to the effect observed in the tantalum examples discussed above. For comparison, the removal rate of a fluoride-free commercial slurry from Rodel was found to be about 1120 nm/min under identical polishing conditions.
  • Example 5 This example shows the beneficial effect of fluoride ions on the CMP of tungsten.
  • the results are summarized in Table 4 below.
  • the polishing slurries contained 4.7 weight percent fumed silica from Wacker, a hydrogen peroxide concentration of 7 volume percent and were polished at a pressure of 7.6 psi and a relative velocity of 236 fpm.
  • the pH was 4.7 to 5.0. Adding the ammonium fluoride essentially tripled the removal rate.
  • polishing slurries to be commercially viable they must meet two other criteria besides having an adequate removal rate and leaving an acceptable surface finish. These are that the polishing rate of silica must be acceptably low and that the static etch rate (the removal rate when no pressure or relative velocity is applied and no particles are present ) of both silica and the metal in the solution must be acceptably low.
  • the static etch rate of copper in a 0.9 M propanoic acid solution with a pH of 3.9 , a hydrogen peroxide concentration of 7.5 volume percent and 1 weight percent ammonium fluoride was 35 nm/min. This is about 17 times lower than the polishing rate for such a solution that contains 2.5 weight percent colloidal silica.
  • the static etch rate of tungsten in solutions with a pH of 3.5 to 4, 7.5 volume percent hydrogen peroxide and up to 2 weight percent ammonium fluoride was less than 10 nm/min.
  • solutions containing 0.9 molar propanoic acid with a pH of about 3.5 and 6.5 to 7.5 volume percent hydrogen peroxide show a static etch rate of essentially zero in solutions containing up to 1 weight percent ammonium fluoride.
  • the polishing rate varied from about 7 nm/min to about 14 nm/min at 3.8 psi pressure and 236 ft./min. relative velocity.
  • aqueous solutions containing abrasive particles either suspended in the solution or incorporated in the polishing pad and up to about 0.6 moles per liter of fluoride ion, at pH values in the range of 2 to 7, are effective in the chemical mechanical polishing of tantalum, copper and tungsten.
  • the optimum fluoride concentration is about 0.27 molar.
  • propanoic acid enhances the polishing rate of these metals in such solutions.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
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  • Metallurgy (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
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  • Mechanical Treatment Of Semiconductor (AREA)

Abstract

La présente invention concerne une composition de polissage chimio-mécanique et un procédé d'utilisation de cette dernière, laquelle composition forme une pâte de polissage chimio-mécanique comprenant: un composé contenant du fluor, un abrasif et de l'eau. On peut facultativement utiliser un oxydant et un acide carboxylique comme additifs ajoutés à la pâte. On obtient une pâte particulièrement utile pour le polissage chimio-mécanique des couches de tantale et de cuivre recouvrant un substrat.
PCT/US1999/013709 1998-06-23 1999-06-17 Composition destinee au polissage chimio-mecanique de couches metalliques WO1999067056A1 (fr)

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US9031998P 1998-06-23 1998-06-23
US60/090,319 1998-06-23

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Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1217651A1 (fr) * 2000-12-20 2002-06-26 Bayer Ag Suspension de polissage chimiomécanique acide pour le polissage des couches de SiO2 isolantes
EP1323798A1 (fr) * 2001-12-27 2003-07-02 Bayer Aktiengesellschaft Compositions pour le polissage chimico-mécanique de structures métalliques et métallo-diélectriques
KR100396881B1 (ko) * 2000-10-16 2003-09-02 삼성전자주식회사 웨이퍼 연마에 이용되는 슬러리 및 이를 이용한 화학기계적 연마 방법
US7018560B2 (en) 2003-08-05 2006-03-28 Rohm And Haas Electronic Materials Cmp Holdings, Inc. Composition for polishing semiconductor layers
US7132058B2 (en) 2002-01-24 2006-11-07 Rohm And Haas Electronic Materials Cmp Holdings, Inc. Tungsten polishing solution
WO2006028759A3 (fr) * 2004-09-08 2006-12-21 Praxair Technology Inc Suspension aqueuse contenant des particules de silice modifiees par l'incorporation de metallate
US7253111B2 (en) 2004-04-21 2007-08-07 Rohm And Haas Electronic Materials Cmp Holding, Inc. Barrier polishing solution
WO2010025623A1 (fr) * 2008-09-05 2010-03-11 安集微电子科技(上海)有限公司 Liquide de polissage chimico-mécanique
US20140017891A1 (en) * 2008-12-10 2014-01-16 Novellus Systems, Inc. Method for depositing tungsten film having low resistivity, low roughness and high reflectivity
US9548228B2 (en) 2009-08-04 2017-01-17 Lam Research Corporation Void free tungsten fill in different sized features
US9653353B2 (en) 2009-08-04 2017-05-16 Novellus Systems, Inc. Tungsten feature fill
US9972504B2 (en) 2015-08-07 2018-05-15 Lam Research Corporation Atomic layer etching of tungsten for enhanced tungsten deposition fill
US9978610B2 (en) 2015-08-21 2018-05-22 Lam Research Corporation Pulsing RF power in etch process to enhance tungsten gapfill performance
US10256142B2 (en) 2009-08-04 2019-04-09 Novellus Systems, Inc. Tungsten feature fill with nucleation inhibition
US10566211B2 (en) 2016-08-30 2020-02-18 Lam Research Corporation Continuous and pulsed RF plasma for etching metals
US10982114B2 (en) 2017-10-25 2021-04-20 Saint-Gobain Ceramics & Plastics, Inc. Composition for conducting material removal operations and method for forming same

