WO2017044690A1 - Methods for depositing a conformal metal or metalloid silicon nitride film and resultant films - Google Patents

Methods for depositing a conformal metal or metalloid silicon nitride film and resultant films Download PDF

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Publication number
WO2017044690A1
WO2017044690A1 PCT/US2016/050874 US2016050874W WO2017044690A1 WO 2017044690 A1 WO2017044690 A1 WO 2017044690A1 US 2016050874 W US2016050874 W US 2016050874W WO 2017044690 A1 WO2017044690 A1 WO 2017044690A1
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Prior art keywords
bis
group
plasma
tris
dimethylamino
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PCT/US2016/050874
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English (en)
French (fr)
Inventor
Xinjian Lei
Moo-Sung Kim
Jianheng LI
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Air Products and Chemicals Inc
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Air Products and Chemicals Inc
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Priority to CN201680052609.0A priority Critical patent/CN108026637A/zh
Priority to US15/757,805 priority patent/US11104990B2/en
Priority to KR1020207034629A priority patent/KR102251774B1/ko
Priority to JP2018512922A priority patent/JP6761028B2/ja
Priority to CN202311209900.2A priority patent/CN117265512A/zh
Priority to EP16766797.1A priority patent/EP3347504B1/en
Application filed by Air Products and Chemicals Inc filed Critical Air Products and Chemicals Inc
Priority to KR1020187010145A priority patent/KR102188750B1/ko
Publication of WO2017044690A1 publication Critical patent/WO2017044690A1/en
Priority to IL257990A priority patent/IL257990B2/en
Anticipated expiration legal-status Critical
Priority to US17/458,183 priority patent/US11732351B2/en
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34—Nitrides
    • C23C16/345—Silicon nitride
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/301—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • C23C16/303—Nitrides
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    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/308—Oxynitrides
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    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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    • C23C16/45531—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations specially adapted for making ternary or higher compositions
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    • H—ELECTRICITY
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    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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    • H01L21/02123—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon
    • H01L21/02167—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material being a silicon carbide not containing oxygen, e.g. SiC, SiC:H or silicon carbonitrides
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Definitions

  • Described herein is a method for depositing a stoichiometric or non- stoichiometric silicon nitride film that is doped with one or more Group 4, 5, 6, or 13 of the Periodic Table metal or metalloid using one or more Group 4, 5, 6, or 13 metal or metalloid precursors. More specifically, described herein are plasma-based, cyclic methods including, but not limited to, plasma enhanced atomic layer deposition
  • PEALD plasma enhanced cyclic chemical vapor deposition
  • PECCVD plasma enhanced cyclic chemical vapor deposition
  • Group 4, 5, 6, 13 containing metal of metalloid dielectric films such as, without limitation, aluminum nitride (AIN) or boron nitride (BN) films can be used for a variety of electronic applications.
  • AIN aluminum nitride
  • BN boron nitride
  • the prior art provides different methods for preparing and using Group13 doped metal or metalloid dielectric films such as AISiN films.
  • US Pat. No. 3,974,003 discloses a chemical vapor deposition (CVD) method for depositing a layer containing.
  • Al, N which comprises providing a substrate to be coated, a carrier gas, and a gaseous mixture of nitrogen source compounds, aluminum source compounds, and silicon source material and heating the substrate to a temperature in the range of about 500-1300° to cause formation of the layer containing Al, N, and Si.
  • the reactants, NH 3 , AICI 3 , and SiH 4 can be used.
  • US Publ. No. 2015/0221495 discloses a cyclic deposition process for forming a film comprising: forming a first layer including a first element on a substrate by supplying a gas containing the first element; forming a second layer including first and second elements by supplying a gas containing the second element to modify the first layer; and forming a thin film having a predetermined thickness by setting the forming of the first layer and the forming of the second layer to one cycle and repeating the cycle at least once.
  • US Pat. No. 8,791 ,034 discloses a CVD method for forming an aluminum- silicon nitride layer upon a substrate uses an metal precursor, a silicon precursor and a nitrogen precursor under CVD conditions to deposit the aluminum-silicon nitride layer upon the substrate.
  • a low temperature e.g., processing temperature of about 500 ° C or less
  • a conformal, high quality, Group 4, 5, 6, 13 element doped such as without limitation, an aluminum-doped silicon nitride or an aluminum-doped silicon carbonitride film wherein the film has one or more of the following characteristics: a density of 2.0 grams per cubic centimeter (g/cc) or greater, a low wet etch rate (as measured in dilute hydrofluoric acid (0.5 wt% HF)), hydrogen content less than 20 atomic weight percent %, a reflective index of 1.80 or greater, and combinations thereof.
  • Figure 1 provides a transmission electron microscope (TEM) image of AISiN film deposited using tris(dimethylamino)aluminum, di-iso-propylaminosilane and nitrogen plasma as described in Example 4, which shows the following step coverage: middle 69% and bottom 78%.
  • TEM transmission electron microscope
  • Figure 2 provides a transmission electron microscope (TEM) image of AISiN film deposited using trimethylaluminum, bis(tert-butylamino)silane and nitrogen plasma as described in Example 6, which shows the following step coverage: middle 81 % and bottom 94%.
  • TEM transmission electron microscope
  • Described herein are methods for forming stoichiometric or non-stoichiometric Group 4, 5, 6, 13 metal or metalloid doped silicon nitride films, such as aluminum, gallium, indium, thallium, boron, or combinations thereof doped, silicon nitride films onto at least a portion of a substrate. More specifically, described herein is an atomic layer deposition (ALD) or cyclic CVD method for depositing an aluminum-doped silicon nitride or aluminum-doped silicon carbonitride film.
  • ALD atomic layer deposition
  • cyclic CVD method for depositing an aluminum-doped silicon nitride or aluminum-doped silicon carbonitride film.
  • a method for depositing an aluminum doped silicon nitride film comprising the steps of:
  • introducing into the reactor a metal precursor selected from the group consisting of AICI 3 , trimethylaluminum (TMA), triethylaluminum,
  • TDMAA tris(dimethylamino)aluminum
  • TDMAA tris(dimethylamino)aluminum
  • TDEAA tris(diethylamino)aluminum
  • introducing into the reactor a plasma containing source to react with at least a portion of the chemisorbed layer and provide at least one reactive site wherein the plasma is generated at a power density ranging from about 0.01 to about 1 .5 W/cm 2 ; e. purging the reactor with a purge gas;
  • organoaminosilane precursor represented by the following Formulae I through IV below:
  • R 1 is selected from a linear d to C 10 alkyl group, a branched C 3 to C 10 alkyl group, a linear or branched C 3 to C 10 alkenyl group, a linear or branched C 3 to C 10 alkynyl group, a Ci to C 6 dialkylamino group, an electron withdrawing group, a C 6 to Ci 0 aryl group, a Ci to C1 0 alkyl silyl group, and a silyl group;
  • R 1 and R 2 are the same. In other embodiments of Formulae I, III and III, R 1 and R 2 are different. In the foregoing or other embodiments of Formula I and IV, R 1 and R 2 can be linked together to form a ring. In these embodiments, the ring can be a substituted or an unsubstituted aromatic or aliphatic ring. In the yet further embodiments, R 1 and R 2 are not linked together to form a ring.
  • the plasma containing source is selected from the group consisting of a nitrogen and argon plasma, a nitrogen and neon plasma, an ammonia plasma, a nitrogen and ammonia plasma, an ammonia and helium plasma, an ammonia and argon plasma, an ammonia and nitrogen plasma, a NF 3 containing plasma, an organoamine containing plasma, and mixtures thereof.
  • the plasma containing source comprises a non-hydrogen containing plasma selected from the group consisting of nitrogen plasma; a plasma comprising nitrogen and helium; a plasma comprising nitrogen and argon plasma; a plasma comprising nitrogen and argon plasma, and a plasma comprising nitrogen and neon.
