US20150104952A1 - Method and composition for selectively removing metal hardmask and other residues from semiconductor device substrates comprising low-k dielectric material and copper - Google Patents

Method and composition for selectively removing metal hardmask and other residues from semiconductor device substrates comprising low-k dielectric material and copper Download PDF

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Publication number
US20150104952A1
US20150104952A1 US14/103,303 US201314103303A US2015104952A1 US 20150104952 A1 US20150104952 A1 US 20150104952A1 US 201314103303 A US201314103303 A US 201314103303A US 2015104952 A1 US2015104952 A1 US 2015104952A1
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Prior art keywords
ammonium
acid
tin
removal composition
composition
Prior art date
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Abandoned
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US14/103,303
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English (en)
Inventor
Hua Cui
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
EKC Technology Inc
Original Assignee
EKC Technology 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 EKC Technology Inc filed Critical EKC Technology Inc
Priority to US14/103,303 priority Critical patent/US20150104952A1/en
Assigned to EKC TECHNOLOGY, INC. reassignment EKC TECHNOLOGY, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: CUI, HUA
Assigned to EKC TECHNOLOGY INC. reassignment EKC TECHNOLOGY INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: CUI, HUA
Priority to JP2016522060A priority patent/JP6523269B2/ja
Priority to US15/028,573 priority patent/US10005991B2/en
Priority to KR1020167012242A priority patent/KR102327432B1/ko
Priority to KR1020167012243A priority patent/KR102334603B1/ko
Priority to JP2016521931A priority patent/JP2016535819A/ja
Priority to CN201480055153.4A priority patent/CN105874562B/zh
Priority to US15/028,501 priority patent/US10155921B2/en
Priority to PCT/US2014/059848 priority patent/WO2015054464A1/en
Priority to CN201480055151.5A priority patent/CN105612599B/zh
Priority to PCT/US2014/059840 priority patent/WO2015054460A1/en
Priority to TW103135159A priority patent/TWI650415B/zh
Priority to TW103135158A priority patent/TWI650414B/zh
Publication of US20150104952A1 publication Critical patent/US20150104952A1/en
Abandoned legal-status Critical Current

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    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/26—Processing photosensitive materials; Apparatus therefor
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    • G03F7/422—Stripping or agents therefor using liquids only
    • G03F7/423—Stripping or agents therefor using liquids only containing mineral acids or salts thereof, containing mineral oxidizing substances, e.g. peroxy compounds
    • 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
    • H01L21/3105—After-treatment
    • H01L21/311—Etching the insulating layers by chemical or physical means
    • H01L21/31105—Etching inorganic layers
    • H01L21/31111—Etching inorganic layers by chemical means
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    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
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    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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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
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    • H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
    • H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
    • H01L21/76801—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing
    • H01L21/76802—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing by forming openings in dielectrics
    • H01L21/76807—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing by forming openings in dielectrics for dual damascene structures
    • 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
    • H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
    • H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
    • H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
    • H01L21/76801—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing
    • H01L21/76802—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing by forming openings in dielectrics
    • H01L21/76814—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing by forming openings in dielectrics post-treatment or after-treatment, e.g. cleaning or removal of oxides on underlying conductors
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
    • C11D2111/10—Objects to be cleaned
    • C11D2111/14—Hard surfaces
    • C11D2111/22—Electronic devices, e.g. PCBs or semiconductors
    • 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
    • H01L21/3105—After-treatment
    • H01L21/311—Etching the insulating layers by chemical or physical means
    • H01L21/31144—Etching the insulating layers by chemical or physical means using masks

Definitions

  • compositions and methods for selectively removing metal hardmask and other residues from integrated circuit (IC) device substrates relate to compositions and methods for selectively removing metal hardmask and other residues from integrated circuit (IC) device substrates, and, more particularly, to compositions and methods useful for selectively removing TiN, TaN, TiNxOy, TiW, and W metal hardmask, and metal hardmasks comprising alloys of the foregoing, as well as other residues from such substrates comprising low-k dielectric materials, TEOS, copper, cobalt and other low-k dielectric materials, using carboxylate compounds.
  • IC integrated circuit
  • Plasma dry etching is commonly used to fabricate vertical sidewall trenches and anisotropic interconnecting vias in copper (Cu)/low-k dual damascene fabrication processes.
  • Cu copper
  • Low-k dual damascene fabrication processes As the technology nodes advance to 45 nm and smaller, the decreasing size of the semiconductor devices makes achieving critical profile control of vias and trenches more challenging.
  • Integrated circuit device companies are investigating the use of a variety of metal hardmasks to improve etch selectivity to low-k materials and thereby gain better profile control.
  • the cleaning solution can also effectively etch the metal hardmask to form an intermediate morphology, e.g., a pulled-back/rounded morphology, or completely remove the metal hardmask.
