WO2011042882A2 - Vitesse de dépôt élevée de sio2 à l'aide d'un dépôt de couche atomique à température extra basse - Google Patents

Vitesse de dépôt élevée de sio2 à l'aide d'un dépôt de couche atomique à température extra basse Download PDF

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Publication number
WO2011042882A2
WO2011042882A2 PCT/IB2010/054544 IB2010054544W WO2011042882A2 WO 2011042882 A2 WO2011042882 A2 WO 2011042882A2 IB 2010054544 W IB2010054544 W IB 2010054544W WO 2011042882 A2 WO2011042882 A2 WO 2011042882A2
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WO
WIPO (PCT)
Prior art keywords
approximately
base
reaction chamber
seem
flow rate
Prior art date
Application number
PCT/IB2010/054544
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English (en)
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WO2011042882A3 (fr
Inventor
Katsuko Higashino
Kazutake Yanagita
Original Assignee
L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude
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Application filed by L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude filed Critical L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude
Publication of WO2011042882A2 publication Critical patent/WO2011042882A2/fr
Publication of WO2011042882A3 publication Critical patent/WO2011042882A3/fr

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Classifications

    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C16/40—Oxides
    • C23C16/401—Oxides containing silicon
    • C23C16/402—Silicon dioxide
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C16/44—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 method of coating
    • C23C16/455—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 method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
    • C23C16/45527—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
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C16/44—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 method of coating
    • C23C16/455—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 method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
    • C23C16/45527—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
    • C23C16/45534—Use of auxiliary reactants other than used for contributing to the composition of the main film, e.g. catalysts, activators or scavengers
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C16/44—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 method of coating
    • C23C16/455—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 method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
    • C23C16/45553—Atomic layer deposition [ALD] characterized by the use of precursors specially adapted for ALD

