EP2701458B1 - MoSi2-based coil heater and tubular heater module having the same - Google Patents

MoSi2-based coil heater and tubular heater module having the same Download PDF

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Publication number
EP2701458B1
EP2701458B1 EP13306161.4A EP13306161A EP2701458B1 EP 2701458 B1 EP2701458 B1 EP 2701458B1 EP 13306161 A EP13306161 A EP 13306161A EP 2701458 B1 EP2701458 B1 EP 2701458B1
Authority
EP
European Patent Office
Prior art keywords
heater
coil
mosi
interheater
distance
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.)
Not-in-force
Application number
EP13306161.4A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP2701458A1 (en
Inventor
Toshiyuki Kuratomi
Takashi Ono
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.)
Riken Corp
Original Assignee
Riken Corp
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Publication date
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Publication of EP2701458A1 publication Critical patent/EP2701458A1/en
Application granted granted Critical
Publication of EP2701458B1 publication Critical patent/EP2701458B1/en
Not-in-force legal-status Critical Current
Anticipated expiration legal-status Critical

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    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/62—Heating elements specially adapted for furnaces
    • H05B3/64—Heating elements specially adapted for furnaces using ribbon, rod, or wire heater
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/40—Heating elements having the shape of rods or tubes
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
    • H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
    • H05B3/141—Conductive ceramics, e.g. metal oxides, metal carbides, barium titanate, ferrites, zirconia, vitrous compounds
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/40—Heating elements having the shape of rods or tubes
    • H05B3/54—Heating elements having the shape of rods or tubes flexible
    • H05B3/56—Heating cables
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
    • H05B2203/018—Heaters using heating elements comprising mosi2