  • a pulled-back/rounded morphology could prevent undercutting the hardmask, which, in turn, could enable reliable deposition of barrier metal, Cu seed layer and Cu filling.
  • fully removing the metal hardmask using the same composition could offer numerous benefits to downstream process steps, particularly chemical mechanical polishing (CMP), by eliminating a need for barrier CMP.
  • cleaning processes are required to remove residues of the plasma etch, photoresist, oxidizer, abrasive, metal and/or other liquids or particles that remain and which can contaminate the surface of the device if they are not effectively removed.
  • Fabrication of advanced generation devices that require copper conductors and low-k dielectric materials typically carbon-doped silicon oxide (SiOCH), or porous low-k materials) give rise to the problem that both materials can react with and be damaged by various classes of prior art cleaners.
  • Low-k dielectrics in particular, may be damaged in the cleaning process as evidenced by etching, changes in porosity/size, and ultimately changes in dielectric properties. Time required to remove residues depends on the nature of the residue, the process (heating, crosslinking, etching, baking, and/or ashing) by which it was created, and whether batch or single wafer cleaning processes can be used. Some residues may be cleaned in a very short period of time, while some residues require much longer cleaning procedures. Compatibility with both the low-k dielectric and with the copper conductor over the duration of contact with the cleaner is a desired characteristic.
  • TiN, TaN, TiNxOy, TiW, and/or W are used as an etching hard mask in the formation of vias and trenches to gain high selectivity to low-k dielectric materials during dry etching steps.
  • Effective cleaning compositions are required that can selectively remove the TiN, TaN, TiNxOy, TiW or W, be compatible with low-k materials, copper, cobalt and other dielectric materials, and also simultaneously remove unwanted etching residues and Cu oxide from the resulting dual damascene structure. Beyond selective cleaning, it is also highly desirable that the achievable removal rate ( ⁇ /min) for the cleaning composition be maintained substantially constant for an extended period of time.
  • the presently disclosed and claimed inventive concept(s) relate to an improved semiconductor processing composition, i.e., a wet cleaning chemistry or removal composition, with one or more carboxylate compounds which provides highly selective removal of metal hardmask from a dual damascene structure without damaging wiring metallurgy and dielectric materials.
  • Semiconductor substrates of the type fabricated in dual damascene back end metallization consist of multiple layers or levels of metal interconnects that are isolated by interlayer dielectrics.
  • the described composition can remove metal hardmask etch residues, photoresist, polymeric materials, and copper oxide from via and trench surfaces without damaging underlying layers that form the structure.
  • the substrates typically comprise copper, cobalt, a low-k dielectric material(s), SiON, SiCN, TEOS and metal hard mask selected from TiN, TaN, TiNxOy, TiW and W, including alloys of Ti and W.
  • the removal composition comprises from 0.1 wt % to 90 wt % at least one oxidizing agent, from 0.0001 wt % to 50 wt % of a carboxylate compound, with the balance up to 100 wt % of the removal composition comprising water, e.g., deionized water.
  • ammonium carboxylates are ammonium carboxylates.
  • ammonium carboxylates are ammonium oxalate, ammonium lactate, ammonium tartrate, ammonium citrate tribasic, ammonium acetate, ammonium carbamate, ammonium carbonate, ammonium benzoate, tetraammonium EDTA, ethylenediaminetetraacetic acid diammonium salt, ammonium succinate, ammonium formate, ammonium 1-H-pyrazole-3-carboxylate, and mixtures thereof.
  • At least one corrosion inhibitor may also be present in the composition, for example, where the composition is to be deployed in semiconductor processing at BEOL applications and other applications where corrosion of Cu or other metal components is a concern.
  • the composition may also include a base, for example, selected from the group consisting of quaternary ammonium salts, such as tetramethylammonium hydroxide (TMAH), tetraethylammonium hydroxide (TEAH) and benzyltrimethylammonium hydroxide (BTAH), and mixtures thereof.
  • TMAH tetramethylammonium hydroxide
  • TEAH tetraethylammonium hydroxide
  • BTAH benzyltrimethylammonium hydroxide
  • the base can also be selected from a primary, secondary or tertiary amine, such as, for example, monoethanol amine (MEA), diglycol amine (DGA), triethanolamine (TEA); and tetrabutyphosphonium hydroxide (TBPH) and mixtures thereof.
  • MEA monoethanol amine
  • DGA diglycol amine
  • TEA triethanolamine
  • TBPH tetrabutyphosphonium hydrox
  • the composition may include one or more acids, for example, an inorganic acid, such as sulfuric acid, nitric acid, phosphoric acid, hydrofluoric acid (HF), or hydrobromic acid, or an organic acid, such as a carboxylic acid, hydroxy carboxylic acid, polycarboxylic acid, amino acid, or a mixture of such acids, as appropriate to adjust the pH of the working composition to a value of from 2 to 14, but preferably in the range of from 3 to 13.