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5516346A (en) * 1993-11-03 1996-05-14 Intel Corporation Slurries for chemical mechanical polishing
US5700383A (en) * 1995-12-21 1997-12-23 Intel Corporation Slurries and methods for chemical mechanical polish of aluminum and titanium aluminide
US5934980A (en) * 1997-06-09 1999-08-10 Micron Technology, Inc. Method of chemical mechanical polishing

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5516346A (en) * 1993-11-03 1996-05-14 Intel Corporation Slurries for chemical mechanical polishing
US5836806A (en) * 1993-11-03 1998-11-17 Intel Corporation Slurries for chemical mechanical polishing
US5700383A (en) * 1995-12-21 1997-12-23 Intel Corporation Slurries and methods for chemical mechanical polish of aluminum and titanium aluminide
US5934980A (en) * 1997-06-09 1999-08-10 Micron Technology, Inc. Method of chemical mechanical polishing

Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100396881B1 (ko) * 2000-10-16 2003-09-02 삼성전자주식회사 웨이퍼 연마에 이용되는 슬러리 및 이를 이용한 화학기계적 연마 방법
SG109480A1 (en) * 2000-12-20 2005-03-30 Bayer Ag Acidic polishing slurry for the chemical-mechanical polishing of sio2 isolation layers
EP1217651A1 (fr) * 2000-12-20 2002-06-26 Bayer Ag Suspension de polissage chimiomécanique acide pour le polissage des couches de SiO2 isolantes
EP1323798A1 (fr) * 2001-12-27 2003-07-02 Bayer Aktiengesellschaft Compositions pour le polissage chimico-mécanique de structures métalliques et métallo-diélectriques
US7132058B2 (en) 2002-01-24 2006-11-07 Rohm And Haas Electronic Materials Cmp Holdings, Inc. Tungsten polishing solution
US7018560B2 (en) 2003-08-05 2006-03-28 Rohm And Haas Electronic Materials Cmp Holdings, Inc. Composition for polishing semiconductor layers
US7253111B2 (en) 2004-04-21 2007-08-07 Rohm And Haas Electronic Materials Cmp Holding, Inc. Barrier polishing solution
WO2006028759A3 (fr) * 2004-09-08 2006-12-21 Praxair Technology Inc Suspension aqueuse contenant des particules de silice modifiees par l'incorporation de metallate
WO2010025623A1 (fr) * 2008-09-05 2010-03-11 安集微电子科技(上海)有限公司 Liquide de polissage chimico-mécanique
US9589835B2 (en) * 2008-12-10 2017-03-07 Novellus Systems, Inc. Method for forming tungsten film having low resistivity, low roughness and high reflectivity
US20140017891A1 (en) * 2008-12-10 2014-01-16 Novellus Systems, Inc. Method for depositing tungsten film having low resistivity, low roughness and high reflectivity
US9548228B2 (en) 2009-08-04 2017-01-17 Lam Research Corporation Void free tungsten fill in different sized features
US9653353B2 (en) 2009-08-04 2017-05-16 Novellus Systems, Inc. Tungsten feature fill
US10103058B2 (en) 2009-08-04 2018-10-16 Novellus Systems, Inc. Tungsten feature fill
US10256142B2 (en) 2009-08-04 2019-04-09 Novellus Systems, Inc. Tungsten feature fill with nucleation inhibition
US9972504B2 (en) 2015-08-07 2018-05-15 Lam Research Corporation Atomic layer etching of tungsten for enhanced tungsten deposition fill
US9978610B2 (en) 2015-08-21 2018-05-22 Lam Research Corporation Pulsing RF power in etch process to enhance tungsten gapfill performance
US10395944B2 (en) 2015-08-21 2019-08-27 Lam Research Corporation Pulsing RF power in etch process to enhance tungsten gapfill performance
US10566211B2 (en) 2016-08-30 2020-02-18 Lam Research Corporation Continuous and pulsed RF plasma for etching metals
US10982114B2 (en) 2017-10-25 2021-04-20 Saint-Gobain Ceramics & Plastics, Inc. Composition for conducting material removal operations and method for forming same

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