WO2005104202A1 - Procede de nettoyage de substrat - Google Patents

Procede de nettoyage de substrat Download PDF

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Publication number
WO2005104202A1
WO2005104202A1 PCT/JP2005/007629 JP2005007629W WO2005104202A1 WO 2005104202 A1 WO2005104202 A1 WO 2005104202A1 JP 2005007629 W JP2005007629 W JP 2005007629W WO 2005104202 A1 WO2005104202 A1 WO 2005104202A1
Authority
WO
WIPO (PCT)
Prior art keywords
ice
cleaning
temperature
pure water
substrate according
Prior art date
Application number
PCT/JP2005/007629
Other languages
English (en)
Japanese (ja)
Inventor
Mikio Takagi
Original Assignee
F.T.L.. Co., Ltd.
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 F.T.L.. Co., Ltd. filed Critical F.T.L.. Co., Ltd.
Priority to JP2006512591A priority Critical patent/JPWO2005104202A1/ja
Publication of WO2005104202A1 publication Critical patent/WO2005104202A1/fr

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02041—Cleaning
    • H01L21/02043—Cleaning before device manufacture, i.e. Begin-Of-Line process
    • H01L21/02052—Wet cleaning only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/02—Cleaning by the force of jets or sprays
    • 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
    • B08B7/0064—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes
    • B08B7/0092—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes by cooling
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0075—Cleaning of glass