  • the pH of the removal composition is preferably in the range of from 7 to 12.
  • the composition may also include from 0.001 wt % to 20 wt % of an amino acid, amine polycarboxylic acid (i.e., aminopolycarboxylic acid), and/or carboxylic acid, polycarboxylic acid chelating agent, or a mixture thereof, which, along with the carboxylate compound, has been observed to stabilize the composition.
  • stabilize is used herein to mean that the achievable etch rate for a hard mask (e.g., a removal rate for TiN of 148 ⁇ /min) remains substantially constant over an extended period of time, e.g., a time period of from twenty two (22) hours and up to thirty five (35) hours or longer at the selected operating temperature, for example, at an operating temperature of 50° C.
  • Oxidizing agents suitable for carrying out the inventive concepts can be selected from the group consisting of hydrogen peroxide (H 2 O 2 ), benzoyl peroxide, tetrabutylammonium peroxymonosulfate, ozone, n-methylmorpholine oxide (NMMO, NMO), ferric chloride, permanganate, peroxoborate, perchlorate, persulfate, ammonium peroxydisulfate, per acetic acid, urea hydroperoxide, percarbonate, perborate, and mixtures thereof. Best results have been observed when the oxidizing agent is hydrogen peroxide (H 2 O 2 ).
  • the invention comprises a method for selectively removing an etching mask consisting essentially of TiN, TaN, TiNxOy, TiW or W, including alloys of Ti or W, relative to underlying low-k, Cu, Co, SiON, SICN, and TEOS materials from a semiconductor substrate having a TiN, TaN, TiNxOy, TiW or W, etching mask thereon, including an etching mask comprising alloys of Ti or W, wherein the method comprises contacting the substrate with a removal composition comprising:
  • ammonium carboxylate selected from the group comprising one or more of ammonium oxalate, ammonium lactate, ammonium tartrate, ammonium citrate tribasic, ammonium acetate, ammonium carbamate, ammonium carbonate, ammonium Benzoate, tetraammonium EDTA, ethylenediaminetetraacetic acid diammonium salt, ammonium succinate, ammonium formate, and ammonium 1-H-pyrazole-3-carboxylate; and
  • the invention comprises a method for selectively removing an etching mask consisting essentially of TiN, TaN, TiNxOy, TiW or W, including alloys of Ti and/or W, relative to underlying low-k, Cu, Co, SiON, SICN, and TEOS materials from a semiconductor substrate having a TiN, TaN, TiNxOy, TiW or W, etching mask thereon, including an etching mask comprising alloys of Ti and/or W, wherein the method comprises contacting the substrate with a removal composition comprising:
  • ammonium carboxylate selected from the group comprising one or more of ammonium oxalate, ammonium lactate, ammonium tartrate, ammonium citrate tribasic, ammonium acetate, ammonium carbamate, ammonium carbonate, ammonium Benzoate, tetraammonium EDTA, ethylenediaminetetraacetic acid diammonium salt, ammonium succinate, ammonium formate, and ammonium 1-H-pyrazole-3-carboxylate;
  • the described and claimed inventive concept(s) embraces an improvement to a composition and method for selectively removing an etching mask consisting essentially of TiN, TaN, TiNxOy, TiW or W, including alloys of Ti or W, relative to underlying low-k, Cu, Co, SiON, SICN, and TEOS materials from a semiconductor substrate having a TiN, TaN, TiNxOy, TiW or W, etching mask thereon, including an etching mask comprising alloys of Ti or W, wherein the improvement comprises incorporating into said removal composition from 0.0001 wt % to 50 wt % of an ammonium carboxylate selected from the group comprising ammonium oxalate, ammonium lactate, ammonium tartrate.
  • ammonium citrate tribasic, ammonium acetate, ammonium carbamate, ammonium carbonate, ammonium benzoate, tetraammonium EDTA, ethylenediaminetetraacetic acid diammonium salt, ammonium succinate, ammonium formate, ammonium 1-H-pyrazole-3-carboxylate whereby said removal composition selectively removes said TiN, TaN, TiNxOy, TiW, W, or alloy of Ti or W etching mask relative to said low-k materials.
  • the amount and type of undesirable residue to be removed in any given processing step will influence the selection of operating pH for the composition.
  • compositions and method according to the inventive concepts described herein are uniquely capable of selectively etching TiN, TaN, TiNxOy, TiW and W, including alloys of Ti and W, are compatible with Cu, Co, low-k and TEOS dielectric materials, and can also simultaneously remove copper oxides, polymeric materials and etch residues from the substrate, i.e., the dual damascene structure, being treated.