  • a plasma enhanced atomic layer deposition (ALD) or plasma enhanced ALD-like method for depositing a conformal Group 4, 5, 6, 13 metal or metalloid silicon nitride or carbonitride film at a low temperature, or one or more deposition temperatures ranging from about 25°C to about 500°C, using a Group 4, 5, 6, 13 metal or metalloid precursor and organoaminosilane precursor having Formulae I through IV described herein in a plasma process which comprises nitrogen and optionally a noble gas.
  • ALD plasma enhanced atomic layer deposition
  • ALD-like method for depositing a conformal Group 4, 5, 6, 13 metal or metalloid silicon nitride or carbonitride film at a low temperature, or one or more deposition temperatures ranging from about 25°C to about 500°C, using a Group 4, 5, 6, 13 metal or metalloid precursor and organoaminosilane precursor having Formulae I through IV described herein in a plasma process which comprises nitrogen and optionally a noble gas.
  • Another aspect of the invention relates to silicon containing films, conformal films and films obtained by the inventive processes.
  • One aspect of the invention relates to an aluminum-doped silicon nitride or an aluminum-doped silicon carbonitride film wherein the film has one or more of the following characteristics: a density of 2.0 grams per cubic centimeter (g/cc) or greater, a low wet etch rate (as measured in dilute hydrofluoric acid (HF)), hydrogen content less than 20 atomic weight percent %, a reflective index of 1 .80 or greater, and combinations thereof.
  • g/cc grams per cubic centimeter
  • HF dilute hydrofluoric acid
  • a further aspect of the invention relates to a gallium-doped silicon nitride or a gallium-doped silicon carbonitride film wherein the film has one or more of the following characteristics: a density of 2.0 grams per cubic centimeter (g/cc) or greater, hydrogen content less than 20 atomic weight percent %, a reflective index of 1 .80 or greater, and combinations thereof.
  • Another aspect of the invention relates to a titanium-doped silicon nitride or a titanium-doped silicon carbonitride film wherein the film has one or more of the following characteristics: a density of 2.0 grams per cubic centimeter (g/cc) or greater, hydrogen content less than 20 atomic weight percent %, a reflective index of 1 .80 or greater, and combinations thereof.
  • Another aspect of the invention relates to a zirconium-doped silicon nitride or a zirconium-doped silicon carbonitride film wherein the film has one or more of the following characteristics: a density of 2.0 grams per cubic centimeter (g/cc) or greater, hydrogen content less than 20 atomic weight percent %, a reflective index of 1 .80 or greater, and combinations thereof.
  • a further aspect of the invention relates to a hafnium-doped silicon nitride or a hafnium-doped silicon carbonitride film wherein the film has one or more of the following characteristics: a density of 2.0 grams per cubic centimeter (g/cc) or greater, hydrogen content less than 20 atomic weight percent %, a reflective index of 1 .80 or greater, and combinations thereof.
  • Another aspect of the invention relates to a tantalum-doped silicon nitride or a tantalum-doped silicon carbonitride film wherein the film has one or more of the following characteristics: a density of 2.0 grams per cubic centimeter (g/cc) or greater, hydrogen content less than 20 atomic weight percent %, a reflective index of 1 .80 or greater, and combinations thereof.
  • An aluminum doped silicon nitride film is considered a "high quality" film if it has one or more of the following characteristics: a density of 2.2 grams per cubic centimeter (g/cc) or greater (e.g., about 2.2 to about 3.0 g/cc, about 2.4 to about 2.9 g/cc and in some cases about 2.4 to about 2.8 g/cc) as measured by X-ray-reflectometry (XRR), a low wet etch rate (as measured in dilute hydrofluoric acid (0.5 wt % HF in Dl water), a hydrogen content of 20 atomic (at.)% or less (e.g., about 1 at.% to about 20 at.%, about 5 at.% to about 20 at.% and in some cases about 1 at% to about 10 at.%) as measured by secondary ion mass spectrometry (SIMS), a reflective index greater of 1.80 or greater (e.g., about 1 .8 to about 2.8, about 2.0 to
  • the content of Group 4, 5, 6, or 13 element such as titanium, hafnium, zirconium, tantalum, tungsten, aluminum, gallium, indium, can vary from 1 to 20 at%, 1 at.% to 15 at.%, and in some cases about 1 at.% to 10 at.%.
  • the aluminum doped silicon nitride film further comprises carbon or aluminum such as a silicon carbonitride or silicon aluminum nitride film.
  • the aluminum doped silicon nitride film further comprises oxygen such as a silicon oxynitride film.
  • the aluminum doped silicon nitride film comprises oxygen and carbon such as a silicon carboxynitride film.
  • aluminum doped silicon nitride refers to a film comprising aluminum, silicon and nitrogen selected from the group consisting of stoichiometric or non- stoichiometric aluminum silicon nitride, aluminum silicon carbonitride, aluminum silicon carboxynitride, and there mixture thereof.
  • the content of aluminum or gallium can vary from 1 to 20 at%, 1 at. % to 15 at. %, and in some cases about 1 at. % to 1 0 at. %.
  • the films are deposited using a Group 4, 5, 6, 13 metal or metalloid precursor such as an metal precursor and an organoaminosilane which is at least one represented by the following Formulae I through IV below:
  • R 1 is selected from a linear Ci to do alkyl group, a branched C 3 to do alkyl group, a linear or branched C 3 to do alkenyl group, a linear or branched C 3 to do alkynyl group, a d to C 6 dialkylamino group, an electron withdrawing group, a C 6 to d 0 aryl group, a d to d 0 alkyl silyl group, a silyl group, organoaminosilyl group, halidosilyl group;
  • R 2 is selected from hydrogen, a linear C 2 to C 10 alkyl group, a branched C 3 to C 10 alkyl group, a linear or branched C 3 to C 6 alkenyl group, a linear or branched C 3 to C 6 alkynyl group, a Ci to C 6 dialkylamino group, a C 6 to Ci 0 aryl group, an electron withdrawing group, and a C 4 to C 10 ary
  • organoaminosilanes having formulae I, II, III, and IV include, but not limited to, di-iso-propylaminosilane, di-sec-butylaminosilane, phenylmethylaminosilane, 2,6-dimethylpiperidinosilane, N-methylcyclohexylaminosilane, N- ethylcyclohexylaminosilane, N-isopropylcyclohexylaminosilane, 2-methylpiperidinosilane, N-silyldecahydroquinoline, 2,2,6,6-tetramethylpiperidinosilane, 2-(N- silylmethylamino)pyridine, N-t-butyldisilazane, N-t-pentyldisilazane, N-(3-methyl-2- pyridyl)disilazane, N-(2-methylphenyl)disilazane, N-(2-ethylphenyl
  • bis(cyclohexylamino)methylsilane bis(iso-propylamino)dimethylsilane, bis(iso- butylamino)dimethylsilane, bis(sec-butylamino)dimethylsilane, bis(tert- butylamino)dimethylsilane, bis(tert-pentylamino)dimethylsilane, and
  • bis(cyclohexylamino)dimethylsilane bis(dimethylamino)silane, bis(diethylamino)silane, bis(ethylmethylamino)silane, bis(tert-butylamino)silane, tris(dimethylamino)silane, tris(iso-propylamino)silane.
  • the organoaminosilane precursors having Formulae I , II, III, and IV described herein exhibit a balance of reactivity and stability that makes them ideally suited as PEALD or PECCVD precursors for semiconductor device manufacturing processes.
  • certain precursors may have boiling points that are too high to be vaporized and delivered to the reactor to be deposited as a film on a substrate.
