EP1958241A2 - Procede pour realiser un traitement chimique a sec de substrats, et son utilisation - Google Patents

Procede pour realiser un traitement chimique a sec de substrats, et son utilisation

Info

Publication number
EP1958241A2
EP1958241A2 EP06829345A EP06829345A EP1958241A2 EP 1958241 A2 EP1958241 A2 EP 1958241A2 EP 06829345 A EP06829345 A EP 06829345A EP 06829345 A EP06829345 A EP 06829345A EP 1958241 A2 EP1958241 A2 EP 1958241A2
Authority
EP
European Patent Office
Prior art keywords
substrate
gas
chlorine
silicon
etching
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
EP06829345A
Other languages
German (de)
English (en)
Inventor
Stefan Reber
Gerhard Willeke
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.)
Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV
Original Assignee
Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV
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 Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV filed Critical Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV
Publication of EP1958241A2 publication Critical patent/EP1958241A2/fr
Ceased legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/91—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics involving the removal of part of the materials of the treated articles, e.g. etching
    • 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
    • C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/53—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone involving the removal of at least part of the materials of the treated article, e.g. etching, drying of hardened concrete
    • C04B41/5338—Etching
    • C04B41/5346—Dry etching
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F71/00—Manufacture or treatment of devices covered by this subclass
    • H10F71/121—The active layers comprising only Group IV materials
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P36/00—Gettering within semiconductor bodies
    • H10P36/03—Gettering within semiconductor bodies within silicon bodies
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P70/00—Cleaning of wafers, substrates or parts of devices
    • H10P70/10—Cleaning before device manufacture, i.e. Begin-Of-Line process
    • H10P70/12—Cleaning before device manufacture, i.e. Begin-Of-Line process by dry cleaning only
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/547—Monocrystalline silicon PV cells
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24479—Structurally defined web or sheet [e.g., overall dimension, etc.] including variation in thickness