  • a composition formulated according to the invention and exhibiting an inherently high etch rate for TiN, TaN, TiNxOy, TiW and W, including alloys of Ti and W, enables processing at relatively low temperature, e.g., temperatures less than 65° C.
  • a relatively low temperature process exhibits a reduced oxidizer decomposition rate, which, in turn, extends the useful composition bath life and pot life.
  • compositions according to the invention which exhibit high and selective etch rates for TiN, TaN, TiNxOy, TiW and W, including alloys of Ti and W are desirable because they can reduce device processing time and thereby increase throughput.
  • compositions according to the invention can effectively deliver high etch rates for TiN, TaN, TiNxOy, TiW and W, including alloys of Ti and W, with single wafer tool applications at a temperature range of from 20° C. to 60° C., and the TiN, TaN, TiNxOy, TiW and W, including alloys of Ti and W, metal hardmask can be fully removed with single wafer application process equipment if so desired.
  • FIGS. 1A and 1B are cross-sectional SEM images of semiconductor wafer segments which show trenches and vias, respectively, during dual damascene device fabrication, but prior to contact with the removal composition of the invention.
  • FIGS. 2A and 2B are cross-sectional SEM images of semiconductor wafer segments of the type shown in FIGS. 1A and 1B after contact with removal composition 1 from Table 1 at 50° C. for 90 sec.
  • FIGS. 3A and 3B are cross-sectional SEM images of semiconductor wafer segments of the type shown in FIGS. 1A and 1B after contact with removal composition 2 from Table 1 at 50° C. for 90 sec.
  • FIGS. 4A and 4B are cross-sectional SEM images of semiconductor wafer segments of the type shown in FIGS. 1A and 1B after contact with removal composition 3 from Table 1 at 53° C. for 90 sec.
  • any composition is expressed as the amount of various components which, when added together, form the composition. Unless specifically stated otherwise, any composition given in percent is percent by weight (wt %) of that component that has been added to the composition.
  • wt % percent by weight
  • the dual damascene process is used to form metal interconnects in the backend metallization, which are then used to electrically interconnect various electrical components in a semiconductor substrate into functional circuits.
  • backend metallization which comprises fabrication of multiple levels, or layers, of metal interconnects isolated by an interlayer dielectric layer(s) and/or barrier layer(s) can be found, for example, in U.S. Pat. No. 8,080,475, the teachings of which are incorporated herein in their entirety by reference.
  • the integration of new materials, such as ultra low-k dielectrics, into microelectronic devices places new demands on cleaning performance. Concurrently, shinking device dimensions reduces the tolerances for changes in critical dimensions for vias and trenches.
  • the present invention is a semiconductor processing composition
  • a semiconductor processing composition comprising water, at least one oxidizing agent, optionally at least one base or acid, depending on the desired pH for the working composition, and from 0.0001 wt % up to 50 wt % of an ammonium carboxylate.
  • the ammonium carboxylate can be selected from the group comprising ammonium oxalate, ammonium lactate, ammonium tartrate.
  • ammonium citrate tribasic, ammonium acetate, ammonium carbamate, ammonium carbonate, ammonium benzoate, tetraammonium EDTA, ethylenediaminetetraacetic acid diammonium salt, ammonium succinate, ammonium formate, ammonium 1-H-pyrazole-3-carboxylate and mixtures thereof.
  • the concentration of ammonium carboxylate is from 0.001 wt % up to 50 wt %.
  • at least one corrosion inhibitor may also be present in the composition where the composition is to be deployed in BEOL semiconductor processing applications and other applications where corrosion of metal components, e.g., Cu and Cu-alloy components, is a concern.
  • the formulations preferably have a pH of from 3 to 13.
  • compositions of the invention are effective in selectively removing an etching mask consisting essentially of TiN, TaN, TiNxOy, TiW or W, including alloys of Ti and/or W, relative to low-k materials from a semiconductor substrate comprising said low-k dielectric material and having a TiN, TaN, TiNxOy, TiW and W, including alloys of Ti and/or W, etching mask thereon.
  • the composition is also functional in simultaneously removing photoresist, polymeric materials, etching residues and copper oxide from the substrate.
  • compositions of the invention may also include from 0.001 wt % to 20 wt % of an amino acid, amine polycarboxylic acid (i.e., aminopolycarboxylic acid), and/or carboxylic acid, polycarboxylic acid chelating agent, or a mixture thereof, preferably from 0.001 wt % to 10 wt %, and more preferably from 0.001 wt % to 5 wt %.
  • the presence of an amino acid, amine polycarboxylic acid (i.e., aminopolycarboxylic acid), and/or carboxylic acid, polycarboxylic acid chelating agent, or a mixture thereof, according to the described and claimed inventive concepts has been observed to stabilize the composition.
