US20010023701A1 - Remover for a ruthenium containing metal and use thereof - Google Patents

Remover for a ruthenium containing metal and use thereof Download PDF

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Publication number
US20010023701A1
US20010023701A1 US09/788,555 US78855501A US2001023701A1 US 20010023701 A1 US20010023701 A1 US 20010023701A1 US 78855501 A US78855501 A US 78855501A US 2001023701 A1 US2001023701 A1 US 2001023701A1
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United States
Prior art keywords
remover
acid
ruthenium
containing metal
ruthenium containing
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Abandoned
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US09/788,555
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English (en)
Inventor
Hidemitsu Aoki
Kaori Watanabe
Norio Ishikawa
Kiyoto Mori
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NEC Corp
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NEC Corp
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Assigned to NEC CORPORATION reassignment NEC CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: AOKI, HIDEMITSU, ISHIKAWA, NORIO, MORI, KIYOTO, WATANABE, KAORI
Publication of US20010023701A1 publication Critical patent/US20010023701A1/en
Priority to US10/123,197 priority Critical patent/US6468357B1/en
Abandoned legal-status Critical Current

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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
    • 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
    • H01L21/3213—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer
    • H01L21/32133—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer by chemical means only
    • H01L21/32134—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer by chemical means only by liquid etching only
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S134/00—Cleaning and liquid contact with solids
    • Y10S134/902—Semiconductor wafer

