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WO2005113167A1 - Compositions et procédés pour sécher des tranches imprimées par séchage durant la fabrication de circuits imprimés - Google Patents

Compositions et procédés pour sécher des tranches imprimées par séchage durant la fabrication de circuits imprimés Download PDF

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Publication number
WO2005113167A1
WO2005113167A1 PCT/US2004/014353 US2004014353W WO2005113167A1 WO 2005113167 A1 WO2005113167 A1 WO 2005113167A1 US 2004014353 W US2004014353 W US 2004014353W WO 2005113167 A1 WO2005113167 A1 WO 2005113167A1
Authority
WO
WIPO (PCT)
Prior art keywords
composition
water
contacting
supercritical fluid
carried out
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/US2004/014353
Other languages
English (en)
Inventor
Chongying Xu
Michael Korzenski
Thomas H. Baum
Alexander Borovik
Eliodor G. Ghenciu
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.)
Advanced Technology Materials Inc
Original Assignee
Advanced Technology Materials 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 Advanced Technology Materials Inc filed Critical Advanced Technology Materials Inc
Priority to PCT/US2004/014353 priority Critical patent/WO2005113167A1/fr
Priority to EP04751653A priority patent/EP1765526A4/fr
Priority to JP2007511332A priority patent/JP2007536730A/ja
Priority to CNA2004800432546A priority patent/CN1960813A/zh
Publication of WO2005113167A1 publication Critical patent/WO2005113167A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
    • B08B7/0021—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by liquid gases or supercritical fluids