Definitions

  • the present invention relates to an MoSi 2 -based coil heater and a tubular heater module using the same.
  • MoSi 2 (molybdenum disilicide)-based heater is used in a tubular heat treatment furnace which can be used at a high temperature in the air.
  • a semi-cylindrical wave-type multi-shank heater and a cylindrical spiral (coil-shaped) heater disclosed in JP-A-8-143365 are known as the MoSi 2 -based heater.
  • the semi-cylindrical wave-type multi-shank heater has been heretofore used in a large-scale tubular heat treatment furnace. When the bore diameter of the semi-cylindrical wave-type multi-shank heater becomes large, there is however a problem of troublesome installation, etc.
  • the cylindrical spiral (coil-shaped) heater has a problem of thermal deformation and temperature uniformity when the coil inner diameter of the heater is not smaller than 300 mm, so that the cylindrical spiral (coil-shaped) heater has not been realized in the existing circumstances.
  • Document US-A-5 763 856 discloses a MoSi 2 -based coil heater with a coil having an inner diameter not smaller than 300mm.
  • An object of the invention is to provide an MoSi 2 -based coil heater which is excellent in durability and temperature uniformity and which has an inner diameter not smaller than 300 mm.
  • the present inventors have found from eager researches that an MoSi 2 -based coil heater high in temperature uniformity, little in thermal deformation and excellent in durability can be obtained by defining the relation between the inner diameter (D) of a coil (in other words, inner diameter (D) of a helix made by a coil) and the interheater distance (t) in a predetermined range even if the inner diameter (D) of the coil is not smaller than 300 mm, so that the present inventors have hit upon the invention.
  • a subject of the invention is an MoSi 2 -based coil heater including: a coil having an inner diameter (D) not smaller than 300 mm; wherein: the inner diameter of the coil and the interheater distance (t) satisfy the condition: 0.9 ⁇ t/(D/2) 1/2 ⁇ 4.0.
  • the MoSi 2 -based coil heater according to the invention is disposed in coil-shaped grooves formed at an inner circumference of a ceramic mold.
  • an MoSi 2 -based coil heater according to the invention in which the inner diameter (D) of a coil and the interheater distance (t) satisfy the aforementioned relational expression, temperature uniformity can be kept high in combination with a rapid temperature rise effect by the MoSi 2 -based heater to be able to contribute to improvement in miniaturization and yield of devices. Moreover, by satisfying the aforementioned relational expression, the MoSi 2 -based coil heater can expand and contract freely in the grooves formed in the inner circumferential surfaces of the ceramic molds so that the MoSi 2 -based coil heater can be kept in a free state. Thus, it is possible to provide a tubular heater module which avoids trouble such as breaking due to restriction in the ceramic molds.
  • the MoSi 2 -based coil heater and the tubular heater module according to the invention are effectively used in a heat treatment apparatus used in a semiconductor manufacturing process, a glass or metal melting furnace, or the like.
  • a coil heater according to the invention can be produced in such a manner that intermediate members each not larger than a semicircle (a half circle) are produced from a wire material with a length up to about 2000 mm obtained by extrusion-molding an MoSi 2 -based powder material and sintering the MoSi 2 -based powder material in a non-oxidizing atmosphere in a vacuum furnace, and the intermediate members are formed into a coil shape by electrically butt bonding, that is, so-called diffusion bonding.
  • a method of producing a coil heater according to the invention is not limited to the aforementioned method.
  • An MoSi 2 -based heater wire material according to the invention is produced in such a manner that a green body for extrusion molding, containing MoSi 2 powder, binder, water, etc. is made and molded into a rod-like raw material of the order of meter (m), and the rod-like raw material is dried, debound and sintered.
  • a water-soluble binder such as methylcellulose, swelling bentonite, or the like can be used as the binder.
  • Sintering is performed in a temperature range of about 1350°C to about 1600°C in a non-oxidizing atmosphere though sintering varies according to the composition of the MoSi 2 -based material and a target organization.
  • the wire diameter of the MoSi 2 -based heater wire material is in a range of 2 mm to 12 mm.
  • the wire diameter is larger than 12 mm, it is difficult to produce the MoSi 2 -based heater wire material because cracks occur in the MoSi 2 -based heater wire material in the drying step after extrusion.
  • a terminal wire material having a diameter about twice as large as the heater wire diameter is generally used for the MoSi 2 -based heater in order to suppress heating of a terminal portion.
  • the wire diameter of the MoSi 2 -based heater wire material is not larger than 12 mm. It is more preferable that the wire diameter is in a range of 2 mm to 8 mm. It is further preferable that the wire diameter is in a range of 3 mm to 6 mm.
  • FIGs. 1A, 1B, and 1C schematically show a process of producing a semicircular intermediate member.
  • the two clamp portions 2 are moved in a direction of 90° with respect to the initial linear direction of the heater wire material 1 until the two clamp portions 2 become parallel with each other.
  • the temperature is in a range of 1400°C to 1550°C, and the tensile load gives a force small enough so as not to expand the heater wire material and not to reduce the diameter of the heater wire material.
  • the heater wire material 1 is cut so as to be shaped like a semicircle and end surfaces 4 are polished so as to become perpendicular to a line tangential to the semicircle to thereby form a semicircular member 11. It is a matter of course that another shape, such as a 1/3 circular shape or a 1/4 circular shape, not larger than the semicircular shape may be used though the number of junctions increases in a bonding process as a postprocess.
  • a coil heater is produced by diffusion bonding of semicircular members 11 to each other.
  • Fig. 2 schematically shows a process of producing a coil heater by diffusion bonding.
  • places near to the end surfaces 4 of the semicircular members 11 are fixed by clamp portions 6 so that the places can be pressed perpendicularly to each joint surface, that is, in a direction tangential to each junction.
  • a predetermined pressure is applied on each joint surface 4 through the clamp portions 6, the joint surface 4 is supplied with electricity and pressurized at a high temperature so that each junction 5 is formed by welding.
  • the clamp portions 6 are designed to be able to fix the semicircular members 11 with a curvature and selected in accordance with the curvature of the coil.
  • the semicircular members 11 are bonded while shifted by a predetermined pitch whenever bonding is completed by a half turn.
  • terminals are bonded to opposite end portions of the coil heater by diffusion bonding likewise.
  • the coil inner diameter (D) and the interheater distance (t) in the coil heater satisfy the relation: 0.9 ⁇ t/(D/2) 1/2 ⁇ 4.0.
  • the interheater distance (t) is defined as the length of a gap between adjacent heaters of the coil (in other words, a distance between adjacent coils of a helix).
  • t/(D/2) 1/2 is smaller than 0.9, deformation becomes large undesirably.