Definitions

  • This invention relates to a remover for a ruthenium containing metal which is effective for removing an undesired ruthenium containing metal adhering to, for example, a semiconductor substrate and the use thereof.
  • a high dielectric-constant film such as Ta 2 O 5 has been used in place of a conventional silicon oxide or nitride film as a capacitance film for a DRAM or FeRAM.
  • Such a high dielectric-constant film permits us to ensure a required accumulated capacitance in a small occupied area and to improve a degree of memory-cell integration.
  • forming an electrode using ruthenium may lead to peeling of a ruthenium containing metal such as ruthenium and ruthenium oxide adhering to the end face or the rear face of a silicon substrate.
  • the peeled metal may adhere to a device forming area or may cause cross contamination between devices or wafers via a carrying system.
  • a procedure such as forming an electrode film within a narrow hole has been frequently employed for reducing an occupied area for a capacitor. It requires even forming of a thin ruthenium film, so that it is often essential to use CVD exhibiting good coverage as a deposition method, where adhesion of the ruthenium containing metal to the end and/or the rear faces of the silicon substrate becomes more prominent.
  • a ruthenium containing metal is known as a so-called lifetime killer to a semiconductor device. In particular, it may cause a variety of problems; for example, it adversely affects device operation due to reduction in carrier mobility and varying a threshold voltage of a transistor with time.
  • a ruthenium containing metal is diffused at a higher rate in a silicon substrate than platinum also known as a lifetime killer.
  • a trace amount of the ruthenium containing metal remaining on the silicon substrate surface may give prominent adverse affects on device properties. As described above, an undesired ruthenium containing metal remaining on a silicon substrate surface may deteriorate reliability of a device.
  • a remover for ruthenium must not only dissolve the ruthenium containing metal but also effectively preventing the dissolved ruthenium containing metal from re-adhering to a silicon substrate.
  • an objective of this invention is to provide a remover for a ruthenium containing metal which can adequately dissolve and remove a ruthenium containing metal such as ruthenium and ruthenium oxide and can satisfactorily prevent re-adhesion of the dissolved ruthenium containing metal, and the use thereof.
  • This invention provides a remover for a ruthenium containing metal, comprising (a) a cerium (IV) nitrate salt and (b) at least one acid selected from the group consisting of nitric acid, perchloric acid and acetic acid.
  • the remover of this invention exhibits prominent performance of removing a ruthenium containing metal owing to synergism in the combination of components (a) and (b) and can satisfactorily prevent re-adhesion of the dissolved ruthenium containing metal.
  • This remover may be used for washing a substrate to which a ruthenium containing metal adheres or for etching a ruthenium film formed on a substrate.
  • the remover of this invention is particularly suitable for removing ruthenium adhering to a semiconductor device (by washing or etching).
  • ruthenium is known as a so-called lifetime killer to a semiconductor device. It may give serious damage to device performance when remaining on the surface of the semiconductor device.
  • the remover according to this invention may efficiently remove a ruthenium containing metal and prevent re-adhesion so that it is suitable for removing the ruthenium containing metal on such a semiconductor substrate.
  • the remover of this invention is particularly effective when used for washing a semiconductor substrate in which a ruthenium containing metal adheres to an area other than a device forming area.
  • it may be significantly effective when used for removing by washing a ruthenium containing metal adhering to an area other than a device forming area after depositing a ruthenium film in the device forming area on the semiconductor substrate.
  • the ruthenium containing metal adhering the area other than the device forming area is mainly made of ruthenium oxide.
  • the remover of this invention may exhibit good performance of removal and re-adhesion for not only ruthenium but also ruthenium oxide. Thus, it may be suitably used for the above washing.
  • an area other than a device forming area includes end and rear faces of a semiconductor substrate and also peripheral areas in the device forming area.
  • the remover of this invention is characterized in that a cerium (IV) nitrate salt is combined with a particular acid.
  • JP-B 7-7757 and JP-A 11-131263 have described that used as an etchant for preparing a chrome mask.
  • a chromium film such that its cross section becomes tapered. It is known that such a taper shape may be suitably formed by conducting wet etching using a composition having the above combination after forming a resist mask on a chromium film because chromium is dissolved by the action of a cerium (IV) nitrate salt while nitric acid peels the resist mask and the chromium film.
  • This invention also provides method of using a remover for a ruthenium containing metal wherein a substrate is washed with a liquid containing at least one of hydrofluoric acid, nitric acid, perchloric acid and oxalic acid for removing the residual remover after removing with the above remover.
  • This process may allow us to effectively remove a residual remover, leading to washing with higher cleanliness.
  • This invention also provides a process for removing a ruthenium containing metal comprising the steps of depositing a ruthenium film in a device forming area on a semiconductor substrate; and spraying a remover containing (a) a cerium (IV) nitrate salt and (b) at least one acid selected from the group consisting of nitric acid, perchloric acid and acetic acid on a given area on the semiconductor substrate while rotating the substantially horizontal semiconductor substrate to remove a ruthenium containing metal adhering to an area other than the device forming area.
  • the removing process may more effectively remove a ruthenium containing metal.
  • FIG. 1 shows an appearance of a silicon substrate after depositing a ruthenium film.
  • FIG. 2 shows another appearance of a silicon substrate after depositing a ruthenium film.
  • Component (a) in this invention is a cerium (IV) nitrate salt.
  • a cerium (IV) nitrate salt include cerium (IV) ammonium nitrate and cerium (IV) potassium nitrate.
  • Cerium (IV) ammonium nitrate is preferable because it less influences device performance.
  • Component (b) in this invention is at least one acid selected from the group consisting of nitric acid, perchloric acid and acetic acid. In other words, these acids may be used alone or in combination as appropriate. Synergism in a combination of such an acid and component (a) provides prominent effect for removing a ruthenium containing metal.
