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WO1996020498A1 - Couche d'oxyde, son procede de formation et dispositif a semi-conducteurs - Google Patents

Couche d'oxyde, son procede de formation et dispositif a semi-conducteurs Download PDF

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Publication number
WO1996020498A1
WO1996020498A1 PCT/JP1995/002730 JP9502730W WO9620498A1 WO 1996020498 A1 WO1996020498 A1 WO 1996020498A1 JP 9502730 W JP9502730 W JP 9502730W WO 9620498 A1 WO9620498 A1 WO 9620498A1
Authority
WO
WIPO (PCT)
Prior art keywords
oxide film
substrate
ultrapure water
forming
cleaning
Prior art date
Application number
PCT/JP1995/002730
Other languages
English (en)
Japanese (ja)
Inventor
Tadahiro Ohmi
Original Assignee
Tadahiro Ohmi
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 Tadahiro Ohmi filed Critical Tadahiro Ohmi
Publication of WO1996020498A1 publication Critical patent/WO1996020498A1/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
    • 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
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
    • H01L21/02227—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process
    • H01L21/0223—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate
    • H01L21/02233—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate of the semiconductor substrate or a semiconductor layer

Definitions

  • the present invention relates to an oxide film, a method for forming the same, and a semiconductor device. More particularly, the present invention relates to a method for removing an organic impurity attached to a semiconductor substrate or the like and forming an oxide film having excellent characteristics such as extremely high withstand voltage. Background art
  • Cleaning of silicon wafers in the semiconductor manufacturing process is one of the most important steps in the semiconductor production process. That is, a large number of various impurities are attached to a silicon wafer, and removal of these impurities is indispensable for manufacturing a device having stable characteristics with a high yield. In particular, as semiconductor devices become more highly integrated and have higher performance, the devices are becoming finer and the wafer size is becoming larger.
  • the inventor of the present invention has conducted a series of studies on the relationship between the cleaning method and the device manufactured thereafter, and in the course of conducting a series of studies, it has been impossible to completely remove organic impurities on the substrate by the conventional cleaning method. We saw that it had a large effect on the dielectric strength of the oxide film. For example currently commonly used for the removal of organic impurities, H 2 S 0 4 + H 9 0. + Ultra pure water cleaning, NH 4 OH + H n 0 2 + Ultra pure water cleaning, HC 1 + H 2 ⁇ 2 + Ultra pure water cleaning, etc. It has been found that a cleaning method that can completely remove organic substances is necessary for formation.
  • the conventional cleaning method a separate cleaning device or cleaning tank is used for each chemical solution, and the silicon wafer is immersed in the cleaning tank in which each chemical solution and ultrapure water are stored sequentially.
  • the residual chemical solution is brought into the wafer in the process, and there is a problem that the chemical solution in the cleaning tank is cross-contaminated.
  • transporting between cleaning tanks transports them into the atmosphere, which results in organic contamination from the air and formation of natural oxide films.
  • the contaminated chemical solution is used more than once and a plurality of silicon wafers are washed at the same time, there is a problem that impurities released from one silicon wafer adhere to other silicon wafers.
  • the present invention solves the above problems, and provides an oxide film having excellent performance such as withstand voltage on a clean silicon wafer surface free from organic contamination, and a method for forming the oxide film. It is intended to provide a device. Disclosure of the invention
  • the method for forming an oxide film according to the present invention comprises the steps of: removing an organic substance attached to a substrate by supplying ultrapure water containing ozone to the substrate while rotating the substrate in an inert gas atmosphere; An oxide film removing step of contacting the oxide film generated in the organic substance removing step with hydrofluoric acid to remove the oxide film, and then contacting the ozone-containing ultrapure water to form an oxide film. , At least.
  • the oxide film forming step it is preferable to supply the ultrapure water containing ozone while rotating the substrate.
  • the concentration of ozone in the ultrapure water is preferably 2 ppm to 10 ppm, and the concentration of organic impurities in the inert gas is preferably 1 ppm or less.
  • the rotation speed of the substrate is preferably set to 100 to 300 rpm, and the supply amount of the ozone-containing ultrapure water is preferably set to 100 to 500 cc Zmin. No.