  • chelating agents include, but are not limited to, 1,2-cyclohexanediamine-N,N,N′,N′-tetraacetic acid; ethylenediaminetetraacetic acid; nitrilotriacetic acid; diethylene triamine pentaacetic acid; 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid; ethylene glycol tetraacetic acid (EGTA); 1,2-bis(o-aminophenoxy)ethane-N,N,N′,N′-tetraacetic acid; N- ⁇ 2-[bis(carboxymethyl)amino]ethyl ⁇ -N-(2-hydroxyethyl)glycine (HEDTA); and ethylenediamine-N,N′-
  • compositions and method according to the inventive concepts described herein are particularly applicable for processing single wafers in single wafer equipment.
  • a common approach is to process wafers a high process temperatures.
  • higher temperatures are known to contribute to degradation of the oxidizing agent which shortens bath life and pot life. It has been observed according to the inventive concepts described herein that satisfactory results can be achieved at substantially lower temperatures in the range of from 20° C. to 60° C. to generate a pullback scheme or to completely remove the metal hardmask when the hardmask comprises TiN.
  • the composition can contain one or more cosolvents that are miscible with water. These cosolvents enhance residue removal. Suitable cosolvents include, but are not limited to, sulfolane, N-methylpyrrolidone, and dimethylsulfoxide.
  • Oxidizing agents useful according to the inventive concept(s) are selected from any substance which has the capability to chemically react with the metal hardmask and effect its removal.
  • Such oxidizing agents include, but are not limited to, the group consisting essentially of hydrogen peroxide (H 2 O 2 ), n-methylmorpholine oxide (NMMO or NMO), benzoyl peroxide, tetrabutylammonium peroxymonosulfate, ozone, ferric chloride, permanganate peroxoborate, perchlorate, persulfate, ammonium peroxydisulfate, per acetic acid, urea hydroperoxide, nitric acid (HNO 3 ), ammonium chlorite (NH 4 ClO 2 ), ammonium chlorate (NH 4 ClO 3 ), ammonium iodate (NH 4 IO 3 ), ammonium perborate (NH 4 BO 3 ), ammonium perchlorate (NH 4 ClO 4 ), ammonium periodate
  • the oxidizing agent or mixture thereof may be present in the composition at from about 0.1 wt % to about 90 wt %, preferably at from about 5 wt % to 90 wt %, and, for best results, preferably 10 wt % to 90 wt %.
  • the composition may also include a base or an acid, as appropriate, to adjust the pH of the working composition.
  • the base can, for example, be selected from quaternary ammonium salts, such as tetramethylammonium hydroxide (TMAH), tetraethylammonium hydroxide (TEAH), benzyltrimethylammonium hydroxide (BTAH) and mixtures thereof.
  • the base can also be selected from primary, secondary and tertiary amines, such as, for example, monoethanol amine (MEA), diglycol amine (DGA), triethanolamine (TEA), tetrabutyphosphonium hydroxide (TBPH), and mixtures thereof.
  • the base can be a combination of quaternary ammonium salts and amines.
  • Suitable acids include, for example, inorganic acids, such as sulfuric acid, nitric acid, phosphoric acid, hydrofluoric acid (HF), or hydrobromic acid, or an organic acid, such as a carboxylic acid, an amino acid, a hydroxy carboxylic acid, a polycarboxylic acid, or a mixture of such acids.
  • the pH of the working composition should be maintained at a value of from 2 to 14, but preferably in the range of from 3 to 12. As noted above, when used in BEOL Cu interconnect fabrication applications, the preferred pH of the working composition is in the range of from 7 to 12 when hydrogen peroxide is used as oxidizer in order to achieve high TiN etch rates.
  • a Cu or Co corrosion inhibitor, or a mixture thereof, is an optional component in the composition of this invention.
  • a Cu or Co corrosion inhibitor(s) will usually be present in the inventive composition and associated process when used for BEOL applications, where the presence of a corrosion inhibitor is needed to protect metal surfaces from being etched or otherwise degraded.
  • a corrosion inhibitor(s) is not generally needed, i.e., Cu or Co, is not exposed to the cleaning chemistry, Cu or Co is absent from the wafer substrate, or slight etching/degradation of copper or cobalt surfaces is not usually a concern.
  • the metal (Cu or Co) corrosion inhibitor is an organic compound, such as an azole, thiol, and/or indole preferably selected from the group consisting of a heterocyclic compound containing at least one nitrogen atom, such as, for example, a pyrrole and derivatives thereof, pyrazole and derivatives thereof, imidazole and derivatives thereof, triazole and derivatives thereof, indazole and derivatives thereof, and thiol-triazole and derivatives thereof, benzotriazole (BTA), tolyltriazole, 5-phenyl-benzotriazole, 5-nitro-benzotriazole, 3-amino-5-mercapto-1,2,4-triazole, 1-amino-1,2,4-triazole, hydroxybenzotriazole, 2-(5-amino-pentyl)-benzotriazole, 1-amino-1,2,3-triazole, 1-amino-5-methyl-1,2,3-triazole, 3-amino-1,2,
  • BTA, pyrazole, or a mixture of BTA and pyrazole, or a mixture of BTA and tolyltriazole are preferred Cu corrosion inhibitors for better cleaning performance.