  • Precursors having higher relative boiling points e.g., greater than about 250°C
  • organoaminosilane precursors having Formula I, II, III or IV have more Si-H groups than those disclosed in prior art, thereby potentially allowing the deposition of high quality aluminum doped silicon nitride via reacting Si-H with Si-NH catalyzed by adsorbed metal precursor to form Si-N-Si linkage.
  • the organoaminosilane precursors of Formula IV having Si-NH group such as bis(tert-butylamino)silane (BTBAS) or bis(sec- butylamino)methylsilane or bis(iso-propylamino)methylsilane may react with adsorbed Al-Me groups to form Al-N-Si bond, then allowing more silicon fragments to be anchored on structured substrates and promoting formation of highly conformal aluminum doped silicon nitride or silicon carbonnitride.
  • BBAS bis(tert-butylamino)silane
  • bis(sec- butylamino)methylsilane or bis(iso-propylamino)methylsilane may react with adsorbed Al-Me groups to form Al-N-Si bond, then allowing more silicon fragments to be anchored on structured substrates and promoting formation of highly conformal aluminum doped silicon nitride or silicon carbonnitride.
  • the organoaminosilane precursors having Formula I to IV described herein comprise 2% or less by weight, or 1 % or less by weight, or 0.5% or less by weight of by-product (after being stored for a time period of 6 months or greater, or one year or greater which is indicative of being shelf stable.
  • the organoaminosilane precursor described herein may be able to deposit high density materials at one or more deposition temperatures, e.g., 400°C or less, 350°C or less, 300°C or less, or 250°C or less, 200°C or less, 150°C or less, 100°C or less, or 50°C or less.
  • alkyl denotes a group derived from an alkane by removal of one hydrogen atom and having from 1 to 10 or from 3 to 6 or from 3 to 4 carbon atoms.
  • exemplary linear alkyl groups include, but are not limited to, methyl, ethyl, n-propyl, n-butyl, and n-pentyl.
  • exemplary branched alkyl groups include, but are not limited to, iso-propyl, tert-butyl, and sec-butyl.
  • cyclic alkyl denotes a cyclic functional group having from 3 to 10 or from 4 to 10 carbon atoms or from 5 to 10 carbon atoms.
  • exemplary cyclic alkyl groups include, but are not limited to, cyclobutyl, cyclopentyl, cyclohexyl, and cyclooctyl groups.
  • aryl denotes an aromatic cyclic functional group having from 5 to 12 carbon atoms or from 6 to 10 carbon atoms.
  • exemplary aryl groups include, but are not limited to, phenyl, benzyl, chlorobenzyl, tolyl, and o-xylyl.
  • alkenyl group denotes a group which has one or more carbon-carbon double bonds and has from 3 to 10 or from 3 to 6 or from 3 to 4 carbon atoms.
  • alkynyl group denotes a group which has one or more carbon-carbon triple bonds and has from 3 to 10 or from 3 to 6 or from 3 to 4 carbon atoms.
  • dialkylamino group denotes a group which has two alkyl groups attached to a nitrogen atom and has from 1 to 10 or from 2 to 6 or from 2 to 4 carbon atoms.
  • exemplary aryl groups include, but are not limited to dimethylamino, diethylamino, and ethylmethylamino.
  • alkylsilyl group denotes a group which has at least one silicon atom as well as 1 to 10 or from 2 to 6 or from 2 to 4 carbon atoms.
  • exemplary alkylsilyl groups include, but are not limited to, methylsilyl (MeSiH 2 -), dimethylsilyl (Me 2 SiH-), trimethylsily (Me 3 Si-).
  • the silyl group refers to H 3 Si- or (H 3 Si) 2 NSiH 2 -.
  • electron withdrawing group denotes an atom or group thereof that acts to draw electrons away from the M-N bond.
  • suitable electron withdrawing groups or substituents include, but are not limited to, nitriles (CN).
  • electron withdrawing substituent can be adjacent to or proximal to N in any one of the Formulae I through III.
  • Further non-limiting examples of an electron withdrawing group includes F, CI, Br, I, CN, N0 2 , RSO, and/or RS0 2 wherein R can be a to C 10 alkyl group such as, but not limited to, a methyl group or another group.
  • trisilylamine derivatives denotes a compound derived from trisilylamine.
  • exemplary trisilylamine derivatives include, but are not limited to, (chlorosilyl)bis(silyl)amine with a formula of (CISiH 2 )N(SiH 3 )2, (bromosilyl)bis(silyl)amine with a formula of (BrSiH 2 )N(SiH 3 )2, (di- isopropylaminosilyl)bis(silyl)amine with a formula of ( l Pr 2 NSiH 2 )N(Sil-l3) 2 ,
  • volatile aluminum precursor denotes an aluminum compound having at least one Al-C bond, Al-N bond, Al-halido bond or combination thereof with a vapor.
  • volatile gallium precursor denotes a gallium compound having at least one Ga-C bond, Ga-N bond, Ga-halido bond or combination thereof with a vapor pressure of 0.5 torr or higher at temperature of 50°C or higher.
  • one or more of the alkyl group, alkenyl group, alkynyl group, alkoxy group, dialkylamino group, aryl group, and/or electron withdrawing group in Formulae I through IV may be substituted or have one or more atoms or group of atoms substituted in place of, for example, a hydrogen atom.
  • substituents include, but are not limited to, oxygen, sulfur, halogen atoms (e.g., F, CI, I, or Br), nitrogen, and phosphorous.
  • fluorinated alkyl group denotes a group wherein the alkyl group has one or more of its atoms such, as a hydrogen atom, substituted with a fluorine atom.
  • organoamine as used herein describes organic compound has at least one nitrogen atom.
  • organoamine examples include methylamine, ethylamine, propylamine, iso-propylamine, tert-butylamine, sec-butylamine, tert-amylamine, ethylenediamine, dimethylamine, trimethylamine, diethylamine, pyrrole, 2,6-dimethylpiperidine, di-n-propylamine, di-iso-propylamine, ethylmethylamine, N-methylaniline, pyridine, and triethylamine.
  • organoamino group refers to an organic group consisting of at least one nitrogen atom derived from secondary or primary
  • step coverage is defined as a percentage of two thicknesses of the deposited metal doped silicon nitride dielectric film in a structured or featured substrate having either vias or trenches or both, with bottom step coverage being the ratio (in %): thickness at the bottom of the feature is divided by thickness at the top of the feature, and middle step coverage being the ratio (in %): thickness on a sidewall of the feature is divided by thickness at the top of the feature.
  • Films deposited using the method described herein exhibit a step coverage of about 60% or greater, about 70% or greater, about 80% or greater, or about 90% or greater which indicates that the films are conformal.
  • dielectric films as used herein is defined as a material having a dielectric constant of 20 or less, 10 or less, 7 or less, 6 or less, 5 or less, 4 or less as measured by mercury probe.
  • the method also includes a Group 4, 5, 6, 13 metal or metalloid precursor.
  • exemplary Group 4, 5, 6, 13 metal or metalloid precursors include, but are not limited to, trimethylaluminum, triethylaluminum, tris(dimethylamino)aluminum,
  • TDMAZ tetrakis(dimethylamino)zirconium
  • TDEAZ tetrakis(diethylamino)zirconium
  • TEMAZ tetrakis(ethylmethylamino)zirconium
  • TiCI 4 titanium chloride
  • TDMAT tetrakis(dimethylamino)titanium
  • TDEAT tetrakis(diethylamino)titanium
  • TEMAT tetrakis(ethylmethylamino)titanium
  • TaCI 5 tantalum chloride
  • TBTDET tert-butylimino tri(dimethylamino)tantalum
  • TBTDMT tert-butylimino tri(ethylmethylamino)tantalum
  • EITDET ethylimino tri(diethylamino)tantalum
  • EITDMT ethylimino tri(ethylmethylamino)tantalum
  • EITEMT tert-amylimino
  • Tri(dimethylamino)tantalum TAIMAT
  • tert-amylimino tri(diethylamino)tantalum pentakis(dimethylamino)tantalum
  • tert-amylimino tri(ethylmethylamino)tantalum tungsten hexachloride, tungsten pentachloride, bis(tert-butylimino)bis(dimethylamino)tungsten (BTBMW), bis(tert-butylimino)bis(diethylamino)tungsten, bis(tert- butylimino)bis(ethylmethylamino)tungsten, and combinations thereof.