  • the oxide film of the present invention is an oxide film formed on the surface of a substrate in a liquid phase.
  • the interface between the substrate and the oxide film and the organic matter in the oxide film have a number of CH 2 groups of 2 in terms of arachidic acid. X 10 14 cm— 2 or less.
  • the semiconductor device of the present invention has an oxide film formed by a thermal oxidation method or an ion-assisted oxidation method after forming an oxide film by the above-described oxide film forming method. I do. Action
  • the method of forming an oxide film according to the present invention is performed in an inert gas atmosphere, and includes at least a step of washing and removing organic impurities with ozone-added ultrapure water, a step of removing an oxide film with HF + ultrapure water, and an oxidation with ozone-added ultrapure water.
  • a film forming step includes at least a step of washing and removing organic impurities with ozone-added ultrapure water, a step of removing an oxide film with HF + ultrapure water, and an oxidation with ozone-added ultrapure water.
  • the ozone-added ultrapure water is supplied to the substrate surface while rotating the substrate, and the organic matter on the surface is oxidized by the ozone-added ultrapure water. At this time, an oxide film is simultaneously formed on the substrate surface. Then rinse with ultrapure water (or ultrapure water with ozone added) to wash away impurities.
  • an oxide film is formed by bringing a clean substrate surface from which organic impurities have been removed into contact with ozone-added ultrapure water.
  • the thickness of this oxide film is preferably from 0.3 to 1.0 nm.
  • the substrate may be immersed in each chemical solution, but it is preferable to perform the treatment by supplying the chemical solution while rotating the substrate. As a result, the substrate is always in contact with a fresh chemical solution, and the processing proceeds uniformly within the surface of the substrate, so that an oxide film having higher insulating properties can be formed. It is preferable that the rotation speed of the substrate is controlled to an optimum rotation speed for each step.
  • the substrate is spun dry to complete the process. So far, all steps are preferably performed continuously in a single vessel.
  • the inert gas flowing downflow in the closed vessel it is preferable to keep the inert gas flowing downflow in the closed vessel.
  • an inert gas atmosphere it is possible to prevent the substrate surface from being exposed to impurity components, and to prevent adhesion of organic substances and formation of a natural oxide film.
  • a natural oxide film is formed after the oxide film stripping step, the oxide film formed by the ozone-added ultrapure water and the subsequent heat treatment becomes non-uniform, so that the insulating properties deteriorate.
  • minute roughness of the surface increases, and the quality of the oxide film formed by ozone-added ultrapure water and subsequent heat treatment is degraded. Therefore, it is desirable to minimize the formation of a natural oxide film.
  • the presence of water alone does not cause the formation of a natural oxide film due to the presence of oxygen alone, and both water and oxygen are generated in parallel. Therefore, if the atmosphere is an inert gas atmosphere, formation of a natural oxide film can be prevented.
  • the content of oxygen in the inert gas is preferably 1 O ppb or less, more preferably 10 ppb or less, and most preferably 1 ppb or less.
  • the amount of organic impurities in the gas is preferably 1 ppb or less, more preferably 1 O ppt or less, and most preferably 1 ppt or less. Nitrogen gas is preferred as such an inert gas.
  • the pressure in the closed vessel becomes higher than the external pressure.
  • the pressure in the closed tank is made higher than that of the outside, it is possible to prevent the air from leaking into the closed tank, and it is possible to more effectively prevent the adhesion of organic substances and the formation of a natural oxide film.
  • the introduction of the inert gas into the closed tank is preferably performed in a downflow manner.
  • the product detached from the surface falls down along the flow of the gas, so that re-adhesion to the substrate can be prevented, so that cleaning with higher cleanliness can be performed.
  • the inert gas preferably has a flow rate that does not disturb the chemical solution layer formed on the surface of the substrate.
  • the concentration of ozone in the ozone-added ultrapure water is preferably 2 ppm to 10 ppm. If it is less than 2 ppm, the oxidation of organic substances may be insufficient.If it exceeds 1 O ppm, the thickness of the oxide film formed on the substrate surface will be too thick, and it will take time to remove it and increase the surface roughness. This is because in some cases,
  • the concentration of ozone in the ozone-added ultrapure water is preferably 2 ppm to 1 O ppm. Within this range, an oxide film with a high withstand voltage can be obtained, and the maximum injected charge Q BD increases even in the TDDB characteristics of the oxide film under constant current stress.