Definitions

  • the SiO 2 film is one of the most common thin films in an integrated circuit (IC).
  • IC integrated circuit
  • CVD chemical vapor deposition
  • ALD atomic layer deposition
  • extra low deposition temperatures are required to prevent oxidation of the interface and the decomposition of thermally unstable substrates.
  • Conformal Si0 2 films at low temperature may be used as sacrificial layers for double patterning masks.
  • ALD processes at lower temperatures tend to produce slower deposition rates than higher temperature process, resulting in lower throughput.
  • alkyl group refers to saturated functional groups containing exclusively carbon and hydrogen atoms.
  • alkyl group refers to linear, branched, or cyclic alkyl groups. Examples of linear alkyl groups include without limitation, methyl groups, ethyl groups, propyl groups, butyl groups, etc. Examples of branched alky!s groups include without limitation, f-butyl. Examples of cyclic alkyl groups include without limitation, cyclopropyl groups, cyclobutyl groups, cyclopentyl groups, cyclohexyl groups, etc.
  • the term "independently" when used in the context of describing R groups should be understood to denote that the subject R group is not only independentiy selected relative to other R groups bearing the same or different subscripts or superscripts, but is also independently selected relative to any additional species of that same R group.
  • the two or three R 1 groups may, but need not be identical to each other or to R 2 or to R 3 .
  • values of R groups are independent of each other when used in different formulas.
  • Step a) of the method comprises simultaneously supplying into a reaction chamber a pulse of a first base and a silicon chloride precursor.
  • the first base and the silicon chloride precursor are each supplied at a flow rate of approximately 1 seem to approximately 100 seem.
  • step b) the reaction chamber is purged.
  • a pulse of a second base and an oxidant selected from ozone or remote plasma activated 0 2 are simultaneously supplied into the reaction chamber in step c).
  • the second base is supplied at a flow rate of approximately 1 to approximately 100 seem.
  • the oxidant is suppiied at a flow rate of approximately 10 to approximately 500 seem.
  • step d) the reaction chamber is purged.
  • the disclosed methods may include one or more of the following aspects:
  • the silicon chloride precursor being selected from the group consisting of dichlorosi!ane (SiH 2 Cb), trichiorosilane (SiHCI 3 ), tetrachlorosilane (SiCI ), hexachlorodisilane (SbCle), and mixtures thereof;
  • reaction chamber having a pressure of approximately 0.1 to
  • reaction chamber having a temperature approximately 50°C and approximately 200°C, preferably between approximately 50°C and approximately 150°C, and more preferably between approximately 50°C and approximately 100°C;
  • the first and second base being independently selected from the group consisting of tertiary amines having the formula NRR'R", cyclic amines, and imines having the formula NR -R", wherein each of R, R ⁇ and R" is an alkyl group which may be bonded each other; and the first and second base being independently selected from the group consisting of trimethylamine, triethy!amine, pyridine, and mixtures thereof.
  • FIG 1 is a graph illustrating the difference in deposition rates between one embodiment of the disclosed method and the prior art.
  • FIG 2 is a graph illustrating the difference in deposition rates between an alternate embodiment of the disclosed method and the prior art.
  • the methods have particular utility in depositing sacrificial layers for double patterning masks which, to reduce the design size, need to deposit S1O2 film at an extra low temperature.
  • Ozone and RP O2 have the advantage of stronger oxidative power and are easier to purge from the deposition chamber than H 2 O.
  • H 2 O is difficult to purge, especially at lower temperatures, due to adsorption on the wall of the deposition chamber.
  • ozone and RP O 2 may be purged from the chamber easily.
  • the disclosed processes are expected to improve the throughput dramatically.
  • the disclosed processes also result in greatly enhanced deposition rates.
  • the disclosed processes form a silicon oxide layer on a substrate (e.g., a semiconductor substrate or substrate assembly) using an oxidant, a base, and a silicon chloride precursor.
  • the processes may be useful in the manufacture of semiconductor, photovoltaic, LCD-TFT, or flat panel type devices.
  • the silicon chloride precursor has the formula Si a H b Cl c , wherein b+c-2a+2.
  • Exemplary precursors include dichlorosilane (SiH 2 CI 2 ),
  • the selected base has an affinity with hydrogen chloride.
  • exemplary bases include trimethylamine, triethylamine, pyridine, or mixtures thereof.
  • the oxidant is ozone or remote plasma activated
  • the disclosed processes form a silicon-oxide layer on a substrate at low temperature using an atomic layer deposition process.
  • the method includes simultaneously suppiying into a reaction chamber a pulse of a first base and the silicon chloride precursor, the first base and the silicon chloride precursor each being supplied at a flow rate of approximately 1 to
  • the first and second base may be the same, for example trimethyl amine.
  • the first base may be trimethyl amine and the second base may be pyridine. This process may be repeated until a silicon oxide layer having the desired thickness is obtained.
  • the desired thickness will vary depending upon the intended use of the silicon oxide layer.
  • the reaction chamber may be any enclosure or chamber within a device in which deposition methods take place such as, and without iimitation, a parallel-plate type reaction chamber, a cold-wall type reaction chamber, a hot-wall type reaction chamber, a single-wafer reaction chamber, a multi- wafer reaction chamber, or other types of deposition systems under conditions suitable to cause the precursors to react and form the layers.
  • the temperature and the pressure within the reaction chamber are held at conditions suitable for the deposition process.
  • the pressure in the reaction chamber may be held between approximately 0.1 Torr and approximately 10 Torr, preferably between approximately 0.2 Torr and approximately 10 Torr, and more preferably between approximately 1 Torr and approximately 10 Torr, as required per the deposition parameters.
  • the temperature in the reaction chamber may be held between approximately 50°C and approximately 200°C, preferably between
  • the reaction chamber contains one or more substrates onto which the thin films will be deposited.