  • Further exemplary Group 4, 5, 6, 13 metal or metalloid precursors include a "borane
  • borane organoamine complex denotes a stable and volatile borane complex formed by reacting borane or diborane with an organoamine.
  • organoamine borane complexes include, but are not limited to borane trimethylamine complex, borane triethylamine complex, dimethylamine borane, borane pyridine complex, borane morpholine complex, borane terf-butylamine complex, borane 4-methylmorpholine complex, borane A/,A/-diisopropylethylamine complex, borane ethylenediamine complex, 2-Methylpyridine borane complex.
  • the Group 4, 5, 6, 13 metal comprises aluminum.
  • the precursor is an aluminum precursor selected from the group consisting of AICI 3 , trimethylaluminum (TMA), triethylaluminum, methylaluminum chloride (MeAICI 2 ), tris(dimethylamino)aluminum (TDMAA), tris(dimethylamino)aluminum
  • TDEAA tris(diethylamino)aluminum
  • the method used to form Group 4, 5, 6, 13 metal or metalloid nitride films are deposition processes.
  • suitable deposition processes for the method disclosed herein include, but are not limited to, plasma enhanced ALD (PEALD) or plasma enhanced cyclic CVD (PECCVD) process that use equipment known in this art.
  • PEALD plasma enhanced ALD
  • PECCVD plasma enhanced cyclic CVD
  • chemical vapor deposition processes refers to any process wherein a substrate is exposed to one or more volatile precursors, which react and/or decompose on the substrate surface to produce the desired deposition.
  • the term "atomic layer deposition process” refers to a self-limiting (e.g., the amount of film material deposited in each reaction cycle is constant), sequential surface chemistry that deposits films of materials onto substrates of varying compositions.
  • the precursors, reagents and sources used herein may be sometimes described as "gaseous", it is understood that the precursors can be either liquid or solid which are transported with or without an inert gas into the reactor via direct vaporization, bubbling or sublimation. In some case, the vaporized precursors can pass through a plasma generator.
  • the aluminum nitride film is deposited using an ALD process. In another embodiment, the aluminum nitride film is deposited using a CCVD process.
  • the aluminum nitride film is deposited using a thermal CVD process.
  • reactor includes without limitation, reaction chamber or deposition chamber having a design and operation known in this art.
  • the ALD-like process is defined herein as a cyclic CVD process that provides a high conformal aluminum nitride film on a substrate as shown by having at least one of the following: percentage of non- uniformity of about 5% or less as measured by ellipsometer, a deposition rate of 0.1 A or greater per cycle, or a combination thereof.
  • the method disclosed herein avoids pre-reaction of the precursors by using PEALD or PECCVD methods that separate the precursors prior to and/or during the introduction to the reactor.
  • deposition techniques such as PEALD or PECCVD processes are used to deposit Group 4, 5, 6, 13 metal or metalloid nitride film.
  • the film is deposited via a PEALD process by exposing the substrate surface alternatively to the one or more the aluminum nitride precursor, nitrogen-containing source, or other precursor or reagent. Film growth proceeds by self-limiting control of surface reaction, the pulse length of each precursor or reagent, and the deposition temperature. However, once the surface of the substrate is saturated, the film growth ceases.
  • the Group 4, 5, 6, 13 metal or metalloid nitride films comprise aluminum and nitrogen or boron and nitrogen or gallium and nitrogen or titanium and nitride.
  • the aluminum or boron or gallium nitride films deposited using the methods described herein are formed in the presence of nitrogen-containing source.
  • a nitrogen-containing source may be introduced into the reactor in the form of at least one nitrogen-containing source and/or may be present incidentally in the other precursors used in the deposition process.
  • Suitable nitrogen- containing source gases may include, for example, nitrogen/argon plasma.
  • the nitrogen-containing source comprises nitrogen/argon plasma source gas that is introduced into the reactor at a flow rate ranging from about 1 to about 2000 standard cubic centimeters (seem) or from about 1 to about 1000 seem.
  • the nitrogen- containing source can be introduced for a time that ranges from about 0.1 to about 100 seconds.
  • the precursor pulse can have a pulse duration that is greater than 0.01 seconds
  • the nitrogen-containing source can have a pulse duration that is less than 0.01 seconds
  • the water pulse duration can have a pulse duration that is less than 0.01 seconds.
  • the purge duration between the pulses that can be as low as 0 seconds or is continuously pulsed without a purge in-between.
  • a nitrogen-containing plasma comprising a nitrogen containing gas such as, without limitation, nitrogen and optionally a noble gas can be generated in situ or remotely, preferably a noble gas with an atomic mass greater than nitrogen's atomic mass (i.e., 28 amu).
  • a noble gas with an atomic mass greater than nitrogen's atomic mass i.e., 28 amu.
  • the nitrogen plasma source gas is introduced into the reactor at a flow rate ranging from about 1 to about 2000 square cubic centimeters (seem) or from about 1 to about 1000 seem or more.
  • the nitrogen containing plasma can be introduced for a time that ranges from about 0.01 to about 100 seconds or more.
  • the precursor pulse can have a pulse duration that is greater than 0.01 seconds
  • the nitrogen-containing plasma can have a pulse duration that is less than 0.01 seconds
  • the water pulse duration can have a pulse duration that is less than 0.01 seconds.
  • the purge duration between the precursor pulse and nitrogen plasmas that can be as low as 0 seconds.
  • a hydrogen plasma can be generated in situ or remotely using pure hydrogen (H 2 )) mixed with a noble gas when a hydrogen plasma can be employed.
  • the weight percentage of the noble gas in the plasma containing both nitrogen and noble gas can vary from 1 wt % to 99 wt % (e.g., about 1 wt % to about 50wt %, about 10 wt % to about 90 wt % and in some cases about 5 wt % to about 95 wt %), whereas the weight percentage of the noble gas in the plasma containing both hydrogen and noble gas can also vary from 1 wt % to 99 wt %.
  • the plasma containing both nitrogen and a noble gas such as argon can facilitate the formation of Group 4, 5, 6, 13 metal or metalloid dielectric films such as an aluminum nitride film having less hydrogen content as well as provide reactive sites such as Al-Me or AI-NMe 2 groups on at least a portion of the chemisorbed surface, especially sidewalls of a structured substrate allowing to anchor silicon containing fragments onto these reactive sites in subsequent deposition cycles, thus boosting the deposition of silicon nitride on the sidewall or bottom of vias or trenches and making step coverage of 60% or greater possible since it is very difficult to achieve such as step coverage.
  • a noble gas such as argon
  • the plasma density which is defined by plasma power over area of electrodes (for example, plasma power of 450W for a 6" wafer ALD reactor, the plasma density is about 2.5W/cm 2 assuming the area of electrode is same as the wafer) and is preferably lower than 2 W/cm 2 in order to reduce potential plasma damage on the substrate as well as any built-in structures on the substrate, yet still produce high quality aluminum nitride film which can be implemented into semi-conductor manufacturing processes.
  • the plasma density of the method described herein ranges from about 0.01 to about 2 W/cm 2 , or from about 0.01 to about 1.5 W/cm 2 , or from about 0.01 to 1 W/cm 2 .
  • Typical plasma frequency ranges from 10 KHz to 2.4 GHz, preferably 10 kHz to 60 MHz.