Definitions

  • the present invention relates to compositions and methodology for drying patterned wafers during the manufacture of integrated circuitry products.
  • patterned images are often dried with hexanes and nitrogen, or with isopropanol and nitrogen.
  • These conventional drying methods do not work well for images having a critical dimension width ⁇ 100nm and aspect ratio greater than 1.
  • the surface tension of isopropanol or hexane pulls the images together, leading to collapse of the lithographic resist and loss of the patterned image, or to degradation of the polymeric resist.
  • the art therefore is in need of improved techniques for drying of patterned wafers which effect complete removal of water, alcohols, etc., without causing collapse of the pattern features or other adverse effects on the patterned wafers.
  • the present invention relates to compositions and methodology for drying of patterned wafers to remove water, alcohols, etc. from the wafer, without causing collapse of the pattern or other adverse effect on the wafer article.
  • the present invention relates to a composition for drying a patterned wafer to remove water therefrom, such composition comprising supercritical fluid, and at least one water-reactive agent that chemically reacts with water to form reaction product(s) more soluble in the supercritical fluid than water.
  • the invention relates to a method of drying a patterned wafer to remove water therefrom, such method comprising contacting said patterned wafer with a composition comprising supercritical fluid, and at least one water-reactive agent that chemically reacts with water to form reaction product(s) more soluble in the supercritical fluid than water.
  • a still further aspect of the invention relates to a method of drying a patterned wafer to remove water therefrom, such method comprising contacting the patterned wafer with a first composition comprising liquid C0 2 , and thereafter contacting the patterned substrate with a second composition comprising SCC02, thereby effecting drying of the patterned substrate without damage to the pattern thereof.
  • Yet another aspect of the invention relates to a method of drying a patterned wafer to remove water therefrom, such method comprising (a) contacting the patterned wafer with a first composition comprising alcohol at pressure above about 1000 psi and temperature below 32°C,
  • FIG. 1 is a scanning electron microscope (SEM) photograph of a patterned wafer showing the details of the pattern structure, utilized as a control sample, relative to FIGS. 2-4.
  • FIG. 2 is an SEM photograph of a patterned wafer of the type shown in FIG. 1 , after air-drying of the wafer.
  • FIG. 3 is an SEM photograph of a patterned wafer of the type shown in FIG. 1 , after drying of the wafer with liquid C0 2 .
  • FIG. 4 is an SEM photograph of a patterned wafer of the type shown in FIG. 1 , after drying of the wafer, first with liquid C0 2 and then with supercritical C0 2 .
  • the present invention is based on the use of supercritical fluid (SCF) as a cleaning medium for drying of patterned wafers, in various approaches that avoid the problems incident to the use of supercritical fluids per se.
  • SCF supercritical fluid
  • supercritical fluids might on first consideration be regarded as potentially useful media for drying of patterned wafers, since supercritical fluids have high diffusivity, low viscosity, near-zero surface tension, and superior penetrating ability, supercritical fluids such as supercritical C0 2 (SCC02) are non-polar and therefore are not useful for drying of patterned wafers.
  • supercritical C0 2 SCC02
  • the solubility of water in supercritical C0 2 is ⁇ 0.1% by weight, making supercritical C0 2 unsuitable for removing residual water on the patterned wafer.
  • the present invention overcomes the problems incident to the use of supercritical fluids as drying media.
  • Supercritical fluids are formed under conditions at which the density of the liquid phase equals the density of the gaseous phase of the substance.
  • C0 2 carbon dioxide
  • the density of the SCF can be varied from liquid-like to gaseous-like, yielding different solvation abilities, by varying the pressure and temperature.
  • Supercritical fluids have a density/solubility and diffusibility approaching that of the liquid and gaseous phase, respectively. Additionally, the surface tension of SCFs is negligible.
  • supercritical C0 2 is a preferred SCF in the broad practice of the present invention, although the invention may be practiced with any suitable SCF species, with the choice of a particular SCF depending on the specific application involved.
  • Other preferred SCF species useful in the practice of the invention include oxygen, argon, krypton, xenon, and ammonia.
  • supercritical fluids are used as drying media for patterned wafers in drying compositions that include one or more water-reactive agents that chemically react with water on the patterned- wafer to form reaction product species that are more soluble in the supercritical fluid than water.
  • HFA hexafluoroacetone
  • the product diol, CH 3 C(OH) 2 CF 3 is highly soluble in SCC02 and is readily dissolved by the supercritical fluid, thereby effectively removing water from the patterned wafer substrate with which the supercritical fluid composition, comprising SCC02 and HFA, is contacted.