  • the Cu or Co corrosion inhibitor or mixture thereof may be present in the composition at from about 0.0001 wt % to about 50 wt %, and preferably, for best results, at from about 0.0001 wt % to about 20 wt %.
  • Cu or Co corrosion inhibitors include, but are not limited to aromatic hydrazides and Schiff base compounds.
  • the described and claimed inventive concept(s) reside in the discovery that complete removal of metal hard mask from semiconductor devices wherein said metal hardmask is in overlapping relationship with a low-k dielectric material can be accomplished by incorporating into the removal composition an effective amount of from 0.0001 wt % up to 50 wt % of a carboxylate compound, but particularly an ammonium carboxylate.
  • the concentration of ammonium carboxylate is from 0.001 wt % up to 10 wt %.
  • carboxylate is used herein to mean the general formula M(RCOO) n , where M is a metal and n is 1, 2, . . . is the number of carboxylate esters within the compound having the general formula RCOOR′, wherein R and R′ are organic groups with the proviso that R′ ⁇ H.
  • RCOOR′ organic groups with the proviso that R′ ⁇ H.
  • M is replaced with NH4 + .
  • Ammonium carboxylates are preferred chemicals for use in the removal formulation(s), and they can be added directly to the composition, or they can be generated as byproducts or intermediates by chemical reaction during processing.
  • compositions of the invention may be embodied in a wide variety of specific formulations, as hereinafter more fully described.
  • specific components of the composition are discussed in reference to weight percentage ranges including a zero lower limit, it will be understood that such components may be present or absent in various specific embodiments of the composition, and that in instances where such components are present, they may be present at concentrations as low as 0.0001 wt %, based on the total weight of the composition in which such components are employed.
  • 100 g. samples of removal compositions were prepared according to the inventive concept(s) described herein. Each sample composition comprised each of the components listed in the various tables which follow at the weights shown in the corresponding formulation row.
  • a 100 g. quantity of sample composition designated “1” shown in Table 1 contained 2 g. of 10% aqueous ammonium tartrate, 7.21 g. of 10% aqueous DGA, 12.43 g. of 1.5% aqueous BTA, 60 g. H 2 O 2 (30% aqueous), and 18.36 g. deionized water (DIW).
  • the removal compositions can be formulated at the point of use, or they can be conveniently formulated beforehand without an oxidizer and then taken to the point of use where the oxidizer is added. There is also no particular sequence for mixing or blending the various ingredients.
  • Etch rate evaluations were carried out after 1 and 2 minutes of chemical treatment at 60° C. and 50° C., respectively, for TiN and 10 minutes for Cu, Co, W, and TEOS.
  • TiN, Cu, Co, and W thicknesses were measured using a Four Dimensions Four Point Probe Meter 333A, whereby the resistivity of the film was correlated to the thickness of the film remaining after contact with the composition of the invention.
  • the TEOS thickness was measured with Auto SE Spectroscopic Ellipsometer by HORIBA JOBIN YVON.
  • the etch rate was calculated as the thickness change (before and after chemical treatment) divided by the chemical treatment time.
  • Chemical solution pH was measured with a Beckman 260 pH/Temp/mV meter.
  • the H 2 O 2 used in the experiments was sourced from J. T. Baker. Residue removal efficiency and TiN hardmask etch were evaluated from SEM results (Hitachi S-5500).
  • compositions shown in Table 1 were prepared using deionized water as the solvent, BTA or a mixture of BTA and pyrazole as Cu corrosion inhibitor, H 2 O 2 as the oxidizing agent, and diglycolamine (DGA) or benzyltrimethylammonium hydroxide (BTAH) as the base to adjust pH.
  • DGA diglycolamine
  • BTAH benzyltrimethylammonium hydroxide
  • Compositions 1, 2 and 3 demonstrated a removal rate for TiN in the range of from 178 ⁇ /min up to 340 ⁇ /min at a relatively low temperature in the range of from 50° C. to 53° C.
  • a copper etch rate of 2.5 ⁇ /min or less is considered good for commercial wafer processing.
  • FIGS. 1A and 1B are SEM images of semiconductor wafer segments which show trenches and vias, respectively, as received following a dual damascene fabrication step, but before treatment with a removal composition.