  • the content of component (a) is preferably 5 wt % or more, more preferably 10 wt % or more, for adequately dissolving and removing a ruthenium containing metal and preventing re-adhesion of the removed ruthenium containing metal.
  • the upper limit of the content is preferably 35 wt % or less, more preferably 30 wt % or less, for effectively preventing precipitation of compound (a).
  • the content of component (b) is preferably 1 wt % or more, more preferably 5 wt % or more, for adequately dissolving and removing a ruthenium containing metal and preventing re-adhesion of the removed ruthenium containing metal.
  • an upper limit of the content may be, for example, 30 wt % or less.
  • a remover in this invention exhibits higher performance for removing a ruthenium containing metal and for re-adhesion prevention by means of synergism provided by a combination of the above components (a) and (b). It is difficult to adequately remove a ruthenium containing metal with component (a) or (b) alone.
  • a remover in this invention usually contains water as component (c), which may enhance performance of the components (a) and (b) for removing a ruthenium containing metal.
  • component (c) is for example 35 to 94 wt %.
  • the remover of this invention may contain a variety of additives such as a surfactant and a water-soluble organic solvent, which may be miscible with water and other components in this invention.
  • a preferable embodiment of a remover in this invention may be one consisting of the above (a), (b) or (c) alone or that to which a small amount of, for example, additive is added.
  • FIG. 1 shows a substrate after depositing a ruthenium film where a silicon substrate 1 is placed on a substrate platform 5 .
  • ruthenium adheres to the end and the rear faces of the silicon substrate 1 .
  • a part of the ruthenium film 2 then becomes ruthenium oxide due to oxidation.
  • the semiconductor substrate to which a ruthenium containing metal such as ruthenium oxide and ruthenium adheres is fed to a carrying system, it may cause cross contamination of a deposition apparatus.
  • a ruthenium containing metal tends to adversely affect device properties. For avoiding such a problem, treatment with a remover is effective.
  • a removing procedure may be conducted by spin washing where only the end and the rear faces are in contact with the remover while introducing nitrogen gas to the device forming surface.
  • examples of a semiconductor substrate include a silicon substrate, a semiconductor substrate made of a III-V group compound such as GaAs, InP and GaN, and a semiconductor substrate made of a II-VI group compound such as ZnSe.
  • this invention is particularly suitable for treating a silicon substrate because this invention exhibits good performance for removing a ruthenium containing metal and is thus prominently effective when being applied to a silicon substrate where deterioration in device performance due to diffusion of ruthenium in the substrate is significant.
  • a silicon substrate on which ruthenium was deposited to a thickness of 100 nm was cut to give an about 2 cm ⁇ 2 cm chip as a sample.
  • the sample was immersed in a remover consisting of an oxidizing agent, an acid and water.
  • Tables 1 to 7 show compositions of a remover. A content of each component is given in wt % to the whole remover. The balance is water.
  • a temperature of the remover was varied in three steps of 40° C., 50° C. and 60° C. After leaving the sample in the remover until the ruthenium film substantially disappeared, the sample was removed, washed with running water for 1 min and dried with nitrogen blow. A dissolution rate for ruthenium was determined from the time taken until the ruthenium film disappeared. The results are shown in Tables 1 to 7, where a dissolution rate is given in ⁇ /min and “CAN” means cerium (IV) ammonium nitrate.
  • ruthenium oxide On a silicon substrate was deposited ruthenium oxide to a thickness of 100 nm and was then formed a resist mask having an opening. The substrate was cut to give an about 2 cm ⁇ 2 cm chip as a sample.
  • the sample was immersed in a remover consisting of an oxidizing agent, an acid and water.
  • Table 8 shows the composition of the remover. A content of each component is given in wt % to the whole remover. The balance is water.
  • a temperature of the remover was varied in three steps of 40° C., 50° C. and 60° C. After leaving the sample in the remover for a given period, the sample was removed, washed with running water for 1 min and dried with nitrogen blow. A dissolution rate for ruthenium oxide was determined from an immersion time and a reduced film thickness. The results are shown in Tables 8, where a dissolution rate is given in ⁇ /min.
  • a silicon substrate on which ruthenium was deposited to a thickness of 100 nm was cut to give an about 2 cm ⁇ 2 cm chip as a sample.
  • the sample was immersed in a remover consisting of an oxidizing agent, an acid and water, where the remover was not stirred or stirred with a stirrer.
  • Table 9 shows the composition of the remover. A content of each component is given in wt % to the whole remover. The balance is water.
  • a temperature of the remover was varied in three steps of 25° C., 30° C. and 40° C. After leaving the sample in the remover until the ruthenium film substantially disappeared, the sample was removed, washed with running water for 1 min and dried with nitrogen blow.
  • a dissolution rate for ruthenium was determined from the time taken until the ruthenium film disappeared. The results are shown in Table 9, where a dissolution rate is given in ⁇ /min. The results indicate that stirring can accelerate dissolution of ruthenium. It may be, therefore, expected that spin washing utilizing physical action can provide more rapid removal than immersing. TABLE 9 Oxidiz- ing agent Acid Stirring 25° C. 30° C. 40° C.
  • a silicon substrate was immersed in a washing, i.e., an aqueous solution of 30 wt % of cerium (IV) ammonium nitrate and 10 wt % of nitric acid, at 40° C. for 5 min.
  • the substrate was removed and determined for an amount of adhering cerium, which was 2.0 ⁇ 10 13 atoms/cm 2 .
  • the substrate was immersed in a washing shown in Table 10, removed, washed with running water for 1 min, dried by nitrogen blow and then determined for an amount of adhering cerium.
  • the results are shown in Table 10. A content of each component is given in wt % to the whole washing. The balance is water. An amount of adhering cerium was determined by total-reflection X-ray fluorescence spectroscopy. The results shown in the table indicate that a washing containing hydrofluoric acid and nitric acid is particularly effective in removing the residual cerium.
  • a remover of this invention in which a cerium (IV) nitrate salt is combined with a particular acid can adequately dissolve and remove a ruthenium containing metal and can effectively prevent re-adhesion of the removed ruthenium containing metal.