  • the ozone-added ultrapure water can be obtained by, for example, electrolyzing ultrapure water. In order to minimize the decrease in concentration due to the decomposition of ozone, it is preferable to manufacture it near the use point.
  • the supply of a chemical solution or ultrapure water is not discontinuous in order to supply a chemical solution or the like while rotating the substrate, and to efficiently and uniformly remove organic substances, remove an oxide film, and form an oxide film. It is preferable to perform the operation continuously as a fluid. In other words, it is important to supply the chemical solution or ultrapure water continuously, not absolutely, in a state where it comes out of the water tap.
  • a nozzle for producing the above continuous flow it is preferable to use a straight pipe type having a uniform inner diameter up to the liquid outlet. And it is preferable to arrange so that the surface of the liquid outlet is horizontal to the substrate. If such a nozzle is used, the chemical solution or ultrapure water flowing out of the outlet will fall directly below the outlet as a continuous fluid, and the drop point will be the center of rotation of the substrate, The dropped chemical solution spreads uniformly in the plane due to centrifugal force, so it is possible to perform uniform cleaning in the plane. In other words, the outlet is restricted In such a case, the chemical solution discharged from the liquid discharge surface becomes a mist and cannot supply a continuous fluid. In addition, when the liquid discharge surface is not horizontal, the amount of the chemical liquid differs from the liquid discharge port, or the chemical liquid does not drop directly below the liquid discharge port, so that it is impossible to supply the liquid uniformly over the surface.
  • the supply position of the chemical solution be the center of rotation of the substrate from the viewpoint of further improving in-plane uniformity.
  • a plurality of chemical solution washing steps may be appropriately performed in addition to the above steps.
  • the transfer since the transfer can be performed in the same tank, it is possible to prevent the adhesion of organic substances, the formation of a natural oxide film, the adhesion of particles, and the like by contact with the air during the transfer of the substrate.
  • the number of rotations of the substrate is an important factor for the degree of cleanliness and the uniformity of the oxide film, and is preferably 100 to 300 rpm, and preferably 250 to 300 rpm. More preferably, it is set to pm.
  • the supply amount of the chemical is preferably from 100 m1 / min to 500 m1Zmin, more preferably from 300 ml / min to 500 ml / min. Since the treatment itself is completed in a short time, the amount of chemical used even at a large flow rate is greatly reduced compared to the conventional method.
  • the supply amount of ultrapure water varies depending on the surface area of the substrate, in the case of a wafer having a diameter of 3 inches to 8 inches, 2.5 to 10 cc of ultrapure water is applied to the surface of the substrate. Preferably it is supplied.
  • pure water cannot be completely covered on the surface if it is less than 2.5 cc, and if it exceeds 10 cc, only a part of ultrapure water flows and one If a channel is formed and the chemical solution is subsequently supplied, the chemical solution will flow preferentially through the flow channel and uniform cleaning will not be possible.
  • the rotation speed is less than 100 rpm, it may not be possible to cover the entire surface with water. That is, a drying part may be partially generated.
  • the rotation speed exceeds 400 rpm, a part of the water striking layer formed on the surface may be destroyed. May be confused.
  • the chemical solution is scattered from the surface by centrifugal force, and the scattered chemical solution adheres to the inner wall of the cleaning tank, and the chemical solution attached to the inner wall may separate from the inner wall and re-attach to the substrate surface. Therefore, during the chemical solution cleaning step and the ultrapure water cleaning step, it is preferable to always wash the inner wall surface of the tank with ultrapure water and to wash out the adhered chemical liquid from the inner wall surface in order to perform highly clean cleaning. As a result, secondary contamination of the substrate by the contaminated chemical solution is prevented, and a clean substrate surface is obtained.
  • FIG. 1 is a perspective view of an apparatus suitable for forming an oxide film according to the present invention.
  • FIG. 2 is a graph showing the residual amount of organic impurities after washing.
  • FIG. 3 is a graph showing the effect of removing the surfactant.
  • FIG. 4 is a graph showing the change in the amount of organic impurities attached when left in a clean room.
  • a nozzle rack that bundles multiple chemical supply nozzles, 4 Backside cleaning nozzle,
  • FIG. 1 shows an oxide film forming apparatus used in this example.