  • dual RF plasma can be employed, one low frequency ranging from 10 kHz to 1 MHz and the other middle frequency selected from group consisting of
  • the deposition methods described herein may involve one or more purge gases.
  • the purge gas which is used to purge away unconsumed reactants and/or reaction byproducts, is an inert gas that does not react with the precursors.
  • Exemplary purge gases include, but are not limited to, argon (Ar), nitrogen (N 2 ), helium (He), neon (Ne), hydrogen (H 2 ), and mixtures thereof.
  • the inert gas that is used as a purge gas comprises a noble gas.
  • the term "noble gas” as used herein means those gases found in Group 18 of the Periodic Table and include, helium (He), neon (Ne), argon (Ar), Xenon (Xe), krypton (Kr), and mixtures thereof.
  • the noble gas used as a purge gas comprises argon.
  • the purge gas comprising Ar is supplied into the reactor at a flow rate ranging from about 10 to about 2000 seem for about 0.1 to 1000 seconds, thereby purging the unreacted precursor material and any byproduct that may remain in the reactor.
  • the respective step of supplying the precursors, the nitrogen-containing source, and/or other precursors, source gases, and/or reagents may be performed by changing the time for supplying them to change the stoichiometric composition of the resulting film.
  • Energy is applied to the at least one of the precursor, nitrogen-containing source, reducing agent, other precursors or combination thereof to induce reaction and to form the film or coating on the substrate.
  • energy can be provided by, but not limited to, thermal, plasma, pulsed plasma, helicon plasma, high density plasma, inductively coupled plasma, X-ray, e-beam, photon, remote plasma methods, and combinations thereof by using equipment known in this art.
  • a secondary RF frequency source can be used to modify the plasma characteristics at the substrate surface.
  • the plasma- generated process may comprise a direct plasma-generated process in which plasma is directly generated in the reactor, or alternatively a remote plasma-generated process in which plasma is generated outside of the reactor and supplied into the reactor.
  • the Group 4, 5, 6, 13 metal or metalloid precursors, organoaminosilane having formulae I to IV, or both may be delivered to the reaction chamber such as a PEALD or PECCVD reactor either single wafer or batch in a variety of ways such as bubbling, vapor draw, or direct liquid injection (DLI).
  • a liquid delivery system may be utilized.
  • a combined liquid delivery and flash vaporization process unit may be employed, such as, for example, the turbo vaporizer manufactured by MSP Corporation of Shoreview, MN, to enable low volatility materials to be volumetrically delivered, which leads to reproducible transport and deposition without thermal decomposition of the precursor.
  • the turbo vaporizer manufactured by MSP Corporation of Shoreview, MN
  • the precursors described herein may be delivered in neat liquid form, or alternatively, may be employed in solvent formulations or compositions comprising same.
  • the precursor formulations may include solvent component(s) of suitable character as may be desirable and advantageous in a given end use application to form a film on a substrate.
  • exemplary solvents can include, without limitation, ether, tertiary amine, alkyl hydrocarbon, aromatic hydrocarbon, tertiary aminoether, and combinations thereof.
  • the difference between the boiling points of the organoaminodisilane and the boiling point of the solvent is 40°C or less.
  • the wt % of silicon precursor compound in the solvent can vary from 1 to 99 wt %, or 10 to 90 wt%, or 20 to 80 wt %, or 30 to 70 wt %, or 40 to 60 wt %, to 50 to 50 wt %.
  • the gas lines connecting from the precursor canisters to the reaction chamber are heated to one or more temperatures depending upon the process requirements and the container of the metal precursor having the formulae I through IV described herein is kept at one or more temperatures for bubbling.
  • a solution comprising the at least one aluminum nitride precursor having the formula described herein is injected into a vaporizer kept at one or more
  • a flow of argon and/or other inert gas may be employed as a carrier gas to help deliver the vapor of the at least one metal precursor to the reaction chamber during the precursor pulsing.
  • the reaction chamber process pressure is about 2 Torr or less. In other embodiments, the reaction chamber process pressure is about 10 Torr or less.
  • a substrate such as, without limitation, a silicon oxide, carbon doped silicon oxide, flexible substrate, or metal nitride substrate is heated on a heater stage in a reaction chamber that is exposed to the aluminum nitride precursor initially to allow the metal precursor to chemically adsorb onto the surface of the substrate.
  • a purge gas such as nitrogen, argon, or other inert gas purges away unabsorbed excess aluminum from the process chamber.
  • a nitrogen-containing source may be introduced into reaction chamber to react with the absorbed surface followed by another gas purge to remove reaction by-products from the chamber. The process cycle can be repeated to achieve the desired film thickness.
  • pumping under vacuum can be used to remove unabsorbed excess aluminum from the process chamber, after sufficient evacuation under pumping, a nitrogen-containing source may be introduced into reaction chamber to react with the absorbed surface followed by another pumping down purge to remove reaction by-products from the chamber.
  • a method for depositing an aluminum doped silicon nitride or gallium doped silicon nitride film via plasma enhanced atomic layer deposition or plasma enhanced ALD-like deposition comprising the steps of: a. providing a substrate into a reactor; b.
  • an aluminum or gallium precursor selected from the group consisting of AICI 3 , trimethylaluminum (TMA), methylaluminum chloride, triethylaluminum, tris(dimethylamino)aluminum (TDMAA), tris(dimethylamino)aluminum (TDMAA), tris(diethylamino)aluminum (TDEAA), gallium chloride, trimethylgallium, triethylgallium, tris(dimethylamino)gallium tris(ethylmethylamino)gallium,
  • tris(diethylamino)gallium under process conditions sufficient to interact with the substrate (e.g., react the aluminum precursor and provide a chemisorbed layer);
  • introducing into the reactor a plasma containing source to react with at least a portion of the chemisorbed layer and provide at least one reactive site wherein the plasma is generated at a power density ranging from about 0.01 to about 1 .5 W/cm 2 ; e. purging the reactor with a purge gas;
  • organoaminosilane precursor represented by the following Formulae I through IV below:
  • R 1 is selected from a linear d to C 10 alkyl group, a branched C 3 to C 10 alkyl group, a linear or branched C 3 to Ci 0 alkenyl group, a linear or branched C 3 to Ci 0 alkynyl group, a Ci to C 6 dialkylamino group, an electron withdrawing group, a C 6 to C 10 aryl group, a Ci to C 10 alkyl silyl group, and a silyl group;
  • the plasma containing source may be introduced into the reactor in the form of at least one nitrogen source and/or may be present incidentally in the other precursors used in the deposition process.
  • Suitable nitrogen-containing source gases may include, for example, ammonia, monoalkylhydrazine, dialkylhydrazine, nitrogen plasma,
  • the plasma is selected from the group consisting of hydrogen plasma, helium plasma, neon plasma, argon plasma, xenon plasma, hydrogen/helium plasma, hydrogen/argon plasma and mixtures thereof.
  • steps b to i are repeated to provide the film with a thickness ranging from about 0.1 to about 500 A, or from about 0.1 to about 5 A, or from about 0.1 to about 10 A, or about 0.1 to about 50 A, or 0.1 to 100 A.
  • steps b to e can be repeated many times before step f to i create a nanolaminate structure comprising an alternating aluminum nitride and silicon nitride with lower aluminum content (i.e. Al content is 10% or less bases XPS measurement).
  • steps f to i are repeated many times to create nanolaminate structure comprising alternating aluminum nitride and silicon nitride with higher aluminum content (e.g., Al content is 10% or higher bases XPS measurement).
  • the plasma containing source may be introduced into the reactor in the form of at least one nitrogen source and/or may be present incidentally in the other precursors used in the deposition process.
  • a plasma comprising hydrogen selected from the group consisting of hydrogen plasma, hydrogen/helium, hydrogen/argon plasma, hydrogen/neon plasma and mixtures thereof can be inserted before step d or h to help removing hydrocarbon generated from the reaction between the aluminum or boron precursor and the surface.