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  • Chemical Kinetics & Catalysis (AREA)
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  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
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  • Cleaning Or Drying Semiconductors (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • ing And Chemical Polishing (AREA)
  • Detergent Compositions (AREA)
US09/788,555 2000-02-23 2001-02-21 Remover for a ruthenium containing metal and use thereof Abandoned US20010023701A1 (en)

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US10/123,197 US6468357B1 (en) 2000-02-23 2002-04-17 Remover for a ruthenium containing metal and use thereof

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2000046150A JP4510979B2 (ja) 2000-02-23 2000-02-23 ルテニウム又は酸化ルテニウム除去液の使用方法、及びルテニウム又は酸化ルテニウムの除去方法
JP2000-046150 2000-02-23

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US (2) US20010023701A1 (zh)
EP (1) EP1130636B1 (zh)
JP (1) JP4510979B2 (zh)
KR (1) KR100416889B1 (zh)
CN (2) CN101538716B (zh)
DE (1) DE60113170T2 (zh)
TW (1) TW527440B (zh)

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020056697A1 (en) * 1998-09-03 2002-05-16 Westmoreland Donald L. Ruthenium and ruthenium dioxide removal method and material
US6468357B1 (en) * 2000-02-23 2002-10-22 Nec Corporation Remover for a ruthenium containing metal and use thereof
US6537461B1 (en) * 2000-04-24 2003-03-25 Hitachi, Ltd. Process for treating solid surface and substrate surface
US20030119319A1 (en) * 2001-12-21 2003-06-26 Micron Technology, Inc. Methods for planarization of group VIII metal-containing surfaces using complexing agents
US20030119321A1 (en) * 2001-12-21 2003-06-26 Micron Technology, Inc. Methods for planarization of Group VIII metal-containing surfaces using oxidizing gases
US20030119316A1 (en) * 2001-12-21 2003-06-26 Micron Technology, Inc. Methods for planarization of group VIII metal-containing surfaces using oxidizing agents
US20040157458A1 (en) * 2001-12-21 2004-08-12 Micron Technology, Inc. Methods for planarization of metal-containing surfaces using halogens and halides salts
US7121926B2 (en) 2001-12-21 2006-10-17 Micron Technology, Inc. Methods for planarization of group VIII metal-containing surfaces using a fixed abrasive article
US7442652B2 (en) 2002-02-04 2008-10-28 Nec Electronics Corporation Method for removing contamination and method for fabricating semiconductor device
US11239093B2 (en) 2018-02-05 2022-02-01 Fujifilm Corporation Method for treating substrate, method for manufacturing semiconductor device, and kit for treating substrate
US11732365B2 (en) 2018-11-14 2023-08-22 Kanto Kagaku Kabushiki Kaisha Composition for removing ruthenium
US12024663B2 (en) 2019-02-13 2024-07-02 Tokuyama Corporation Onium salt-containing treatment liquid for semiconductor wafers