  • 1 is a closed tank body
  • 2 is a lid
  • 3 is a nozzle rack in which a plurality of chemical solution supply nozzles are bundled
  • 4 is a back surface cleaning nozzle
  • 5 is a rotating wafer holder
  • 6 is a rotating motor
  • 7 is a non-rotating motor.
  • the active gas inlet, 8 is a waste liquid outlet
  • 9 is a silicon wafer.
  • Nitrogen gas (purity: 99.99999%) is introduced from the inert gas inlet 7 in FIG. 1, a 6-inch silicon wafer 15 is set on the wafer holder 4, and the lid 2 is closed. 2.5 to 10 cc ultrapure water was supplied from the first nozzle of the nozzle rack 3 to the surface of the nozzle, and rotated at 300 rpm to uniformly wet the surface of the nozzle. This improves wettability and smoothes other processes.
  • ozone-added ultrapure water (2 ppm) was supplied from the second nozzle at 300 cc / min for 3 minutes to oxidize organic substances on the surface.
  • the ozone of the second nozzle was stopped, rinsed with ultrapure water, and ozone-added ultrapure water and impurities were washed and flown.
  • a 0.5% aqueous solution of hydrofluoric acid was supplied from the third nozzle at 300 cc Zmin for 2 minutes to remove the oxide film on the surface, and then from the first nozzle. Ultrapure water was supplied, and the chemicals and impurities were washed and flushed.
  • the wafer was dried by spinning at 3000 rpm.
  • the same chemical solution as for the front surface cleaning was constantly supplied from the back surface cleaning nozzle 3 toward the back surface, and the back surface was also cleaned at the same time.
  • the oxide film was peeled off with a 0.5% hydrofluoric acid aqueous solution. At this stage, the amount of organic substances adhering to the silicon surface was measured.
  • the cleaning method was as follows: (1) Batch cleaning by immersion using ammonia-hydrogen peroxide ultrapure water (0.05: 1: 5) at 80-90 ° C; (2) 80-90.
  • Figure 2 shows the ATR spectrum of the substrate surface after cleaning the silicon wafer by the above-mentioned cleaning method.
  • the scale of the vertical axis in FIG. 2 the film Langmuir-Buroje' preparative method Arakijin cadmium or scan Teariruamin, band intensity on a monomolecular film on a silicon wafer obtained by forming various areas, CH 2 stretching vibration And a calibration curve for the amount of adhesion was created, and the amount of organic impurities attached was determined from this.
  • the organic substance removal effect of ozone-added ultrapure water has a superior cleaning effect compared to other chemicals, and the effect is further improved by spin cleaning, and the organic matter is completely removed.
  • each of the ATRs was immersed in an aqueous solution of (a) a cationic, (b) anionic, and (c) a nonionic surfactant, and washed with each method. It is a spectrum.
  • the numbers (4) to (6) in the figure correspond to the numbers of the cleaning method in FIG. As shown in FIG. 3, it can be seen that the cleaning of this example has an excellent effect even on organic impurities such as a surfactant.
  • an oxide film was formed in a liquid in the same manner as in Example 1, and then the oxide film was formed at a low substrate temperature of 450 ° C in a plasma of a mixed gas of Ar and oxygen gas (300: 8).
  • a gate oxide film (7 nm) was grown by an argon ion-assisted oxidation method for growing a GaN film, and a MOS diode was fabricated in the same manner as in Example 1.
  • a bias was applied so that the energy of 7 Lugon ions was 9 eV.
  • a conventional MOS diode was fabricated in the same manner.
  • Table 2 shows the breakdown voltage of the gate oxide film of the fabricated MOS diode.
  • the numbers of the chemicals correspond to those in Table 1, and for reference, the oxide film formed directly by the ion assist acid method without forming an oxide film in the solution is shown as (Reference Example).
  • the gate oxide film of this example has a high withstand voltage, despite the growth of the oxide film at a low temperature, and greatly improves the reliability of the ultra-thin oxide film. You. That is, according to the present invention, a low-temperature process of a semiconductor device can be realized.
  • the breakdown voltage of the gate oxide film is improved by more than twice by forming the oxide film in the solution before the ion assisted oxidation.
  • the wafer was set in the ion-assisted oxidizing apparatus by being transported through the N 2 gas seal. This is to prevent organic impurities from adhering to the surface again by transporting in the air, as organic substances adhere to the surface just by leaving the wafer in the clean room as shown in Fig. 4. .
  • the characteristics of an oxide film of a silicon wafer can be significantly improved, and an oxide film with high characteristics can be formed even in a low-temperature process, so that higher performance and higher performance can be achieved.
  • An integrated semiconductor device can be realized.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Cleaning Or Drying Semiconductors (AREA)
  • Formation Of Insulating Films (AREA)