  • the water-reactive agent in the supercritical fluid-based wafer drying composition can be of any suitable type, including for example, other halogenated aldehydes and ketones; halogenated diketones, e.g., l,l,l,5,5,5-hexafluoro-2,4-pentanedione, alternatively denoted as (hfac)H; halogenated esters; carboxylic anhydrides, e.g., (CH 3 CO) 2 0; siloxanes, halogenated silanes; and any other compounds and materials that easily react with water and form derivatives soluble in supercritical C0 2 or other supercritical fluid species.
  • halogenated aldehydes and ketones e.g., l,l,l,5,5,5-hexafluoro-2,4-pentanedione, alternatively denoted as (hfac)H
  • halogenated esters e.g., (CH 3 CO)
  • the water-reactive agent can be formulated in the supercritical fluid composition at any suitable concentration that is effective for water removal from the patterned wafer substrate.
  • the concentration of the water-reactive agent can be a concentration in a range of from about 0.01 to about 10.0 % by weight, based on the total weight of the supercritical fluid and the water-reactive agent, with concentrations of from about 0.1 to about 7.5 % by weight, on the same total weight basis being more preferred, and from about 0.1 to about 5.0 % by weight, on the same total weight basis being most preferred.
  • the supercritical fluid drying composition in addition to the supercritical fluid and the water- reactive agent, can contain other components, e.g., co-solvent(s) for removal of components other than water from the patterned substrate, active agent(s) other than the water-reactive agent, surfactant(s), chelating agent(s), etc., as necessary or desirable in a given application of the drying composition.
  • co-solvent(s) for removal of components other than water from the patterned substrate
  • active agent(s) other than the water-reactive agent e.g., surfactant(s), chelating agent(s), etc.
  • an “active agent” is a material that induces chemical reaction and/or physical enhancement of solubility, either in the cleaning composition, or at the surface of the patterned substrate structure, to enhance the cleaning and/or removal action of the composition, relative to a corresponding composition lacking such material.
  • Illustrative co-solvent species can include, but are not limited to, xylene, methanol, ethanol, and higher alcohols, N-alkylpyrrolidiones, such as N-methyl-, N-octyl-, or N-phenyl-pyrrolidones, dimethylsulfoxide, sulfolane, catechol, ethyl lactate, acetone, methyl ethyl ketone, butyl carbitol, monoethanolamine, butyrol lactone, diglycol amine, alkyl ammonium fluoride T- butyrolactone butylene carbonate, ethylene carbonate, propylene carbonate, etc.
  • the co-solvent species may be a single component co-solvent or two or more solvent components.
  • the co-solvent may be present in the supercritical fluid-based drying composition at any suitable concentration, consistent with solubility of the co-solvent in the supercritical fluid.
  • active agents include, without limitation, acids, bases, reducing agents, and oxidizing agents.
  • the reducing agent may require activation, e.g., by an activation process involving thermal, optical, and/or sonic activation.
  • Surfactants useful in the drying compositions of the present invention may likewise be of any suitable type, including anionic, neutral cationic, and zwitterionic types.
  • Illustrative surfactant species include, without limitation, acetylenic alcohols and diols, and long alkyl chain secondary and tertiary amines.
  • Chelating agents useful in the drying compositions of the invention may be of any suitable type including, for example, polycarboxylic acids such as iminodiacetic acid and lauryl ethylenediamine triacetic acid, j8-diketones such as: 2,4-pentanedione; l,l,l-trifluoro-2,4- pentandione; and l,l,l,5,5,5-hexafluoro-2,4-pentanedion, substituted dithiocharbanates, malonic acid esters, and polyethylene glycols.
  • polycarboxylic acids such as iminodiacetic acid and lauryl ethylenediamine triacetic acid
  • j8-diketones such as: 2,4-pentanedione; l,l,l-trifluoro-2,4- pentandione; and l,l,l,l,5,5,5-hexafluoro-2,4-pentanedion, substitute
  • Illustrative species of acids useful in drying compositions of the invention include, without limitation, perfluorocarboxyic acids, and alkyl or aryl sulfonic acids.
  • Illustrative species of bases useful in drying compositions of the invention include, but are not limited to, amines, such as alkyl amines.
  • Oxidizing agents useful in the broad practice of the invention include, without limitation, oxygen, ozone and nitrous oxide.
  • Reducing agents usefully employed in the drying compositions of the invention include, without limitation, hydrogen, ammonia, xylenes, hydrides, silane, alkylsilanes, hydrazine hydrate or alkyl hydrazine.
  • compositions can be employed within the scope of the present invention, and such compositions can alternatively comprise, consist or consist essentially of specific identified component(s) described herein, as desired in a given application of the invention.
  • the contacting of the patterned substrate with the drying composition is carried out for a suitable period of time, which in a specific embodiment can for example be on the order of from about 20 to about 60 seconds, although other (longer or shorter) periods of contacting may be usefully employed depending on the nature and amount of the water to be removed from the patterned substrate, and the process conditions employed for drying.
  • the contacting vessel in which the supercritical fluid-based composition is contacted with the patterned substrate can be rapidly decompressed to separate the supercritical fluid composition from the patterned substrate and exhaust the regasified supercritical fluid from the contacting vessel, so that the non-supercritical component(s), such as the soluble water reaction product(s), can be entrained in the regasified supercritical fluid and likewise be removed from the drying locus.