  • the plasma comprises a non- hydrogen plasma.
  • the aluminum precursor in step b can be replaced with a metal precursor to provide a metal doped silicon and nitrogen containing dielectric film as opposed to conventional metal doped silicon and nitrogen containing conducting film such as TiSiN with less than 10 at. % silicon content deposited from tetrakis(dimethylamino)titanium (TDMAT), silane and ammonia.
  • the metal precursor can be selected from the group consisting of zirconium chloride (ZrCI 4 , tetrakis(dimethylamino)zirconium (TDMAZ),
  • TDEAZ tetrakis(diethylamino)zirconium
  • TEMAZ tetrakis(ethylmethylamino)zirconium
  • Tris(ethylmethylamino)(ethylcyclopentadienyl)hafnium Titanium chloride (TiCI 4 ), tetrakis(dimethylamino)titanium (TDMAT), tetrakis(diethylamino)titanium (TDEAT), tetrakis(ethylmethylamino)titanium (TEMAT), tantalum chloride (TaCI 5 ), tert-butylimino tri(diethylamino)tantalum (TBTDET), tert-butylimino tri(dimethylamino)tantalum
  • TBTDMT tert-butylimino tri(ethylmethylamino)tantalum
  • EITDET ethylimino tri(diethylamino)tantalum
  • EITDMT ethylimino tri(ethylmethylamino)tantalum
  • EITEMT tert-amylimino
  • the metal precursor may be introduced into the reactor after
  • organoaminosilane precursor i.e., the organoaminosilane precursor is introduced in step b while the metal precursor is introduced in step f.
  • a method for depositing gallium doped silicon nitride or aluminum doped silicon carbonitride film via plasma enhanced atomic layer deposition or plasma enhanced ALD-like deposition comprising the steps of:
  • introducing into the reactor at least one metal precursor is selected from the group consisting of AICI 3 , trimethylaluminum (TMA), triethylaluminum, methylaluminum chloride, tris(dimethylamino)aluminum (TDMAA), tris(dimethylamino)aluminum (TDMAA), tris(diethylamino)aluminum (TDEAA), gallium chloride, trimethylgallium, triethylgallium, tris(dimethylamino)gallium, tris(ethylmethylamino)gallium, tris(diethylamino)gallium and other volatile aluminum or gallium precursors;
  • R 1 is selected from a linear d to C 10 alkyl group, a branched C 3 to C 10 alkyl group, a linear or branched C 3 to Ci 0 alkenyl group, a linear or branched C 3 to Ci 0 alkynyl group, a Ci to C 6 dialkylamino group, an electron withdrawing group, a C 6 to Ci 0 aryl group, a Ci to C 10 alkyl silyl group, and a silyl group;
  • organoaminosilane precursor interacts (e.g., reacts on) with at least a portion of the surface of the substrate to provide a chemisorbed layer;
  • the plasma containing source may be introduced into the reactor in the form of at least one nitrogen source and/or may be present incidentally in the other precursors used in the deposition process.
  • Suitable nitrogen-containing source gases may include, for example, ammonia, monoalkylhydrazine, dialkylhydrazine, nitrogen plasma, nitrogen/hydrogen, nitrogen/helium, nitrogen/argon plasma, ammonia plasma, nitrogen/ammonia plasma, ammonia/helium plasma, ammonia/argon plasma, ammonia/nitrogen plasma, NF 3 plasma, organoamine plasma, and mixtures thereof.
  • the plasma is selected from the group consisting of hydrogen plasma, helium plasma, neon plasma, argon plasma, xenon plasma, hydrogen/helium plasma, hydrogen/argon plasma and mixtures thereof.
  • the metal precursor may be introduced into the reactor after organoaminosilane precursor, i.e., the organoaminosilane precursor is introduced in step b while the metal precursor is introduced in step f .
  • the above steps define one cycle for the method described herein; and the cycle can be repeated until the desired thickness of the film is obtained.
  • the steps of the methods described herein may be performed in a variety of orders, may be performed sequentially or concurrently (e.g., during at least a portion of another step), and any combination thereof.
  • the respective step of supplying the precursors and plasma containing source may be performed by varying the duration of the time for supplying them to change the stoichiometric composition of the resulting nitride film, although always using nitrogen in less than a stoichiometric amount relative to the available Group 4, 5, 6, 13 metal or metalloid.
  • the resultant Group 4, 5, 6, 13 metal or metalloid doped silicon nitride films or coatings can be exposed to a post-deposition treatment such as, but not limited to, a plasma treatment, chemical treatment, ultraviolet light exposure, electron beam exposure, and/or other treatments to affect one or more properties of the film.
  • a post-deposition treatment such as, but not limited to, a plasma treatment, chemical treatment, ultraviolet light exposure, electron beam exposure, and/or other treatments to affect one or more properties of the film.
  • the film or the as-deposited film is subjected to a treatment step.
  • the treatment step can be conducted during at least a portion of the deposition step, after the deposition step, and combinations thereof.
  • Exemplary treatment steps include, without limitation, treatment via high temperature thermal annealing ; plasma treatment; ultraviolet (UV) light treatment; laser; electron beam treatment and combinations thereof to affect one or more properties of the film.
  • the films deposited with the silicon precursors having one or two Si-C-Si linkages described herein when compared to films deposited with previously disclosed silicon precursors under the same conditions, have improved properties such as, without limitation, a wet etch rate that is lower than the wet etch rate of the film before the treatment step or a density that is higher than the density prior to the treatment step.
  • as-deposited films are intermittently treated.
  • These intermittent or mid-deposition treatments can be performed, for example, after each ALD cycle, after every a certain number of ALD, such as, without limitation, one (1 ) ALD cycle, two (2) ALD cycles, five (5) ALD cycles, ten (10) or more ALD cycles, fifty (50) or more, hundred (100) or more, five hundred (500) or more.
  • the annealing temperature is at least 100°C or greater than the deposition temperature. In this or other embodiments, the annealing temperature ranges from about 400°C to about 1000°C. In this or other embodiments, the annealing treatment can be conducted in a vacuum ( ⁇ 760 Torr), inert environment or in oxygen containing environment (such as H 2 0, N 2 0, N0 2 or 0 2 ).
  • film is exposed to broad band UV or, alternatively, an UV source having a wavelength ranging from about 150 nanometers (nm) to about 400 nm.
  • the as- deposited film is exposed to UV in a different chamber than the deposition chamber after a desired film thickness is reached.
  • the plasma source is selected from the group consisting of hydrogen plasma, plasma comprising hydrogen and helium, plasma comprising hydrogen and argon, helium plasma, argon plasma, nitrogen plasma, ammonia plasma, and combination thereof.
  • the method described herein may be used to deposit a Group 4, 5, 6, 13 metal or metalloid doped silicon nitride film on at least a portion of a substrate.
  • suitable substrates include but are not limited to, silicon, germanium, silicon/germanium, Si0 2 , Si 3 N 4 , OSG, FSG, silicon carbide, hydrogenated silicon carbide, silicon nitride, hydrogenated silicon nitride, silicon carbonitride, hydrogenated silicon carbonitride, boronitride, anti reflective coatings, photoresists, a flexible substrate such as IGZO, organic polymers, porous organic and inorganic materials, metals such as copper and aluminum, and diffusion barrier layers such as but not limited to TiN, Ti(C)N, TaN, Ta(C)N, Ta, W, or WN.
  • the films are compatible with a variety of subsequent processing steps such as, for example, chemical mechanical planarization (CMP) and anisotropic etching processes.