Definitions

  • the present invention relates to a method for cleaning a substrate. More specifically, the present invention relates to a method for cleaning electronic devices such as a substrate of an electronic device, a semiconductor wafer, a liquid crystal substrate, a photomask, and a glass substrate.
  • the present invention relates to a method for removing film-like dust, particles, foreign matter, and the like (hereinafter, referred to as “particles”) by cleaning. More specifically, the present invention relates to an improvement in the so-called ice cleaning method.
  • Japanese Unexamined Patent Publication No. 479326/1992 responds to the above request, and uses a mixture of ice fine particles and pure water as a washing means. Specifically, ice fine particles and pure water stored in a tank are mixed by a nozzle. The method of injecting is shown. There is also mention of mixing alcohol with pure water.
  • a spray method, an ultrasonic method, the above method, and the like are known (see “Applied Physics”, Vol. 59, No. 11, (1990), 1509 ⁇ 1510).
  • Japanese Patent No. 3380021 proposes a cleaning method in which a mixture of, for example, isopropyl alcohol (IPA) and ice fine particles produced by the above-mentioned applied physics is sprayed onto a substrate at a temperature of 0 ° C. or less.
  • IPA isopropyl alcohol
  • Japanese Patent Application Laid-Open No. 2003-151942 discloses a method in which a mixture of pure water and isopropyl alcohol is mixed with a tank, cooled, formed into a sherbet shape, and injected together with a carrier gas. Proposed.
  • the ice formation temperature is 3 ° C at an IPA concentration of 5% by weight.
  • pure water used as a carrier fluid has a temperature of 0 ° C. or more, and may melt ice.
  • a cleaning agent consisting of a mixture of ice fine particles produced by the aforementioned applied physics and an IPA aqueous solution is sprayed onto a substrate. If the detergent is stirred by applying ultrasonic vibration for a certain period of time before spraying, it rapidly solidifies and becomes a so-called sherbet-like shape, deteriorating the sprayability.
  • the so-called shear bet is sprayed onto the substrate to be cleaned using a gas as a carrier gas due to poor fluidity.
  • a gas as a carrier gas due to poor fluidity.
  • the gas itself since the gas itself has no particle cleaning effect, a high cleaning effect cannot be expected.
  • Ice particles which have been proposed in Applied Physics, are high in hardness, so that there is a risk of damaging semiconductor devices, and the production cost is high due to force.
  • the present invention solves the above-mentioned problems and further improves ice washing, and comprises a first pure water and a first compound having a freezing point lower than 0 ° C.
  • a first solid-liquid mixture comprising a first ice and a first solid-liquid mixture comprising a second ice, consisting of a second pure water or substantially a second pure water power, the balance being 0 ° C
  • a fluid containing a second compound having the following freezing point is added to a second temperature, followed by at least a portion or all of the first ice at a third temperature below 0 ° C.
  • the substrate is washed with the second solid-liquid mixture.
  • (A) Fluid a complete liquid or solid-liquid mixture that is added to the first solid-liquid mixture
  • Second solid-liquid mixture solid-liquid mixture after addition of fluid, that is, a cleaning agent used for substrate cleaning
  • First ice ice in which first pure water has solidified
  • Second pure water pure water that forms a fluid or forms a fluid with a second compound (eg, IPA)
  • Second compound a compound that may be contained in the fluid
  • Table 1 shows various components of the fluid added to the first solid-liquid mixture.
  • composition of ice in the second solid-liquid mixture used for washing is as follows.
  • Case 1 First ice only (Claim 4).
  • the first ice may be partially melted and reduced, or the first pure water may be solidified and increased (the same applies in the following cases).
  • Case 2 ice solidified after addition of first ice + second pure water (Claim 8;). That is, it corresponds to A and D in Table 1, and ice is generated after the addition of the first fluid.
  • the first solid-liquid mixture is cooled to a first temperature between 0 ° C and a freezing point of the first compound below 0 ° C.
  • the first compound and the second compound include, for example, isopropyl alcohol (freezing point—88.9 ° C.), methyl alcohol (freezing point: —114.1 ° C.); acetone (freezing point—94.82 ° C.) ), Ethyl alcohol (freezing point-114.5 ° C). It is preferable that the first compound and the second compound are the same.
  • examples of the first and second compounds isopropyl alcohol (IPA) will be mainly described.
  • the force of adding the second pure water to the first solid-liquid mixture or (mouth) the first solid-liquid mixture has a solidification point of 0 ° C. or less with the second pure water.
  • a fluid consisting of the second compound is added.
  • the temperature of the second pure water is significantly higher than 0 ° C, the first ice having a cleaning effect is completely melted, while the temperature of the second pure water is lower than 0 ° C. If the supercooling temperature is extremely low, a large amount of ice will be generated in the piping, and if mixing becomes difficult, particles will be generated by damaging the inner wall of the piping with force.
  • the temperature of the second pure water to be added depends on the amount thereof, but is preferably 5 to 10 ° C or lower.
  • the second pure water + IPA is used as the fluid.
  • the temperature of the fluid must be such that it does not melt all of the first ice and may solidify itself but has a liquid portion.
  • the first ice (Cases 1 to 4) or other than the first ice obtained in Cases 2 to 4 contributes to the washing.
  • the amount of ice is not particularly limited, it depends on the degree of contamination. When a large glass substrate is washed in about 30 seconds to 3 minutes, the amount of ice is about 10 to 50%, and a smaller amount is preferable.
  • the action of the fluid is as follows.
  • cleaning is performed by a method such as impinging a second solid-liquid mixture having a third temperature lower than 0 ° C. on a substrate, or spinning the substrate by spin coating. U. If the contact temperature of the second solid-liquid mixture to the substrate (third temperature) is higher than 0 ° C, ice tends to melt and must be avoided.
  • the first ice may be produced by the method described in Applied Physics above, but preferably, the first ice is cooled by cooling a liquid comprising the first compound and water.
  • the method according to claim 2 for producing one ice is preferred.
  • the ice produced in this manner is more easily crushed than the ice produced by the above-mentioned applied physics, so that the substrate is not scratched, and the crushed ice chips wrap the particles and remove the particles. The cleaning effect is high even with relatively low-speed injection and spinner.
  • FIG. 1 is an equilibrium diagram showing the freezing points of isopropanol and water.
  • FIG. 2 is a diagram schematically showing concentrations and temperatures of a starting material, an intermediate material, and a final material of a coolant in the present invention.
  • FIG. 3 is a graph showing temperature changes of a coolant starting material, an intermediate material, and a final material in the present invention.
  • FIG. 4 is a schematic diagram illustrating changes in liquid temperature, IPA concentration, and ice production in the method of the present invention.
  • FIG. 5 is a diagram of an aspirator used in claim 5 of the present invention.