Abstract

L'invention porte sur un procédé de formation d'une couche d'oxyde à fort pouvoir diélectrique exempte de contamination organique sur la surface d'une galette de silicium. Ledit procédé s'applique à la fabrication d'un dispositif à semi-conducteurs à forte densité d'intégration et hautes performances. Le procédé de formation consiste à: diriger de l'eau ionisée d'une grande pureté sur un substrat en rotation pour en éliminer les matières organiques, mettre en contact la couche d'oxyde ainsi formée avec de l'acide fluorhydrique pour l'éliminer, et mettre le substrat en contact avec de l'eau ionisée d'une grande pureté pour former une couche d'oxyde.
PCT/JP1995/002730 1994-12-27 1995-12-27 Couche d'oxyde, son procede de formation et dispositif a semi-conducteurs WO1996020498A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP32577194A JP3669728B2 (ja) 1994-12-27 1994-12-27 酸化膜及びその形成方法、並びに半導体装置
JP6/325771 1994-12-27

Publications (1)

Publication Number Publication Date
WO1996020498A1 true WO1996020498A1 (fr) 1996-07-04

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PCT/JP1995/002730 WO1996020498A1 (fr) 1994-12-27 1995-12-27 Couche d'oxyde, son procede de formation et dispositif a semi-conducteurs

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WO (1) WO1996020498A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4181171A1 (fr) * 2021-11-12 2023-05-17 Siltronic AG Procédé de nettoyage d'une plaquette de semi-conducteur

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100677965B1 (ko) * 1999-11-01 2007-02-01 동경 엘렉트론 주식회사 기판처리방법 및 기판처리장치
JP4162211B2 (ja) * 2002-09-05 2008-10-08 コバレントマテリアル株式会社 シリコンウエハの洗浄方法および洗浄されたシリコンウエハ
JP4164324B2 (ja) * 2002-09-19 2008-10-15 スパンション エルエルシー 半導体装置の製造方法

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04354334A (ja) * 1991-05-31 1992-12-08 Tadahiro Omi 半導体の洗浄方法及び洗浄装置
JPH0529307A (ja) * 1991-07-23 1993-02-05 Seiko Epson Corp オゾン酸化法
JPH05283389A (ja) * 1992-03-31 1993-10-29 Nec Corp 半導体基板洗浄方法
JPH069300A (ja) * 1992-06-08 1994-01-18 Nec Corp 結晶成長用基板の前処理方法
JPH06244174A (ja) * 1993-08-04 1994-09-02 Tadahiro Omi 絶縁酸化膜の形成方法
JPH0714817A (ja) * 1993-06-22 1995-01-17 Tadahiro Omi 回転薬液洗浄方法及び洗浄装置

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04354334A (ja) * 1991-05-31 1992-12-08 Tadahiro Omi 半導体の洗浄方法及び洗浄装置
JPH0529307A (ja) * 1991-07-23 1993-02-05 Seiko Epson Corp オゾン酸化法
JPH05283389A (ja) * 1992-03-31 1993-10-29 Nec Corp 半導体基板洗浄方法
JPH069300A (ja) * 1992-06-08 1994-01-18 Nec Corp 結晶成長用基板の前処理方法
JPH0714817A (ja) * 1993-06-22 1995-01-17 Tadahiro Omi 回転薬液洗浄方法及び洗浄装置
JPH06244174A (ja) * 1993-08-04 1994-09-02 Tadahiro Omi 絶縁酸化膜の形成方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4181171A1 (fr) * 2021-11-12 2023-05-17 Siltronic AG Procédé de nettoyage d'une plaquette de semi-conducteur
WO2023083628A1 (fr) * 2021-11-12 2023-05-19 Siltronic Ag Procédé de nettoyage d'une tranche de semi-conducteur

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Publication number Publication date
JP3669728B2 (ja) 2005-07-13
JPH08181137A (ja) 1996-07-12

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