  • CMP chemical mechanical planarization
  • the deposited films have applications, which include, but are not limited to, computer chips, optical devices, magnetic information storages, coatings on a supporting material or substrate, microelectromechanical systems (MEMS), nanoelectromechanical systems, thin film transistor (TFT), light emitting diodes (LED), organic light emitting diodes (OLED), IGZO, and liquid crystal displays (LCD).
  • MEMS microelectromechanical systems
  • TFT thin film transistor
  • LED light emitting diodes
  • OLED organic light emitting diodes
  • IGZO liquid crystal displays
  • Typical RF power used was 125W over electrode area of 150 mm wafer susceptor to provide a power density of 0.7 W/cm 2 .
  • the film depositions comprised the steps listed in Table 1 for thermal ALD and plasma enhanced ALD (PEALD), respectively.
  • % non-uniformity ((max thickness - min thickness)/(2 * average (avg) thickness))x 100.
  • Film structure and composition were analyzed using Fourier Transform Infrared (FTIR) spectroscopy, X-Ray Photoelectron Spectroscopy (XPS) and dynamic Secondary Ion Mass Spectrometry (DSIMS). The density for the films was measured with X-ray Reflectivity (XRR).
  • FTIR Fourier Transform Infrared
  • XPS X-Ray Photoelectron Spectroscopy
  • DIMS dynamic Secondary Ion Mass Spectrometry
  • Comparable Example 1 PEALD silicon nitride film using di-iso-propylaminosilane (DIPAS) and nitrogen plasma
  • ALD cycle was comprised of the following process steps:
  • organoaminosilane pulse 1 second
  • Example 1 PEALD aluminum doped silicon nitride film using trimethylaluminum (TMA), di-iso-propylaminosilane (DIPAS) and nitrogen plasma
  • the silicon wafer was loaded into the CN-1 reactor equipped with showerhead design with 13.56 MHz direct plasma and heated to 300°C with chamber pressure of 2 torr.
  • the precursors, trimethylaluminum (TMA) as the metal precursor and di-iso-propylaminosilane (DIPAS) as organoaminosilane precursor, were delivered using the vapor draw method into the reactor.
  • Nitrogen plasma was used as plasma source.
  • silicon nitride helps slightly to improve the growth rate of silicon nitride, i.e., increasing the growth rate from 0.16 A to 0.19 A/cycle.
  • the step coverage for silicon nitride middle 1 1 % and bottom 32%.
  • Tnmethylaluminum (TMA) was used as metal precursor and nitrogen plasma was used as plasma source.
  • TMA Tnmethylaluminum
  • ⁇ S TMA pulse 0.1 second
  • Steps b to e were repeated for 100 cycles, 200 cycles, and 400 cycles respectively.
  • the growth rate for aluminum nitride was calculated from the graph of thickness vs number of cycles as 0.58 A/cycle.
  • Comparable Example 2b PEALD silicon nitride film using di-iso-propylaminosilane (DIPAS) and nitrogen plasma
  • the silicon wafer was loaded into the CN-1 reactor equipped with showerhead design with 13.56 MHz direct plasma and heated to 300°C with chamber pressure of 2 torr.
  • Di-iso-propylaminosilane (DIPAS) was used as silicon precursor and nitrogen plasma was used as plasma source.
  • the ALD cycle was as following:
  • DIPAS/purge/plasma/purge 1.0s/10s/10 * s/10s.
  • the cycles were repeated for 250 cycles, 500 cycles, 1000, and 1500 cycles respectively.
  • the growth rate for silicon nitride was calculated from the graph of thickness vs number of cycles as 0.15 A/cycle.
  • Example 2 PEALD aluminum doped silicon nitride film using trimethylaluminum (TMA), di-iso-propylaminosilane (DIPAS), and nitrogen plasma
  • the silicon wafer was loaded into the CN-1 reactor equipped with showerhead design with 13.56 MHz direct plasma and heated to 300°C with chamber pressure of 2 torr.
  • Trimethylaluminum (TMA) as metal precursor and di-iso- propylaminosilane (DIPAS) as organoaminosilane precursor were delivered using vapor draw method into the reactor.
  • the ALD cycle was comprised of the process steps provided in Table 1 and using the following process parameters. a. Prepare the reactor and load wafer
  • Plasma pulse 5 seconds
  • the super cycle is repeated 50 times (i.e.
  • the silicon wafer was loaded into the CN-1 reactor equipped with showerhead design with 13.56 MHz direct plasma and heated to 300°C with chamber pressure of 2 torr. Trimethylaluminum (TMA) was used as metal precursor and nitrogen plasma was used as plasma source.
  • TMA Trimethylaluminum
  • the ALD cycle was conducted using the following process parameters.
  • ⁇ S TMA pulse 0.5 second
  • Steps b to e were repeated for 100 cycles, 200 cycles, and 300 cycles respectively.
  • the growth rate for aluminum nitride was calculated from the graph of thickness vs number of cycles as 0.72 A/cycle.
  • Example 3 PEALD aluminum doped silicon nitride film using trimethylaluminum (TMA) and di-iso-propylaminosilane (DIPAS), and nitrogen plasma
  • the step coverage middle 68% and bottom 82%; this demonstrates that introducing the metal precursor further enhances the step coverage.
  • the secondary-ion mass spectrometry (SIMS) measurement of deposited aluminum doped silicon nitride shows Si, 31 at%, Al, 8.5 at%, N, 47 at%, C, 2 at%, 0,1 .7 at%, and H,9.5 at%.
  • TDMAA tris(dimethylamino)aluminum
  • showerhead design with 13.56 MHz direct plasma and heated to 300°C with chamber pressure of 2 torr.
  • the ALD cycle was conducted using the following process parameters.
  • TDMAA pulse 2 seconds
  • Steps b to e were repeated for 100 cycles, 200 cycles, and 300 cycles respectively.
  • the growth rate for aluminum nitride was calculated from the graph of thickness vs number of cycles as 0.60 A/cycle.
  • Example 4 PEALD aluminum doped silicon nitride film using
  • TDMAA tris(dimethylamino)aluminum
  • DIPAS di-iso-propylaminosilane
  • showerhead design with 13.56 MHz direct plasma and heated to 300°C with chamber pressure of 2 torr.
  • one super cycle consisting of aluminum nitride having steps b to e are repeated once, followed by steps f to i for 10 times (i.e.
  • TDMAA tris(dimethylamino)aluminum
  • the silicon wafer was loaded into the CN-1 reactor equipped with showerhead design with 13.56 MHz direct plasma and heated to 300°C with chamber pressure of 2 torr.
  • Tris(dimethylamino)aluminum (TDMAA) as metal precursor ammonia plasma was used as plasma source.
  • the ALD cycle was conducted using the following process parameters.
  • TDMAA pulse 2 seconds
  • Steps b to e were repeated for 100 cycles, 200 cycles, and 300 cycles respectively.
  • the growth rate for aluminum nitride was calculated from the graph of thickness vs number of cycles as 0.74 A/cycle.
  • Comparable Example 5b PEALD silicon nitride film using di-iso-propylaminosilane (DIPAS) and ammonia plasma
  • DIPAS/purge/plasma/purge 1.0s/10s/10 * s/15s was repeated for 500 cycles to provide 23 A corresponding to a silicon nitride growth rate of about 0.046 A/cycle.
  • Example 5 PEALD aluminum doped silicon nitride film using
  • TDMAA tris(dimethylamino)aluminum
  • DIPAS di-iso-propylaminosilane
  • showerhead design with 13.56 MHz direct plasma and heated to 300°C with chamber pressure of 2 torr.
  • Tris(dimethylamino)aluminum (TDMAA) as metal precursor and di-iso- propylaminosilane (DIPAS) as organoaminosilane precursor were delivered using vapor draw method into the reactor.
  • Ammonia plasma was used for plasma.
  • one super cycle consisting of aluminum nitride having steps b to e in Table 1 are repeated once, followed by steps f to i in Table 1 for 10 times (i.e.
