EP0938599A1 - Procede et dispositif pour controler une matiere fondue servant a la production de cristaux - Google Patents

Procede et dispositif pour controler une matiere fondue servant a la production de cristaux

Info

Publication number
EP0938599A1
EP0938599A1 EP98947503A EP98947503A EP0938599A1 EP 0938599 A1 EP0938599 A1 EP 0938599A1 EP 98947503 A EP98947503 A EP 98947503A EP 98947503 A EP98947503 A EP 98947503A EP 0938599 A1 EP0938599 A1 EP 0938599A1
Authority
EP
European Patent Office
Prior art keywords
crucible
camera
melt
initiated
process step
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.)
Withdrawn
Application number
EP98947503A
Other languages
German (de)
English (en)
Inventor
Burkhard ALTEKRÜGER
Joachim Aufreiter
Dieter BRÜSS
Klaus Kalkowski
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.)
Leybold Systems GmbH
Original Assignee
Leybold Systems GmbH
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
Priority claimed from DE19738438A external-priority patent/DE19738438B4/de
Priority claimed from DE1998117709 external-priority patent/DE19817709B4/de
Application filed by Leybold Systems GmbH filed Critical Leybold Systems GmbH
Publication of EP0938599A1 publication Critical patent/EP0938599A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/20—Controlling or regulating
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/20—Controlling or regulating
    • C30B15/22—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal
    • C30B15/26—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal using television detectors; using photo or X-ray detectors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B11/00—Measuring arrangements characterised by the use of optical techniques
    • G01B11/08—Measuring arrangements characterised by the use of optical techniques for measuring diameters
    • 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
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10S117/90—Apparatus characterized by composition or treatment thereof, e.g. surface finish, surface coating
    • 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
    • Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10T117/10—Apparatus
    • Y10T117/1004—Apparatus with means for measuring, testing, or sensing
    • 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
    • Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10T117/10—Apparatus
    • Y10T117/1004—Apparatus with means for measuring, testing, or sensing
    • Y10T117/1008—Apparatus with means for measuring, testing, or sensing with responsive control means
    • 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
    • Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10T117/10—Apparatus
    • Y10T117/1004—Apparatus with means for measuring, testing, or sensing
    • Y10T117/1012—Apparatus with means for measuring, testing, or sensing with a window or port for visual observation or examination