  • the non-supercritical component(s) such as the soluble water reaction product(s)
  • Such decompression step may be conducted for a suitable period of time, e.g., on the order of
  • composition and method can be usefully employed to clean residual water from small dimensions on semiconductor substrates subsequent to photolithographic image patterning processes without the occurrence of pattern collapse.
  • the present invention contemplates use of supercritical fluid-based drying compositions as part of a two-step process for obtaining efficient drying without the collapse of the pattern features.
  • an initial drying step is carried out by contacting the patterned substrate with liquid C0 2 , followed by a second drying step including contacting the patterned substrate with SCC02, to achieve drying of the patterned substrate without accompanying damage to the patterned wafer.
  • the liquid phase C0 2 in the first step has a higher density than
  • FIG. 1 is a scanning electron microscope (SEM) photograph of a patterned wafer showing the details of the pattern structure, utilized as a control sample, relative to FIGS. 2-4.
  • SEM scanning electron microscope
  • FIG. 2 is an SEM photograph of a patterned wafer of the type shown in FIG. 1 , after such air-drying of the wafer. As shown in FIG. 2, the water and alcohol were not completely removed, and the residual amounts of these contaminants caused collapsing of the pattern structure to occur.
  • FIG. 3 is an SEM photograph of a patterned wafer of the type shown in FIG. 1, after such drying of the wafer with liquid C0 2 . As shown in FIG. 3, the water and alcohol were not completely removed, and the residual amounts of these contaminants caused a high level of collapse of the pattern structure to take place.
  • a third test wafer was dried in a two-step process as described hereinabove, including a first step of contacting the patterned wafer with liquid C0 2 and a second step of contacting the patterned wafer, after the first contacting step, with supercritical C0 2 .
  • FIG. 4 is an SEM photograph of a patterned wafer of the type shown in FIG.
  • the two-step process described above can be carried out at any suitable process conditions and for any suitable durations in the respective first and second steps.
  • the first liquid C0 2 contacting step can be carried out at temperature in a range of from about 20°C to about 30°C for a time in a range of from about 0.5 to about 20 minutes
  • the second SCC02 contacting step can be carried out at temperature in a range of from about 32°C to about 75°C for a duration in a range of from about 0.5 to about 20 minutes.
  • the present invention contemplates use of supercritical fluid-based drying compositions as part of a three-step process for obtaining efficient drying without the collapse of the pattern features.
  • an initial drying step is carried out in which the patterned substrate is contacted with alcohol at a pressure above about 1000 psi and temperature below the critical temperature of C0 2 , 32°C, for a suitable period of time, e.g. from about 1 minute to about 15 minutes.
  • the alcohol can be a single component alcohol, or it can be a mixture of alcohol species, and the alcohol can be recirculated in contact with the patterned substrate, or it can be contacted in a batch or a semibatch mode.
  • the second step is carried out after the alcohol contacting step, and involves contacting the patterned substrate with an alcohol C0 2 solution to remove alcohol from the first contacting step.
  • This second step preferably is carried out with recirculation of the alcohol/C0 2 solution through the contacting chamber containing the patterned substrate, although the contacting may be carried out in a single-pass manner, or in a batch or semi-batch mode of operation.
  • the second step contacting can be carried out at a temperature in a range of from about 22°C to about 31°C for a duration in a range of from about 0.5 to about 20 minutes.
  • the alcohol can be a single component alcohol, or it can be a mixture of alcohol species.
  • the alcohol utilized in the first and second contacting steps can be the same as or different from each other.
  • the alcohol can be of any suitable type.
  • such alcohol comprises a C 1 -C 4 alcohol (i.e., methanol, ethanol, propanol, or butanol), or a mixture of two or more of such alcohol species.
  • the third step is carried out after the alcohol/C0 2 solution contacting step, and involves rinsing the patterned substrate with SCC02.
  • Such supercritical fluid rinse step can be carried out at a temperature in a range of from about 32°C to about 75°C and pressure in a range of from about 80 to about 300 atm., for a duration in a range of from about 0.5 to about 30 minutes.
  • Each of the first, second and third steps can be carried out in a same process vessel, suitably valved, piped and manifolded for delivery, and, if desired, recirculation, of the successive drying compositions.
  • the alcohol/C0 2 solution can be formulated with the alcohol at any suitable concentration.
  • the concentration of the alcohol in the alcohol/C0 2 solution is from about 1 to about 15% by weight, based on the total weight of the alcohol and C0 2 components in the alcohol/C0 2 solution.
  • the alcohol/C0 2 solution can also be formulated with other components as desired, such as those (e.g., co-solvents, active agent(s), surfactant(s) and/or chelating agent(s)) illustratively described hereinabove.