  • a phase diagram of a compound such as IPA and water constituting a cleaning agent gives information such as a solidification temperature when the cleaning agent is stirred for a long time at a certain temperature and approaches an equilibrium state.
  • concentration of IPA with respect to the total mass after adding a fluid such as pure water is shown in Fig. 1-Source system diagram (Source 1 "Solvent Handbook", March 10, 1977, Kodansha, p. 347) If the concentration is higher outside the mixed phase of solid phase and liquid phase specified in the above, the whole may become liquid phase in the temperature range of 0 ° C to 130 ° C, which is practical for washing, and ice may disappear. Becomes large.
  • the method according to claim 3, wherein the IPA concentration is in the solid phase + liquid phase mixed phase region of the binary phase diagram of the compound is preferable.
  • ternary phase diagrams for which IPA, methyl alcohol, water, etc. are difficult to obtain but in that case, the ice freezing point is determined experimentally, and the temperatures and concentrations of the coolant, intermediate substance, and final substance are determined similarly. There is a need.
  • the concentration region is defined as in claim 3, the concentration and temperature regions on the state diagram will be described with reference to FIG.
  • the fluid is assumed to consist of pure water.
  • FIG. 2 is a schematic diagram of a binary system of the water and the diagonal mixture, in which the first solid-liquid mixture has a concentration and a temperature in a hatched region rising to the right.
  • the temperature of the added pure water partially overlaps with the temperature of the first solid-liquid mixture.
  • the concentration of the second solid-liquid mixture becomes lower than that of the first solid-liquid mixture due to the addition of pure water, and the temperature of the second solid-liquid mixture becomes higher than that of the first solid-liquid mixture due to the temperature of the added pure water. Or it will be low or the same temperature.
  • FIG. 3 shows only the temperature change when the second pure water at about 0 ° C. is added.
  • the first temperature T of the first solid-liquid mixture is an ice formation temperature lower than 0 ° C, and the temperature T obtained by adding the second pure water at about 0 ° C is higher than T. Then inject
  • the temperature of the second solid-liquid mixture slightly increases unless the mixture is artificially cooled, and decreases when the mixture is artificially cooled. Therefore, the temperature T of the second solid-liquid mixture is
  • the first ice is generated by cooling and stirring the compound such as IPA and the first pure hydraulic fluid.
  • the first ice does not substantially melt and substantially does not generate ice in the process of changing the temperature of the fluid from the second temperature to the third temperature. .
  • FIG. 4 shows the IPA concentration (wt%) on the horizontal axis, the liquid temperature (° C) on the vertical axis, the circles in the figure show the step order, and the right side shows ice formation for each step order. Show changes in volume.
  • first stage mixing IPA with pure water produces a 10% IPA aqueous solution (room temperature, no ice).
  • the second step (circle 2), the solution is cooled to -10 ° C (T) and held
  • the first solid-liquid mixture can be indirectly cooled or directly cooled.
  • the fluid added to the first solid-liquid mixture is a supercooled liquid in a temperature range of -3 to -10 ° C (Claim 10), and may be cooled even lower than the supercooled area.
  • the fluid contains ice (claim 6, second ice), it can be used for washing.
  • pure water and IPA the second compound.
  • the concentration of the second compound is less than or equal to 5% by weight, preferably less than or equal to 2% by weight, and lower than the concentration of IPA in the first solid-liquid mixture.
  • the supercooling temperature of the fluid is reduced by the soybean curd such as IPA, and no ice is generated. At the moment when the completely liquid fluid and the first solid-liquid mixture are mixed, the temperature of the fluid rapidly drops due to the action of sensible heat (Fig. 4 , Circle 1 ⁇ circle 2 ').
  • the main purpose is to use the liquid portion in the added fluid as an ice carrier, and to minimize the generation of (second) ice after the addition of the second pure water, You. Therefore, the ice generated in the second stage and the IPA solution are mixed well so that the ice is evenly dispersed, and the ice is bombarded to adjust the size to an appropriate size, and then no gas is used. Another advantage is that the substrate can be cleaned at once.
  • a fourth step of further mixing the solid-liquid mixture in the third step and indirectly cooling the temperature only without changing the concentration See circle 3 in Figure 4 ⁇ circle 4).
  • the amount of ice in the equilibrium diagram can be larger than that at 3 ° C. Is achieved, and the second ice can be generated and sprayed together with the first ice.
  • the near equilibrium state increase or decrease against the theoretical amount of equilibrium mosquito ⁇ et calculation is that within ⁇ 5 weight 0/0. If the cooling temperature in the fourth stage is 7 ° C, T is less than T and equilibrates with less ice than in the second stage (circled 2 ', -30 ° C)
  • FIG. 5 shows an example of an aspirator for an embodiment in which the fluid is pure water.
  • 1 is a tank of a mixed liquid of IPA and the first pure water (that is, the first solid-liquid mixture)
  • 2 is a cooling jacket for flowing a cooling medium, and externally cooling the tank 1
  • 3 is an additive pure water.
  • the center tube that sprays water, 4 is the outer tube
  • 5 is ice particles.
  • the mixture of IPA and pure water flowing into the tank 1 is stirred by an ultrasonic generator (not shown), a stirrer, a blade, or the like, and is cooled by a refrigerant from the outside.
  • the mixture of the ice particles 5 and the IPA solution is pumped toward the tip of the outer tube 4 by a pump (not shown).
  • pure water is also pumped through the outer tube 3 by a pump (not shown), is injected from the tapered tip, and is further mixed with the mixture.
  • the pumping speed of pure water must be higher than the pumping speed of the above mixture. preferable.
  • the jet speed from the tip 4a of the outer tube is 100 m / sec or less, and since it is relatively low, the entrainment of air is small, and the damage to the elements formed on the substrate is also reduced.
  • the distance between the aspirator and the substrate is preferably 5 to 50 mm. It is preferable that the larger amount of the second pure water and the first solid-liquid mixture flow through the center tube 3.
  • the spray nozzle at the tip 4a can be divergent on one surface and plate-shaped fan-shaped, conical-shaped or needle-shaped on an orthogonal surface. Further, a coaxial cooling pipe can be attached to the tip 4a for indirect cooling.
  • an IPA solution having an IPA concentration of 3 to 5% by weight and a temperature of 3 ° C to 17 ° C is suitable.
  • the addition of pure water in the first method is carried out in a suitable insulated vessel equipped with a stirrer, and further stirred while cooling in the above-mentioned range of 13 ° C to 15 ° C. As a result, a change from the circle 3 to the circle 4 in FIG. 44 occurs, and further ice particles are generated. Next, this is sprayed on the glass substrate.
  • the ice fine particles produced by the method according to claims 2 to 7 of the present invention have a small damage to the substrate and are suitable for cleaning fine elements.
  • the occurrence of cavitation is prevented, the reduction of the liquid contact area due to gas mixing is prevented, and the damage is further reduced by reducing the collision speed against the substrate. it can.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Cleaning Or Drying Semiconductors (AREA)