  • the super cycle is repeated 100 times (i.e. (aluminum nitride:
  • the secondary-ion mass spectrometry (SIMS) measurement of deposited aluminum doped silicon nitride shows Si, 21 .2 at%, Al, 2.6 at%, N, 42 at%, C, 0.01 at%, O, 5.5 at%, 1-1,18.6 at%.
  • Comparable Example 6a PEALD silicon nitride film using bis(tert-butylamino)silane (BTBAS) and nitrogen plasma
  • the silicon wafer was loaded into the CN-1 reactor equipped with showerhead design with 13.56 MHz direct plasma and heated to 300°C with chamber pressure of 2 torr.
  • Bis(tert-butylamino)silane (BTBAS) as organoaminosilane precursor ammonia plasma was used as plasma source.
  • the cycle consisting of
  • BTBAS/purge/plasma/purge 1 .0s/10s/10 * s/10s was repeated for 500, 1000, and 1500 cycles respectively.
  • the growth rate for aluminum nitride was calculated from the graph of thickness vs number of cycles as 0.28 A/cycle.
  • Example 6 PEALD aluminum doped silicon nitride film using trimethylaluminum (TMA), bis(tert-butylamino)silane (BTBAS), and nitrogen plasma
  • the silicon wafer was loaded into the CN-1 reactor equipped with showerhead design with 13.56 MHz direct plasma and heated to 300°C with chamber pressure of 2 torr.
  • Trimethylaluminum (TMA) as metal precursor and bis(tert- butylamino)silane (BTBAS) as organoaminosilane precursor were delivered using vapor draw method into the reactor.
  • the secondary-ion mass spectrometry (SIMS) measurement of deposited aluminum doped silicon nitride shows Si, 33.3 at%, Al, 7.1 at%, N, 45.2 at%, C, 2.4 at%, O, 0.7 at%, H.1 1 .3 at%.
  • TMA Trimethylaluminum
  • ⁇ S TMA pulse 0.5 seconds
  • Steps b to e were repeated for 200 cycles and 300 cycles respectively.
  • the growth rate for aluminum nitride was calculated from the graph of thickness vs number of cycles as 1 .21 A/cycle.
  • BTBAS bis(tert-butylaminosilane
  • ammonia plasma was used as plasma source.
  • the cycle consisting of BTBAS/purge/plasma/purge 1 .0s/10s/10 * s/15s was repeated for 500, 1000, and 1500 cycles.
  • the growth rate for silicon nitride was calculated from the graph of thickness vs number of cycles as 0.045 A/cycle.
  • Example 7 PEALD aluminum doped silicon nitride film using trimethylaluminum (TMA), bis(tert-butylamino)silane (BTBAS), and ammonia plasma
  • TMA Trimethylaluminum
  • BBAS bis(tert- butylamino)silane
  • Ammonia plasma was used as plasma.
  • one super cycle consisting of aluminum nitride having steps b to e in Table 1 are repeated once, followed by steps f to i in Table 1 for 10 times (i.e.
  • the step coverage: middle 88% and bottom 91 % also demonstrates that introducing TMA further enhances the step coverage.
  • Comparable Example 8a PEALD silicon nitride film using di-iso-propylaminodisilane (DIPADS) and nitrogen plasma
  • DIPADS Di-iso-propylaminodisilane
  • DIPADS/purge/plasma/purge 1.0s/10s/15 * s/5s.
  • the cycles were repeated for 250 cycles, 500 cycles, and 750 cycles respectively.
  • the growth rate for silicon nitride was calculated from the graph of thickness vs number of cycles as 0.38 A/cycle.
  • TMGa/purge/plasma/purge 0.5s/10s/15 * s/5s. The cycles were repeated for 100 cycles,200 cycles, and 400 cycles respectively.
  • the growth rate for gallium nitride was calculated from the graph of thickness vs number of cycles as 0.42 A/cycle.
  • Example 8 PEALD gallium doped silicon nitride film using trimethylgallium (TMGa), di- iso-propylaminodisilane (DIPADS), and nitrogen plasma
  • TMGa Trimethylgallium
  • DIPADS di-iso- propylaminodisilane
  • gallium doped silicon nitride 250A corresponding to a silicon nitride growth rate of about 0.48 A/cycle (about 28% increase compare to PEALD silicon nitride using only DIPADS) assuming 11 A gallium nitride, demonstrating significant improvement of growth rate of silicon nitride via alternating deposition of gallium nitride and silicon nitride, i.e. deposited gallium nitride layer boosts deposition of silicon nitride.
  • gallium doped silicon nitride 320A corresponding to a silicon nitride growth rate of about 0.56 A/cycle (about 47% increase compare to PEALD silicon nitride using only DIPADS) assuming 42 A gallium nitride, demonstrating significant improvement of growth rate of silicon nitride via alternating deposition of gallium nitride and silicon nitride, i.e. deposited gallium nitride layer boosts deposition of silicon nitride significantly.
  • TDMAT tetrakis(dimethylamino)titanium
  • the silicon wafer was loaded into the CN-1 reactor equipped with showerhead design with 13.56 MHz direct plasma and heated to 300°C with chamber pressure of 2 torr.
  • TDMAT was used as titanium precursor and nitrogen plasma was used as plasma source.
  • the growth rate for titanium nitride was calculated from the graph of thickness vs number of cycles as 1 .1 1 A/cycle.
  • Example 9 PEALD titanium doped silicon nitride film using
  • TDMAT tetrakis(dimethylamino)titanium
  • DIPAS di-iso-propylaminosilane
  • the silicon wafer was loaded into the CN-1 reactor equipped with showerhead design with 13.56 MHz direct plasma and heated to 300°C with chamber pressure of 2 torr.
  • TDMAT tetrakis(dimethylamino)titanium
  • DIPAS di- iso-propylaminosilane
  • titanium doped silicon nitride 230 A corresponding to a silicon nitride growth rate of about 0.24 A/cycle based on XRF measurement of 36 A of titanium nitride, demonstrating significant improvement of growth rate of silicon nitride via alternating deposition of titanium nitride and silicon nitride, i.e. deposited titanium nitride layer boosts deposition of silicon nitride.
  • titanium doped silicon nitride 285 A corresponding to a silicon nitride growth rate of about 0.28 A/cycle (about 26% increase compare to PEALD silicon nitride using only DIPAS) based on XRF measurement of 65 A of titanium nitride, demonstrating significant improvement of growth rate of silicon nitride via alternating deposition of titanium nitride and silicon nitride, i.e. deposited titanium nitride layer boosts deposition of silicon nitride
  • Example 10 PEALD titanium doped silicon nitride film using
  • TDMAT tetrakis(dimethylamino)titanium
  • BBAS bis(tert-butylamino)silane
  • nitrogen plasma tetrakis(dimethylamino)titanium
  • BTBAS bis(tert-butylamino)silane
  • showerhead design with 13.56 MHz direct plasma and heated to 300°C with chamber pressure of 2 torr.
  • Ar flow rate 50sccm
  • titanium doped silicon nitride 265 A corresponding to a silicon nitride growth rate of about 0.29 A/cycle ( about 26% increase compare to PEALD silicon nitride using only BTBAS) based on XRF measurement of 35 A of titanium nitride,
  • (BTBAS/purge/plasma/purge 1 .0s/10s/10 * s/10s for 20 cycles).
  • titanium doped silicon nitride 305 A corresponding to a silicon nitride growth rate of about 0.30 A/cycle (( about 30% increase compare to PEALD silicon nitride using only BTBAS) based on XRF measurement of 62 A of titanium nitride, demonstrating significant improvement of growth rate of silicon nitride via alternating deposition of titanium nitride and silicon nitride, i.e. deposited titanium nitride layer boosts deposition of silicon nitride

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