Definitions

  • the invention relates to a process for the dry chemical treatment of substrates selected from the group consisting of silicon, ceramic, glass and quartz glass, in which the substrate is treated in a heated reaction chamber with a gas containing hydrogen chloride as an etchant, and a process which can be prepared in this way Substrate.
  • substrates selected from the group consisting of silicon, ceramic, glass and quartz glass, in which the substrate is treated in a heated reaction chamber with a gas containing hydrogen chloride as an etchant, and a process which can be prepared in this way Substrate.
  • the invention also relates to uses of the aforementioned method.
  • etching processes are known from the prior art for the surface treatment and cleaning of wafers, which are based on wet and dry chemical reactions with different chemicals.
  • the methods used in the surface treatment and cleaning of such substrates can be divided into the following applications: Removal of surface areas to remove crystal damage from wafers. An example of this is the so-called damage rates in the pretreatment of solar cells.
  • Removal of typically thin surface layers to remove surface contaminants from the wafer includes, for example, wet chemical oxidation with hot nitric acid as an etchant and subsequent etching with hydrofluoric acid to remove the SiO?
  • the cleaning of the volume of a wafer by temperature treatment which can be accompanied by further etching steps.
  • An example of this is so-called gettering, ie tempering in a phosphorus-containing atmosphere (eg POCl 3 and O2), followed by removal of the surface area, as a result of which contamination has accumulated from the volume of the wafer as a result of the treatment.
  • gettering ie tempering in a phosphorus-containing atmosphere (eg POCl 3 and O2)
  • Texture of surfaces of solar cells is that a previously damaged crystal surface is often required to ensure a homogeneous texture, as is the case, for example, with acidic wet chemical texture etching or a plasma texture etcher.
  • a method for dry chemical treatment of substrates is selected from the group consisting of silicon, ceramic, glass and
  • Quartz glass is provided, in which the substrate is treated in a heated reaction chamber with an etching gas from a chlorine-containing gas or a gas containing at least one chlorine-containing compound.
  • the substrate is cleaned by selecting the temperature and the concentration of the chlorine-containing compound in the etching gas so that the volume contained compounds Cleaning and / or foreign atoms are at least partially removed.
  • this method entails that the temperature-controlled etching gas triggers a chemical reaction with the silicon and with the foreign atoms contained in silicon, as a result of which the silicon is converted from the solid into the gaseous phase and the foreign atoms are converted into chlorides.
  • the gas composition and the temperature effects can be exploited that represent a significantly better alternative to the etching application known from the prior art.
  • the HCl gas etches the Si surface very quickly, isotropically and with a high degree of uniformity, ie a reflective surface is generated.
  • metal atoms are also converted with chlorine from the etching gas to solid chlorides, which can be removed with the gas stream.
  • metals especially iron, which is particularly harmful to solar cells, are very mobile and easy to diffuse in silicon. Contaminant precipitates can dissolve and atoms of the precipitate can mobilize. This is used according to the invention by exposing a silicon wafer to a temperature treatment in an atmosphere containing chlorine.
  • the etching gas preferably contains hydrogen chloride or consists entirely of hydrogen chloride.
  • concentration of the chlorine-containing compound can be selected from the range from 1 to 100% by volume. At the same time, a temperature of 700 to 1600 ° C. is preferred in order to allow the foreign atoms contained in the volume of the substrate to diffuse onto the surface of the substrate.
  • a variant of the method according to the invention relates to the removal of contaminants from the
  • Substrate that is in the form of precipitates is preferably chosen at temperatures in the range from 300 to 1000 ° C., since precipitates can be dissolved at this temperature and the individual constituents then diffuse to the surface. It is only after the precipitates have dissolved that they are then accessible to the chlorine-containing compound and, as described, can be chemically reacted and removed.
  • the concentration of the chlorine-containing compound in the etching gas is preferably selected so that foreign atoms or dissolved constituents of precipitates in the area of the substrate are converted into the corresponding chlorides.
  • the temperature and the concentration of the chlorine-containing compound in the etching gas in the method according to the invention are preferably matched to one another such that the rate of diffusion of the foreign atoms in the direction of the substrate surface is greater than the etching rate for the substrate.
  • Another preferred variant of the method according to the invention provides for isotropic etching and removal during the treatment of a surface layer of the substrate.
  • surface layers of a silicon wafer can be removed with extremely high etching rates of> 40 ⁇ m / min without causing further crystal damage.
  • the surface layer is preferably removed in a thickness in the range from 5 to 50 ⁇ m, particularly preferably in the range from 10 to 20 ⁇ m.
  • the methods known from the prior art require about 2 for the removal in a thickness in the latter region up to 5 min.
  • the method according to the invention can achieve an acceleration by a factor of 10 here.
  • the impurities and foreign atoms released during the etching can preferably be removed in a simple manner by the gas stream.
  • medium etching rates can be achieved at medium temperatures, ie temperatures in the range from 900 to 1100 ° C., which allow a controlled texturing of the surface.
  • a texturing can increase the coupling of light, for example for solar cells, that is, reduce the reflectivity, by treating the surface at the temperatures mentioned with the gas composition according to the invention.
  • light refraction or light scattering takes place, which ensures improved light utilization, particularly in the case of crystalline silicon thin-film solar cells.
  • Another variant provides that the surface of a silicon wafer is textured, on which a silicon layer is subsequently deposited, so that buried holes are formed on the former surface of the wafer by the wet deposition. These holes have a reflective effect on incoming light rays and thus also contribute to increasing the utilization of light (so-called guiding traffic).
  • Another preferred variant of the method according to the invention provides for the removal of surface layers to remove surface contamination from substrates.
  • Lower temperatures are temperatures in the range of about 300 to choose to 900 0 C, and then the surface of a silicon wafer is cleaned by the reactive chlorine-containing gas by effectively as metal impurities, only a very thin silicon layer is removed.
  • the combination of different pretreatment steps is particularly preferred in the method according to the invention in order to enable an overall process of pretreating substrates.
  • a variant of an overall process designed in this way which can be carried out as a continuous process, has the following steps: a) A substrate made of silicon is obtained by gettering with an etching gas from a chlorine-containing gas or a gas containing a chlorine-containing compound at temperatures in the range from 300 to 1600 0 C to remove contamination
  • step a) before, after or simultaneously with
  • Step b) or all three steps can be carried out simultaneously.
  • the overall process described here can be supplemented by further process steps. These include: d) A layer of silicon is deposited on the substrate treated with steps a) to c) by at least partially replacing the etching gas with a deposition gas containing chlorosilanes. e) The layer deposited in d) becomes isotropic
  • a layer of silicon is deposited by at least partially replacing the etching gas with a deposition gas containing chlorosilanes with complementary doping to produce a pn junction. Step e) can be done both before and after
  • Step f) are carried out.
  • the invention also provides a method for texturing tion of wafers in which a wafer in a heated reaction chamber at temperatures of 900 to 1100 0 C by a Texture gas from a chlorine-containing gas or at least one chlorine-containing compound gas is treated.
  • a substrate selected from the group consisting of silicon, ceramic, glass and quartz glass is also provided, which can be produced by the previously described method. Such substrates are distinguished by a purity which is superior to that known from the prior art.
  • the method according to the invention is used in the treatment steps described in the pretreatment of substrates, ie the purification of the volume of substrates, the removal of crystal damage in wafers, the removal of surface impurities in substrates and the texturing of wafers.
  • FIG. 2a shows a microscopic picture of the surface of a substrate textured according to the invention.
  • 2b shows a reflection spectrum of a substrate textured according to the invention.
  • 3 shows a micrograph of the cross section of a wafer which has been textured according to the invention and then coated with an additional silicon layer.
  • example 1
  • silicon wafers were made from metallurgical (ie contaminated with approx. 0.5 at% dopants and metals) raw materials. posed. These still contained large amounts of dopants and, somewhat more difficult to detect, also of metals. Such silicon wafers were examined either directly or after volume cleaning in a hot 20% HCl in an E 2 atmosphere (1300 ° C., 5 min) by means of mass spectrometry. 1 shows the prepared measurement results: the dopants which are difficult to convert into chlorides are fully retained, while, for example, the more easily changeable copper is reduced by more than an order of magnitude.
  • FIG. 2a a superficially microporous hole structure.
  • the reflection behavior is plotted in FIG. 2b): before the etching treatment, an Si substrate has between 25 and 45% reflection, then between 5 and 15%. Also in a production of this structure according to the invention, i.e. additional volume cleaning, the measured properties would be maintained.
  • a silicon layer was deposited in-situ on a surface similar to that shown in FIGS. 2a ⁇ and b).
  • the cross section in Fig. 3 shows that the holes created by the texture partially. remain as pores and thereby create a light-reflecting effect. Despite the rough surface, the deposited layer grows very evenly and with high crystal quality.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Drying Of Semiconductors (AREA)
  • Cleaning Or Drying Semiconductors (AREA)
  • Cleaning By Liquid Or Steam (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