Definitions

  • the invention relates to a device according to the preamble of patent claim 1 and a method according to the preamble of patent claim 4.
  • a method for pulling a single crystal from a melt in which the individual crystals are pulled up while the data based on numerous conditions which influence the pulling process are recorded and compared with corresponding other data (EP 0 536 405 AI) .
  • z. B a laser beam on the surface of a melt located in a crucible. The position of the molten surface is determined on the basis of the detection of a reflected laser beam, and the crucible is raised in accordance with the difference between the measured position and a predetermined position.
  • an optical system or a method for regulating the growth of a silicon crystal in which the diameter of a silicon crystal which is drawn from a melt is measured with the aid of a television camera, the surface of this melt having a meniscus which acts as a light area is visible in the vicinity of the silicon crystal (EP 0 745 830 A2).
  • an image pattern of part of the bright area near the silicon crystal is first imaged by means of a camera.
  • the characteristics of the image pattern are then detected.
  • the characteristic of an image pattern is, for example, the light intensity gradient.
  • An edge of the bright area is then defined as a function of the detected characteristics.
  • the invention is therefore based on the object of monitoring the melting process of raw materials, from which single crystals are subsequently drawn.
  • the advantage achieved by the invention is, in particular, that the process time is shortened, overheating of the melt and crucible is avoided and the ⁇ 2 "age of the melt is minimized. It is through the use of a special sensor It is therefore possible to carry out a meltdown check before the melted material has completely melted. In addition, individual differences per batch can be recognized and taken into account.
  • FIG. 1 shows a schematic diagram of a device according to the invention
  • 2a shows a plan view of a crucible with melting material
  • FFiigg .. 22bb a graphical representation of the brightness distribution along a horizontal line on the crucible
  • FIG. 3 shows an enlarged representation of a measuring window of a camera directed at the surface of a crucible
  • Fig. 4 is a flowchart relating to the process flow in the detection of solid or liquid components of a melt.
  • This device 1 shows a device 1 with which it is possible to recognize the melting of a melting material at an early stage.
  • This device 1 is based on an optical principle, according to which those areas of a melt which are liquid emit less visible light than those areas which are still solid or which have solidified out of the melt.
  • the color and / or color saturation principle can also be used, because molten materials differ from unmelted material not only in terms of brightness, but also in terms of color and / or color saturation.
  • a camera 2 which can be a CCD video camera.
  • This camera 2 is arranged obliquely above a crucible 7, in which a melt 3 is located. With this camera 2, the surface 4 of the melt 3 or at least a part of this surface 4 is viewed.
  • the crucible 7 can be moved via a shaft 5 and a gear 6 with the aid of a motor 9, for example from top to bottom. It is also possible to make it rotate.
  • the crucible 7 is located in a housing which consists of an upper part 12, a middle part 13 and a lower part 14.
  • the lower part 14 is provided with two gas outlet openings 25, 26.
  • An electric heater 16 is arranged around the gel 7 and is supplied with electrical energy from a heating power supply 17.
  • parts (not shown) can be brought into the vicinity of the melt 3.
  • the threaded rod 18 is surrounded by a cylindrical bulge or a tube 23 of the upper part 12, which is provided with a gas inlet opening 24.
  • the output signals of the camera 2 are fed to an image evaluation unit 37, which exchanges data with a controller 38.
  • This control 38 can be influenced by means of an operating unit 39, for example a keyboard.
  • Control 38 it is possible to control the drive 6, 9 for the crucible 7 and the heating power supply 17.
  • the crucible 7 is shown in a view from above.
  • liquid material 50 e.g. B. liquid silicon, in which there are some islands
  • the liquid melt 50 emits less brightness than the solidified islands 51 to 54 because the solidified material reflects the visible light better than the liquid material. As a result, the islands 51 to 54 appear lighter than the liquid material 50 surrounding them.
  • a measurement window is designated, which corresponds to the viewing angle of the camera 2, d. H. the camera 2 captures the area of the crucible 7 defined by the measuring window 55.
  • the reference number 56 denotes a measuring line, the meaning of which will be discussed further below.
  • 2b shows the brightness of the content of the crucible in an x coordinate. It can be seen here that in those places where the fixed islands 51 to 54 are located, a greater brightness B ⁇ . . . B4 prevails as in those places where the liquid melt is located.
  • measuring window 55 shows the measuring window 55 with the melt 50 and the islands 51 to 54 located therein once again on an enlarged scale.
  • About the measuring Window 55 are several horizontal and vertical measuring lines 60 to 69 and 70 to 86, which form a grid. These measuring lines 60 to 69, 70 to 86 are scanning lines and columns of the CCD camera 2. The measuring window recorded by the CCD camera 2 is thus scanned line by line and column by column, ie the scanning lines and - shown in FIG. columns are controlled time-multiplexed.
  • the area of island 52 can be calculated.
  • the areas of the other islands 51, 53, 54 can be calculated in a corresponding manner. This in turn creates the possibility of determining the ratio of the liquid surface to the solid surface. Various values can be set for these ratios, upon reaching which certain process steps are carried out.
  • the disappearance of the portion of the solid surface is of particular interest because this state indicates a finished melt. Since the disappearance of the solid bodies can be simulated for various reasons, a predetermined holding time is observed during which the
  • the process flow according to the invention is shown in the form of a flow chart.
  • start - block 100 the surface of the melt imaged by the CCD camera 2 is read as an image in digital form into a memory (not shown), which is indicated by block 101.
  • the scanned image is now, cf.
  • Block 102 scanned line by line and / or column by column and checked for brightness. Whenever the difference in brightness between adjacent points in a row and / or a column exceeds a predetermined threshold value, the location coordinate of the transition point - the so-called edge - is determined and stored, cf. Block 103.
  • the points P j to P9 of the island 52 can be found.
  • a curve can be laid through these points P j to P, so that the contour of the island 52 is known.
  • the area of the island 52 can be calculated from this.
  • a predefined melt-solid behavior can be defined, upon reaching which a certain process step is to be carried out. This is indicated by block 105.
  • Such a process step can consist, for example, in reducing the heating power for the heating element 16 or in increasing the speed of the crucible.
  • the threshold for the number of edges can e.g. B. can be entered via the control unit 39.
  • This hold time ensures that all materials have actually melted and that you can now start pulling a crystal.
  • the selected holding time depends on the number of revolutions of the crucible. If the crucible is turned quickly, the holding time can be shortened because the increased number of turns means that any that are still not melted
  • Chunks get to an area faster where they melt.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Length Measuring Devices By Optical Means (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Investigating And Analyzing Materials By Characteristic Methods (AREA)