  • t/(D/2) 1/2 is larger than 4.0, temperature uniformity is lowered undesirably in addition to increase of deformation. It is preferable that 0.9 ⁇ t/(D/2) 1/2 ⁇ 3.0 is satisfied.
  • each terminal is machined to have the same diameter as the heater wire material so as to be able to be bonded to the heater wire material. Moreover, it is preferable that the terminal is bent into an L shape so that the other side of the terminal is exposed outside from a ceramic mold.
  • a heat insulating material used in the tubular heater module according to the invention is a tubular ceramic mold.
  • An alumina material high in heat resistance is preferred as the material of the tubular ceramic mold.
  • wire breaking may be often caused by abnormal heating due to local deformation when the expansion/contraction is restricted. Accordingly, an idea to prevent the expansion/contraction from being restricted is required for disposing the MoSi 2 -based coil heater in the mold.
  • the MoSi 2 -based heater according to the background art is U-shaped and takes a method of hanging down the MoSi 2 -based heater by staples. In Fig.
  • an MoSi 2 -based coil heater 21 is disposed in a free state in coil-shaped grooves 31 formed in a ceramic mold 30. That is, though the MoSi 2 -based coil heater 21 is supported by one side surface of each groove, the MoSi 2 -based coil heater 21 is allowed to move freely on the grooves without protruding out of the grooves. For this reason, it is preferable that the inner surface of each of the grooves 31 in the ceramic mold exhibits little reaction to the MoSi 2 -based coil heater 21 and has a hardness sufficient to be not deformed.
  • the groove has a sufficient width and a sufficient depth to prevent the MoSi 2 -based coil heater 21 from being restricted.
  • staples may be put across some of the grooves to prevent the MoSi 2 -based coil heater from protruding out of the grooves 31.
  • a pseudo-semicircular intermediate member having an inner diameter of 300 mm were clamped and the intermediate member was molded from the rod-like sintered compact of 3 mm ⁇ ⁇ 700 mm by bending (bending temperature 1450°C) according to the method shown in Figs. 1A, 1B and 1C .
  • the intermediate member was cut into a semicircular shape, and two cut surfaces of the intermediate member were polished so as to be on one plane.
  • the semicircular members were bonded like a coil having a pitch (P) of 23 mm by butt resistance welding according to the method shown in Fig. 2 .
  • a coil heater having 20 turns was produced from 40 semicircular members.
  • terminals produced from the 6 mm ⁇ rod-like sintered compact by machining were bonded to opposite ends.
  • Grooves having a groove width of 6 mm and a depth of 10 mm were formed at intervals of a pitch (P) of 23 mm in a pair of semi-cylindrical ceramic molds having an inner diameter of 294 mm, an outer diameter of 460 mm and a height of 500 mm.
  • the coil heater having 20 turns was set to be entirely located inside the grooves in one semi-cylindrical ceramic mold.
  • the other semi-cylindrical ceramic mold was put thereon. Joint surfaces of the molds were bonded to each other by a heat-resistant ceramic adhesive agent. Incidentally, grooves through which terminals passed were processed in the joint surfaces of the molds.
  • Alumina heat-insulating materials having a thickness of 100 mm were disposed in a lower portion (bottom portion) and an upper portion (lid portion) of the produced tubular heater module, and a B thermocouple for control of the temperature of the heater module was set in a position 10 mm far toward the center from the inner circumferential surface of the heater module and 250 mm far from the lid portion. Measurement of the temperature distribution was performed in the condition that the temperature of the heater module was set at 1500°C, and another B thermocouple for measurement of the temperature distribution was set in a position 50 mm far toward the center from the inner circumferential surface of the heater module and in a range of 300 mm between a position 100 mm far from the lid portion and a position 100 mm far from the bottom portion. The temperature changed slightly in accordance with the positional relation with respect to the coil but the difference ⁇ T between the maximum and minimum of the temperature was not larger than 3°C.
  • the temperature was changed in a range of room temperature to 1500°C.
  • a pattern of cooling to the room temperature after keeping the temperature at 1500°C for 1 hour was repeated by 500 cycles.
  • Fig. 4 whether deformation was observed or not, was determined based on the positional relation of the coil heater after the test to the heater grooves of the molds. When there was any place where a section of the heater protrudes inward from the inner circumferential ends of the heater grooves beyond the semicircular region, determination was made that deformation was present.
  • Coil heaters and cylindrical heater modules were produced in the same method as in Example 1 except that the interheater distance t with respect to each coil inner diameter D was set at each distance shown in Table 1 in the condition that the wire diameter of the heater wire material was still 3 mm and the coil inner diameter D of the coil heater was set at 300 mm, 600 mm and 900 mm in respective Examples as shown in Table 1.
  • the size of each ceramic mold an inner diameter and an outer diameter corresponding to the coil inner diameter were set but a height was set at 500 mm in all examples. Accordingly, the number of turns was set to be a number corresponding to the interheater distance t .
  • Grooves having a groove width of 6 mm and a depth of 10 mm were formed in the pair of semi-cylindrical ceramic molds in respective Examples as in Example 1, but those were formed at the intervals of a pitch (P) of 13 mm in case the interheater distance t was 10, a pitch (P) of 23 mm in case the interheater distance t was 20, a pitch (P) of 33 mm in case the interheater distance t was 30, a pitch (P) of 43 mm in case the interheater distance t was 40, a pitch (P) of 53 mm in case the interheater distance t was 50, a pitch (P) of 63 mm in case the interheater distance t was 60, a pitch (P) of 73 mm in case the interheater distance t was 70, a pitch (P) of 83 mm in case the interheater distance t was 80 or a pitch (P) of 93 mm in case the interhea
  • Example 1 the temperature distribution was measured and the life test was further performed in the same manner as in Example 1. Results thereof, inclusively of the result in Example 1, are shown in Table 1.
  • Table 1 the case where the temperature distribution is not larger than 3°C is evaluated as ⁇
  • the case where the temperature distribution is larger than 3°C but not larger than 5°C is evaluated as O
  • the case where the temperature distribution is larger than 5°C is evaluated as ⁇ .
  • the life test the aforementioned case where there is no deformation is evaluated as ⁇ , and the case where there is any deformation is evaluated as ⁇ .
  • Example 1 Inner Diameter D, mm Interheater Distance t, mm t/(D/2) 1/2 Temperature Distribution Accelerated Life Test Comprehensive Evaluation
  • 300 20 1.6 ⁇ ⁇ ⁇ Example 2 300 30 2.4 ⁇ ⁇ ⁇ Example 3 300 40 3.3 ⁇ ⁇ ⁇ Example 4 600 20 1.2 ⁇ ⁇ ⁇ Example 5 600 30 1.7 ⁇ ⁇ ⁇ Example 6 600 40 2.3 ⁇ ⁇ ⁇ Example 7 600 50 2.9 ⁇ ⁇ ⁇ Example 8 600 60 3.5 ⁇ ⁇ ⁇ Example 9 600 70 4 ⁇ ⁇ ⁇ Example 10 900 20 0.9 ⁇ ⁇ Example 11 900 30 1.4 ⁇ ⁇ ⁇ Example 12 900 40 1.9 ⁇ ⁇ ⁇ Example 13 900 50 2.4 ⁇ ⁇ ⁇ Example 14 900 60 2.8 ⁇ ⁇ ⁇ Example 15 900 70 3.3 ⁇ ⁇ ⁇ Example 16 900 80 3.8 ⁇ ⁇ ⁇ Comparative Example 1 300 10 0.8 ⁇ ⁇ ⁇ Comparative Example 2