  • the one or more substrates may be any suitable substrate used in semiconductor, photovoltaic, flat panel or LCD-TFT device manufacturing. Examples of suitable substrates include without Iimitation silicon substrates, silica substrates, silicon nitride substrates, silicon oxy nitride substrates, tungsten substrates, titanium nitride, tantalum nitride, or combinations thereof. Additionally, substrates comprising tungsten or noble metals (e.g. platinum, palladium, rhodium or gold) may be used.
  • the substrate may also have one or more layers of differing materials already deposited upon it from a previous manufacturing step. The silicon chloride precursor, the base, and the oxidant may be obtained in gas form. Therefore, they may be directly introduced into the reaction chamber.
  • the remote piasma activated (RP) oxygen is produced by ionizing O2 in a remote plasma source which contains high voltage electrodes used to ionize oxygen gas.
  • the remote plasma may be generated with a power ranging from approximately 1 kW to approximately 10 kW, more preferably from approximately 2.5 kW to approximateiy 7.5 kW.
  • a mixture of oxygen and O radicals are introduced into the reaction chamber.
  • the O ions remain trapped in the remote plasma source, thereby preventing any damage to the substrate.
  • Remote plasma units are commercially available, such as the MKS instruments' R * evoiution ® reactive gas generator.
  • Solid or liquid silicon chloride precursors may be supplied either in neat form or in a blend with a suitable solvent, such as ethyl benzene, xylenes, mesitylene, decane, dodecane.
  • a suitable solvent such as ethyl benzene, xylenes, mesitylene, decane, dodecane.
  • the silicon chloride precursor may be present in varying concentrations in the solvent.
  • the neat or blended silicon chloride precursor is supplied into the reaction chamber in vapor form.
  • the vapor form may be produced by vaporizing the neat or blended precursor solution through a conventional vaporization step such as direct vaporization, distillation, or by bubbling.
  • the neat or blended precursor may be fed in liquid state to a vaporizer where it is vaporized before it is introduced into the reaction chamber.
  • the neat or blended precursor may be vaporized by passing a carrier gas into a container containing the silicon chloride precursor or by bubbling the carrier gas into the silicon chloride precursor.
  • the carrier gas may include, but is not limited to, Ar, He, N2,and mixtures thereof.
  • Bubbling with a carrier gas may aiso remove any dissolved oxygen present in the neat or blended precursor solution.
  • the carrier gas and silicon chloride precursor are then introduced into the reaction chamber as a vapor.
  • the container of silicon chloride precursor may be heated to a temperature that permits the precursor to be in its liquid phase and to have a sufficient vapor pressure.
  • the container may be maintained at temperatures in the range of, for example, approximately 0°C to
  • the temperature of the container may be adjusted in a known manner to control the amount of precursor vaporized.
  • the silicon chloride precursor and the base are simultaneously supplied into the reaction chamber.
  • the silicon chloride precursor and the base may be mixed together prior to introduction into the reaction chamber.
  • the base and the silicon chloride precursor may be separately, but simultaneously, introduced into the reaction chamber.
  • a pulse of the base and the silicon chloride precursor is supplied into the reaction chamber at a flow rate of approximately 1 to approximately 100 seem.
  • the flow rate of the base may be greater than the flow rate of the silicon chloride precursor.
  • Excess base and precursor are then removed from the reaction chamber by purging with an inert gas, such as, for example, Ar.
  • the purge may last for the same duration as the pulse of the base and the silicon chloride precursor.
  • the reaction pressure during the step of supplying the precursor may be higher than during the purge step.
  • the oxidant and the base are simultaneously supplied into the reaction chamber.
  • the oxidant and the base may be mixed together prior to introduction into the reaction chamber.
  • the base and the oxidant are introduced separately, but simultaneously, into the reaction chamber.
  • a pulse of the base and the oxidant is supplied into the reaction chamber.
  • the base is supplied at a flow rate of approximately 1 to
  • the oxidant is supplied at a flow rate of
  • Excess base and oxidant are then removed from the reaction chamber by purging with an inert gas, such as, for example, Ar.
  • the purge may last for the same duration as the pulse of the base and the oxidant.
  • Si0 2 film was deposited by ALD using HCDS, ozone, and
  • TMA trimethylamine
  • the reaction chamber was controlled at 2 Torr, 70°C, and 100 seem of Ar was continuously flowing.
  • the deposition process included the following steps: 1 ) supply a pulse of 1 seem of HCDS and 15 seem of TMA to the reaction chamber for 10 seconds, 2) purge the excess precursors by slm of Ar for 0 seconds, 3) supply 4.6 seem of ozone/200 seem of O2 and 5 seem of TMA to the chamber for 20 seconds 4) purge excess precursors by 1 slm of Ar for 20 seconds.
  • the sequence from 1 ) to 4) was repeated until the deposited layer achieved suitable thickness.
  • the method was repeated with water replacing ozone.
  • the method was repeated with no trimethylamine.
  • the results are provided in FIG 1 .
  • the results show that higher deposition rates are achieved from the combination of ozone with trimethylamine as compared to water with trimethylamine and ozone alone. All values contain ⁇ 0.25A/cycle as natural oxide layer. The value of 0 3 without TMA is equal to non-tested sample.
  • Si0 2 film was deposited by ALD using HCDS, remote plasma activated O2, and trimethylamine (TMA).
  • the reaction chamber was controlled at 2 Torr, 70°C, and 100 seem of Ar was continuously flowing.
  • the deposition process included the following steps: 1 ) supply a pulse of 1 seem of HCDS and 15 seem of TMA to the reaction chamber for 10 seconds, 2) purge the excess precursors by 1 slm of Ar for 10 seconds, 3) supply remote plasma activated 200 seem of 0 2 and 15 seem of TMA and 1 slm of Ar to the chamber for 20 seconds 4) purge the excess precursors by 1 slm of Ar for 20 seconds.
  • the sequence from 1 ) to 4) was repeated until the deposited layer achieved suitable layer thickness.
  • the method was repeated with water replacing ozone.
  • the method was repeated with no trimethylamine.
  • the results are provided in FIG 2.
  • the results show that higher deposition rates are achieved from the combination of activated 0 2 with trimethylamine as compared to water with trimethylamine and activated 0 2 alone. All values contain ⁇ 0.25A/cyc!e as natural oxide layer.
  • the value of plasma activated 0 2 can oxidize Si substrate, so plasma activated 0 2 without TMA contains natural Si0 2 and oxidized substrate at interface.