Abstract

L'invention concerne un dispositif pour contrôler une matière fondue servant à la production de cristaux. A cet effet, il est prévu une caméra qui fournit une image représentant au moins des parties de la surface du contenu d'un creuset. Ce dispositif d'évaluation permet d'évaluer l'image fournie par la caméra, notamment en ce qui concerne les fractions solides et liquides de la surface du contenu du creuset.
EP98947503A 1997-09-03 1998-09-02 Procede et dispositif pour controler une matiere fondue servant a la production de cristaux Withdrawn EP0938599A1 (fr)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
DE19738438 1997-09-03
DE19738438A DE19738438B4 (de) 1997-09-03 1997-09-03 Einrichtung und Verfahren für die Bestimmung des Durchmessers eines Kristalls
DE1998117709 DE19817709B4 (de) 1998-04-21 1998-04-21 Verfahren für die Überwachung einer Schmelze für die Herstellung von Kristallen
DE19817709 1998-04-21
PCT/EP1998/005565 WO1999011844A1 (fr) 1997-09-03 1998-09-02 Procede et dispositif pour controler une matiere fondue servant a la production de cristaux

Publications (1)

Publication Number Publication Date
EP0938599A1 true EP0938599A1 (fr) 1999-09-01

Family

ID=26039641

Family Applications (2)

Application Number Title Priority Date Filing Date
EP98114783A Withdrawn EP0903428A3 (fr) 1997-09-03 1998-08-06 Appareillage et méthode pour déterminer les diamètres d'un cristal
EP98947503A Withdrawn EP0938599A1 (fr) 1997-09-03 1998-09-02 Procede et dispositif pour controler une matiere fondue servant a la production de cristaux

Family Applications Before (1)

Application Number Title Priority Date Filing Date
EP98114783A Withdrawn EP0903428A3 (fr) 1997-09-03 1998-08-06 Appareillage et méthode pour déterminer les diamètres d'un cristal

Country Status (6)

Country Link
US (2) US6341173B2 (fr)
EP (2) EP0903428A3 (fr)
JP (2) JPH11153418A (fr)
KR (2) KR20000068898A (fr)
TW (1) TW460637B (fr)
WO (1) WO1999011844A1 (fr)

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CN108680106B (zh) * 2018-06-15 2020-05-05 中国科学院上海光学精密机械研究所 Kdp类晶体生长参数的实时测量系统及其测量方法
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DE102019132219B4 (de) * 2019-11-27 2021-10-21 MAX-PLANCK-Gesellschaft zur Förderung der Wissenschaften e.V. Verfahren zum Kalibrieren eines Systems, System, Durchflussmesszellenanordnung und Speichermedium
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CN112857297B (zh) * 2021-01-07 2023-01-24 西安奕斯伟材料科技有限公司 单晶棒直径测量装置、单晶棒生长系统及方法
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CN114688984B (zh) * 2022-01-12 2022-12-06 苏州天准科技股份有限公司 单双光圈的检测方法、存储介质、终端和拉晶设备
CN114399489B (zh) * 2022-01-12 2022-11-25 苏州天准科技股份有限公司 拉晶过程中光圈直径的监测方法、存储介质和终端
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Also Published As

Publication number Publication date
JPH11153418A (ja) 1999-06-08
KR20000068898A (ko) 2000-11-25
US6341173B2 (en) 2002-01-22
EP0903428A2 (fr) 1999-03-24
EP0903428A3 (fr) 2000-07-19
TW460637B (en) 2001-10-21
KR19990029481A (ko) 1999-04-26
WO1999011844A1 (fr) 1999-03-11
US20010043733A1 (en) 2001-11-22
US6203610B1 (en) 2001-03-20
JP2001505523A (ja) 2001-04-24

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