  • FIGS. 2A and 2B are views of the wafer segments, similar to the wafer segments shown in FIGS. 1A and 1B , after contact with removal composition 1 for 90 sec. at a temperature of 50° C. Residue was removed, but some TiN hardmask remained as noted in FIG. 2A .
  • FIGS. 3A and 3B are views of wafer segments, similar to the wafer segments shown in FIGS. 1A and 1B , after contact with removal composition 2 for 90 sec. at a temperature of 50° C.
  • FIGS. 4 a and 4 B are views of wafer segments, similar to the wafer segments shown in FIGS. 1A and 1B , after contact with removal composition 3 for 90 sec. at a temperature of 53° C. TiN hardmask and residue have been completely removed.
  • compositions shown in Table 2 were prepared using deionized water as the solvent, BTA as Cu corrosion inhibitor, H 2 O 2 as the oxidizing agent, and tetramethylammonium hydroxide (TMAH) as the base to adjust pH.
  • TMAH tetramethylammonium hydroxide
  • Each of the removal compositions which contain, respectively, the compounds ammonium lactate, ammonium tartrate, ammonium carbonate, and ammonium citrate tribasic at the amounts indicated, demonstrated a higher TiN etch rate compared with the corresponding control, composition 4, that did not contain an ammonium carboxylate.
  • the formulations shown in Table 4 were prepared using DGA to adjust the pH, and BTA was used as the copper corrosion inhibitor.
  • TiN and Cu etch rate evaluations were carried out as described above at a temperature of 50° C. and pH of 8. The removal compositions demonstrated a higher TiN etch rate and a similar Cu etch rate when compared to the control, composition 13, that did not contain an ammonium carboxylate.
  • the formulations shown in Table 5 were prepared using TMAH to adjust the pH, and BTA was used as the copper corrosion inhibitor.
  • TiN and Cu etch rate evaluations were carried out as described above at a temperature of 50° C. and pH of 8. The removal compositions demonstrated a higher TiN etch rate and a similar Cu etch rate when compared to the control, composition 17, that did not contain an ammonium carboxylate.
  • the formulations shown in Table 6 were prepared using benzyltrimethylammonium hydroxide (BTAH) to adjust the pH, and BTA was used as the copper corrosion inhibitor.
  • BTAH benzyltrimethylammonium hydroxide
  • TiN and Cu etch rate evaluations were carried out as described above at a temperature of 50° C. and pH of about 8. The removal compositions demonstrated a higher TiN etch rate and a similar Cu etch rate when compared to the control, composition 21, that did not contain an ammonium carboxylate.
  • the formulations shown in Table 7 were prepared using tetraethylammonium hydroxide (TEAH) to adjust the pH, and BTA was used as the copper corrosion inhibitor.
  • TEAH tetraethylammonium hydroxide
  • TiN and Cu etch rate evaluations were carried out as described above at a temperature of 50° C. and pH of 8. The removal compositions demonstrated a higher TiN etch rate and a similar Cu etch rate when compared to the control, composition 25, that did not contain an ammonium carboxylate.
  • the formulations shown in Table 8 were prepared using DGA to adjust the pH, but no copper corrosion inhibitor was used.
  • TiN and TEOS removal rate evaluations were carried out as described above at a temperature of 50° C. and pH of about 8.
  • the removal compositions demonstrated a high TiN etch rate in the range of from a low of 144 ⁇ /min to a high of 179 ⁇ /min when compared to the control, composition 31, which had a TiN etch rate of 87 ⁇ /min.
  • the presence of the compounds ammonium carbonate, ammonium acetate, ammonium oxalate, ammonium lactate and ammonium tartrate at concentrations of from 1.46 wt % to less than 3 wt % operate to provide the removal compositions of the invention with the capability to deliver very high TiN etch rates at relatively low temperature, e.g., 50° C. It is noteworthy according to the described and claimed inventive concepts that none of the compounds ammonium carbonate, ammonium acetate, ammonium oxalate, ammonium lactate or ammonium tartrate had significant effect on TEOS removal rate when compared to the control, composition 31.
  • the formulations shown in Table 9 were prepared without the use of a pH adjustment agent.
  • the Cu corrosion inhibitor used was Wintrol A-90, a commercial mixture of BTA and tolyltriazole.
  • the desired TiN and Cu etch rates and pH were obtained by varying hydrogen peroxide and ammonium carboxylate concentrations. In these examples, several carboxylates in various concentrations were used. Hydrogen peroxide concentration was either 20 wt % or 80 wt %.
  • the formulation pH's ranged from a low of pH 5 up to pH 8.4, and the TiN etch rate, i.e., the removal rate, ranged from a low of 18 ⁇ /min up to 170 ⁇ /min.
  • the formulations shown in Table 10 were prepared with tartaric acid, or TMAH, or without any pH adjustment agent.