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JP3761457B2 (ja) 2001-12-04 2006-03-29 Ｎｅｃエレクトロニクス株式会社 半導体基板の薬液処理装置
KR100672933B1 (ko) * 2003-06-04 2007-01-23 삼성전자주식회사 세정 용액 및 이를 이용한 반도체 소자의 세정 방법
EP2090675B1 (en) * 2008-01-31 2015-05-20 Imec Defect etching of germanium
WO2019142788A1 (ja) 2018-01-16 2019-07-25 株式会社トクヤマ 次亜塩素酸イオンを含む半導体ウェハの処理液
JP2023078483A (ja) * 2020-03-18 2023-06-07 富士フイルム株式会社 基板の処理方法
TW202208323A (zh) 2020-08-07 2022-03-01 日商德山股份有限公司 半導體晶圓用處理液
CN116529421A (zh) 2020-11-26 2023-08-01 株式会社德山 半导体晶片处理液及其制造方法
KR20230104741A (ko) 2020-12-18 2023-07-10 가부시끼가이샤 도꾸야마 천이 금속의 반도체의 처리 방법, 및 천이 금속 산화물의 환원제 함유 처리액
US20240087911A1 (en) 2020-12-18 2024-03-14 Tokuyama Corporation Method for treating transition metal semiconductor, and reducing agent-containing treatment liquid for transition metal oxide

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Cited By (28)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020056697A1 (en) * 1998-09-03 2002-05-16 Westmoreland Donald L. Ruthenium and ruthenium dioxide removal method and material
US6451214B1 (en) * 1998-09-03 2002-09-17 Micron Technology, Inc. Ruthenium and ruthenium dioxide removal method and material
US6537462B1 (en) * 1998-09-03 2003-03-25 Micron Technology, Inc. Ruthenium and ruthenium dioxide removal method and material
US6613242B2 (en) 1998-10-26 2003-09-02 Hitachi Ltd Process for treating solid surface and substrate surface
US6468357B1 (en) * 2000-02-23 2002-10-22 Nec Corporation Remover for a ruthenium containing metal and use thereof
US6537461B1 (en) * 2000-04-24 2003-03-25 Hitachi, Ltd. Process for treating solid surface and substrate surface
US7264677B2 (en) 2000-04-24 2007-09-04 Renesas Technology Corp. Process for treating solid surface and substrate surface
US7025896B2 (en) 2000-04-24 2006-04-11 Renesas Technology Corp. Process for treating solid surface and substrate surface
US20060037627A1 (en) * 2000-04-24 2006-02-23 Miwako Nakahara Process for treating solid surface and substrate surface
US20030205553A1 (en) * 2000-04-24 2003-11-06 Miwako Nakahara Process for treating solid surface and substrate surface
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CN1311351A (zh) 2001-09-05
KR20010085498A (ko) 2001-09-07
KR100416889B1 (ko) 2004-02-05
CN101538716B (zh) 2011-02-09
DE60113170D1 (de) 2005-10-13
JP4510979B2 (ja) 2010-07-28
TW527440B (en) 2003-04-11
DE60113170T2 (de) 2006-07-13
CN101538716A (zh) 2009-09-23
CN100491594C (zh) 2009-05-27
EP1130636B1 (en) 2005-09-07
EP1130636A2 (en) 2001-09-05
JP2001234373A (ja) 2001-08-31
US6468357B1 (en) 2002-10-22

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