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  • Cleaning Or Drying Semiconductors (AREA)

Abstract

Le séchage de tranches imprimées est réalisé en effectuant l'enlèvement de l'eau des tranches imprimées sans déformation ou détérioration des structures imprimées sur celles-ci. Le séchage est réalisé dans un aspect de l'invention avec une composition contenant un fluide supercritique, et au moins un agent réagissant avec l'eau qui réagit chimiquement avec l'eau pour former un ou des produits de réaction plus solubles dans le fluide supercritique que dans l'eau. Des méthodologies diverses sont décrites pour l'utilisation de fluides supercritiques pour sécher des tranches imprimées, qui évitent la déficience de (faible solubilité dans l'eau) des fluides supercritiques tel que le CO2 supercritique.
PCT/US2004/014353 2004-05-07 2004-05-07 Compositions et procédés pour sécher des tranches imprimées par séchage durant la fabrication de circuits imprimés Ceased WO2005113167A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
PCT/US2004/014353 WO2005113167A1 (fr) 2004-05-07 2004-05-07 Compositions et procédés pour sécher des tranches imprimées par séchage durant la fabrication de circuits imprimés
EP04751653A EP1765526A4 (fr) 2004-05-07 2004-05-07 Compositions et procédés pour sécher des tranches imprimées par séchage durant la fabrication de circuits imprimés
JP2007511332A JP2007536730A (ja) 2004-05-07 2004-05-07 集積回路製品を製造する間にパターン形成されたウエハーを乾燥させるための組成物及び方法
CNA2004800432546A CN1960813A (zh) 2004-05-07 2004-05-07 在制备集成电路产品过程中用于干燥构图晶片的组合物和方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/US2004/014353 WO2005113167A1 (fr) 2004-05-07 2004-05-07 Compositions et procédés pour sécher des tranches imprimées par séchage durant la fabrication de circuits imprimés

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WO2005113167A1 true WO2005113167A1 (fr) 2005-12-01

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EP (1) EP1765526A4 (fr)
JP (1) JP2007536730A (fr)
CN (1) CN1960813A (fr)
WO (1) WO2005113167A1 (fr)

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US8440573B2 (en) * 2010-01-26 2013-05-14 Lam Research Corporation Method and apparatus for pattern collapse free wet processing of semiconductor devices
TWI627667B (zh) 2012-11-26 2018-06-21 應用材料股份有限公司 用於高深寬比半導體元件結構具有污染物去除之無黏附乾燥處理
US10283344B2 (en) 2014-07-11 2019-05-07 Applied Materials, Inc. Supercritical carbon dioxide process for low-k thin films
US10026629B2 (en) * 2014-10-17 2018-07-17 Tokyo Electron Limited Substrate liquid processing apparatus, substrate liquid processing method, and computer-readable storage medium storing substrate liquid processing program
WO2017062135A1 (fr) 2015-10-04 2017-04-13 Applied Materials, Inc. Procédé de séchage pour des structures à rapport largeur/longueur élevé
KR102062873B1 (ko) * 2015-10-04 2020-01-06 어플라이드 머티어리얼스, 인코포레이티드 작은 열 질량의 가압 챔버
KR102145950B1 (ko) 2015-10-04 2020-08-19 어플라이드 머티어리얼스, 인코포레이티드 기판 지지체 및 배플 장치
KR102055712B1 (ko) 2015-10-04 2019-12-13 어플라이드 머티어리얼스, 인코포레이티드 감소된 용적의 처리 챔버
JP7394563B2 (ja) * 2019-09-12 2023-12-08 東京エレクトロン株式会社 基板処理装置の洗浄方法及び基板処理システム

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Also Published As

Publication number Publication date
CN1960813A (zh) 2007-05-09
JP2007536730A (ja) 2007-12-13
EP1765526A4 (fr) 2007-11-14
EP1765526A1 (fr) 2007-03-28

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