La présente invention concerne un procédé pour réaliser un traitement chimique à sec de substrats choisis dans le groupe comprenant le silicium, la céramique, le verre et le verre de quartz, le substrat étant traité dans une chambre réactionnelle chauffée avec un gaz qui contient du chlorure d'hydrogène en tant qu'agent d'attaque chimique. L'invention a également pour objet un substrat réalisé selon le procédé de l'invention. L'invention concerne aussi des applications du procédé mentionné précédemment.
EP06829345A 2005-12-08 2006-12-06 Procede pour realiser un traitement chimique a sec de substrats, et son utilisation Ceased EP1958241A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102005058713A DE102005058713B4 (de) 2005-12-08 2005-12-08 Verfahren zur Reinigung des Volumens von Substraten, Substrat sowie Verwendung des Verfahrens
PCT/EP2006/011716 WO2007065658A2 (fr) 2005-12-08 2006-12-06 Procede pour realiser un traitement chimique a sec de substrats, et son utilisation

Publications (1)

Publication Number Publication Date
EP1958241A2 true EP1958241A2 (fr) 2008-08-20

Family

ID=38055877

Family Applications (1)

Application Number Title Priority Date Filing Date
EP06829345A Ceased EP1958241A2 (fr) 2005-12-08 2006-12-06 Procede pour realiser un traitement chimique a sec de substrats, et son utilisation

Country Status (6)

Country Link
US (1) US8569175B2 (fr)
EP (1) EP1958241A2 (fr)
JP (1) JP5133257B2 (fr)
CN (1) CN101326619A (fr)
DE (1) DE102005058713B4 (fr)
WO (1) WO2007065658A2 (fr)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5176423B2 (ja) * 2007-08-10 2013-04-03 東京エレクトロン株式会社 石英製品のベーク方法及び記憶媒体
JP6108453B2 (ja) * 2013-05-21 2017-04-05 大陽日酸株式会社 基板の再利用方法及び基板洗浄装置
CN103467108A (zh) * 2013-08-21 2013-12-25 长兴攀江冶金材料有限公司 一种环保型硅质干式料的制备方法
JP5938113B1 (ja) 2015-01-05 2016-06-22 信越化学工業株式会社 太陽電池用基板の製造方法
SG10202010798QA (en) * 2019-11-08 2021-06-29 Tokyo Electron Ltd Etching method and plasma processing apparatus

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JPH11121441A (ja) * 1997-10-20 1999-04-30 Fuji Electric Co Ltd 炭化けい素半導体基板の製造方法
JP2003100693A (ja) * 2001-09-26 2003-04-04 Toshiba Ceramics Co Ltd シリコン部材の純化方法

Also Published As

Publication number Publication date
US8569175B2 (en) 2013-10-29
WO2007065658A2 (fr) 2007-06-14
US20090197049A1 (en) 2009-08-06
JP5133257B2 (ja) 2013-01-30
JP2009518834A (ja) 2009-05-07
WO2007065658A3 (fr) 2007-11-08
DE102005058713A1 (de) 2007-06-14
CN101326619A (zh) 2008-12-17
DE102005058713B4 (de) 2009-04-02

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