Abstract

Dans le contexte du lavage au jet d’un grand substrat mince, comme un substrat semi-conducteur ou un substrat de verre, il est prévu un procédé de nettoyage ayant un effet nettoyant important sans endommager le substrat. On ajoute de l’eau pure (3) à une solution aqueuse d’alcool isopropyle (AIP), en particulier un mélange solide liquide (4a) composé de glace (5) et d’une solution eau AIP de façon à réguler la concentration AIP en fonction de tout le mélange pour obtenir un jet plus puissant. Il s’ensuit que le nettoyage peut être réalisé sans utiliser de gaz porteur. Autre possibilité, on ajoute une solution AIP à la place de l'eau pure (3) pour améliorer de manière similaire la puissance du jet et également pour réguler le point de congélation e’ mieux doser la quantité de glace formée.
PCT/JP2005/007629 2004-04-21 2005-04-21 Procede de nettoyage de substrat WO2005104202A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2006512591A JPWO2005104202A1 (ja) 2004-04-21 2005-04-21 基板の洗浄方法

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JP2004125728 2004-04-21
JP2004-125728 2004-04-21

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009522778A (ja) * 2005-12-30 2009-06-11 ラム リサーチ コーポレーション 微粒子除去のための方法および装置
JP2009522783A (ja) * 2005-12-30 2009-06-11 ラム リサーチ コーポレーション 半導体基板を洗浄するための方法および装置
CN102161042A (zh) * 2010-12-09 2011-08-24 武汉奋进电力技术有限公司 颗粒冰带电水冲洗装置
JP2012230253A (ja) * 2011-04-26 2012-11-22 Osaka Univ 基板の洗浄方法
CN109311063A (zh) * 2016-01-27 2019-02-05 科尔森冰爆有限公司 冰喷射系统和方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0479326A (ja) * 1990-07-23 1992-03-12 Mitsubishi Electric Corp 基板表面の洗浄装置
JPH08294680A (ja) * 1995-04-27 1996-11-12 Mitsubishi Heavy Ind Ltd 含氷粒水噴射装置
JP3380021B2 (ja) * 1993-12-28 2003-02-24 株式会社エフティーエル 洗浄方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0479326A (ja) * 1990-07-23 1992-03-12 Mitsubishi Electric Corp 基板表面の洗浄装置
JP3380021B2 (ja) * 1993-12-28 2003-02-24 株式会社エフティーエル 洗浄方法
JPH08294680A (ja) * 1995-04-27 1996-11-12 Mitsubishi Heavy Ind Ltd 含氷粒水噴射装置

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009522778A (ja) * 2005-12-30 2009-06-11 ラム リサーチ コーポレーション 微粒子除去のための方法および装置
JP2009522783A (ja) * 2005-12-30 2009-06-11 ラム リサーチ コーポレーション 半導体基板を洗浄するための方法および装置
JP2009522780A (ja) * 2005-12-30 2009-06-11 ラム リサーチ コーポレーション 二相の基板洗浄化合物を使用するための方法およびシステム
KR101414371B1 (ko) 2005-12-30 2014-07-01 램 리써치 코포레이션 파티클 제거 방법 및 장치
CN102161042A (zh) * 2010-12-09 2011-08-24 武汉奋进电力技术有限公司 颗粒冰带电水冲洗装置
JP2012230253A (ja) * 2011-04-26 2012-11-22 Osaka Univ 基板の洗浄方法
CN109311063A (zh) * 2016-01-27 2019-02-05 科尔森冰爆有限公司 冰喷射系统和方法

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