  • Wintrol A-90 was used as a Co corrosion inhibitor.
  • several carboxylates in various concentrations were used.
  • Hydrogen peroxide concentration ranged from 20 wt % to 80 wt %.
  • the formulation pH ranged from a low of pH 5 up to pH 11.
  • the Co etch rate was insignificant in all cases (i.e., the highest Co etch rate was 1.17 ⁇ /min).
  • compositions shown in Table 12 were prepared using TMAH to adjust the pH, and BTA was used as copper corrosion inhibitor.
  • Carboxylates used were potassium citrate tribasic monohydrate, potassium sodium tartrate tetrahydrate, and potassium L-lactate in compositions 56, 57 and 58, respectively. Each of these compositions demonstrated a higher TiN etch rate and a similar Cu etch rate when compared to the control, composition 55, that did not contain a carboxylate.
  • ammonium carboxylate at a concentration of 1.46 wt % to 3 wt % and at a pH ranging from about 4 to slightly higher than 11 was shown to significantly increase the W removal rate when compared to the corresponding ammonium carboxylate-free control compositions 66, 70 and 72 at the same pH.
  • compositions of the invention were observed to unexpectedly stabilize the compositions of the invention.
  • stabilize is used herein to mean that the achievable etch rate for a hard mask, i.e., the rate at which hardmask is removed, remains substantially constant over an extended period of time, e.g., a time period of from twenty two (22) hours up to at least thirty five (35) hours at the selected operating temperature.
  • chelating agents which are operable according to the described and claimed inventive concepts include, but are not limited to, 1,2-cyclohexanediamine-N,N,N′,N′-tetraacetic acid (CDTA); ethylenediaminetetraacetic acid; nitrilotriacetic acid; diethylene triamine pentaacetic acid; 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid; ethylene glycol tetraacetic acid (EGTA); 1,2-bis(o-aminophenoxy)ethane-N,N,N′,N′-tetraacetic acid; N- ⁇ 2-[bis(carboxymethyl)amino]ethyl ⁇ -N-(2-hydroxyethyl)glycine
  • Pot life is a measure of the ability of the removal composition formula to perform optimally over time and without significant variation in functionality over time. Pot life is a strong function of temperature. After many hours of treatment at high temperature, the chemicals in the mixture can decompose and the formula will lose functionality.
  • the data presented in Table 17 demonstrates that with CDTA in removal compositions 74 and 75, the TiN etch rate remained stable, i.e., substantially constant, over a period of 22 hours.
  • the initial TiN etch rate was 157 ⁇ /min, and it remained at 156 ⁇ /min for composition 75 over a 22 hour period.
  • the initial TiN etch rate was 168 ⁇ /min and remained at 157 ⁇ /min over a 22 hour period.
  • the TiN etch rate declined from an initial etch rate of 219 ⁇ /min to an etch rate of 99 ⁇ /min after 22 hours.
  • the data presented in Table 19 demonstrate that with 0.001% and 0.005% of CDTA in removal compositions 77 and 78, respectively, the TiN etch rate remained stable, i.e., substantially constant, over a period of 24 hours.
  • the initial TiN etch rate was 27.33 ⁇ /min, and it remained at 24.41 ⁇ /min for composition 77 over a 24 hour period.
  • the initial TiN etch rate was 26.91 ⁇ /min and remained at 26.24 ⁇ /min over a 24 hour period.
  • Table 20 The formulations shown in Table 20 were prepared using DGA to adjust the pH, and BTA was used as copper corrosion inhibitor. Tetraammonium EDTA was used to stabilize the TiN etch rate.
  • Table 22 The formulations in Table 22 were prepared using DGA to adjust pH. BTA was used as copper corrosion inhibitor. The ammonium carboxylate selected was tetraammonium EDTA. The results shown in Table 22 indicate that tetraammonium EDTA in removal composition 81 exhibited a higher TiN etch rate when compared to the control, composition 82, which contained no ammonium carboxylate.

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US14/103,303 US20150104952A1 (en) 2013-10-11 2013-12-11 Method and composition for selectively removing metal hardmask and other residues from semiconductor device substrates comprising low-k dielectric material and copper
TW103135159A TWI650415B (zh) 2013-10-11 2014-10-09 用於選擇性清除硬遮罩之清除組成物及其方法
TW103135158A TWI650414B (zh) 2013-10-11 2014-10-09 用於選擇性清除硬遮罩之清除組成物及其方法
JP2016521931A JP2016535819A (ja) 2013-10-11 2014-10-09 ハードマスクを選択的に除去するための除去組成物及びその方法
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KR1020167012242A KR102327432B1 (ko) 2013-10-11 2014-10-09 경질 마스크를 선별적으로 제거하기 위한 제거 조성물
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US20160254182A1 (en) 2016-09-01
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