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Formation Of Insulating Films (AREA)

Abstract

L'invention concerne des procédés de dépôt de couche atomique à basse température pour former des films de SiO2 à l'aide d'un précurseur de chlorure de silicium, d'un oxydant, et d'une base.
PCT/IB2010/054544 2009-10-07 2010-10-07 Vitesse de dépôt élevée de sio2 à l'aide d'un dépôt de couche atomique à température extra basse WO2011042882A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US24952209P 2009-10-07 2009-10-07
US61/249,522 2009-10-07

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Publication Number Publication Date
WO2011042882A2 true WO2011042882A2 (fr) 2011-04-14
WO2011042882A3 WO2011042882A3 (fr) 2011-09-01

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PCT/IB2010/054544 WO2011042882A2 (fr) 2009-10-07 2010-10-07 Vitesse de dépôt élevée de sio2 à l'aide d'un dépôt de couche atomique à température extra basse

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014183218A (ja) * 2013-03-19 2014-09-29 Hitachi Kokusai Electric Inc 半導体装置の製造方法、基板処理装置及びプログラム
US9941123B1 (en) 2017-04-10 2018-04-10 Lam Research Corporation Post etch treatment to prevent pattern collapse
CN109811329A (zh) * 2019-03-19 2019-05-28 合肥安德科铭半导体科技有限公司 一种氧化物薄膜的低温原子层沉积方法
US10600648B2 (en) 2017-04-20 2020-03-24 Lam Research Corporation Silicon-based deposition for semiconductor processing

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7084076B2 (en) 2003-02-27 2006-08-01 Samsung Electronics, Co., Ltd. Method for forming silicon dioxide film using siloxane

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100505668B1 (ko) * 2002-07-08 2005-08-03 삼성전자주식회사 원자층 증착 방법에 의한 실리콘 산화막 형성 방법

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7084076B2 (en) 2003-02-27 2006-08-01 Samsung Electronics, Co., Ltd. Method for forming silicon dioxide film using siloxane

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014183218A (ja) * 2013-03-19 2014-09-29 Hitachi Kokusai Electric Inc 半導体装置の製造方法、基板処理装置及びプログラム
US9548198B2 (en) 2013-03-19 2017-01-17 Hitachi Kokusai Electric Inc. Method of manufacturing semiconductor device, substrate processing apparatus, and recording medium
US9941123B1 (en) 2017-04-10 2018-04-10 Lam Research Corporation Post etch treatment to prevent pattern collapse
US10600648B2 (en) 2017-04-20 2020-03-24 Lam Research Corporation Silicon-based deposition for semiconductor processing
CN109811329A (zh) * 2019-03-19 2019-05-28 合肥安德科铭半导体科技有限公司 一种氧化物薄膜的低温原子层沉积方法

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