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Resistance Heating (AREA)
EP13306161.4A 2012-08-23 2013-08-21 MoSi2-based coil heater and tubular heater module having the same Not-in-force EP2701458B1 (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2012184115A JP5508487B2 (ja) 2012-08-23 2012-08-23 管状ヒーターモジュール

Publications (2)

Publication Number Publication Date
EP2701458A1 EP2701458A1 (en) 2014-02-26
EP2701458B1 true EP2701458B1 (en) 2016-12-14

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ID=49084955

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EP13306161.4A Not-in-force EP2701458B1 (en) 2012-08-23 2013-08-21 MoSi2-based coil heater and tubular heater module having the same

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EP (1) EP2701458B1 (zh)
JP (1) JP5508487B2 (zh)
KR (1) KR101439051B1 (zh)
CN (1) CN103634953B (zh)

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3812324A (en) * 1971-07-08 1974-05-21 Itt Glow coil ignitor
KR100297282B1 (ko) * 1993-08-11 2001-10-24 마쓰바 구니유키 열처리장치 및 열처리방법
JPH08143365A (ja) 1994-11-15 1996-06-04 Riken Corp 二珪化モリブデンヒーター
SE522581C2 (sv) * 2002-02-27 2004-02-17 Sandvik Ab Element av molybdensilicidtyp
US8119954B2 (en) * 2003-01-07 2012-02-21 Micropyretics Heaters International, Inc. Convective heating system for industrial applications
JP2005100695A (ja) * 2003-09-22 2005-04-14 Ngk Insulators Ltd 基板加熱方法、抵抗発熱体付基板及びその製造方法
JP2005175366A (ja) * 2003-12-15 2005-06-30 Seiko Epson Corp ヒータおよびヒータ付き炉
KR101484341B1 (ko) * 2007-03-05 2015-01-19 산드빅 인터렉츄얼 프로퍼티 에이비 히터 요소 및 전기로용 인서트
EP2427412A4 (en) * 2009-05-05 2013-01-16 Sandvik Intellectual Property HEATING ELEMENT

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
None *

Also Published As

Publication number Publication date
KR101439051B1 (ko) 2014-09-05
KR20140026303A (ko) 2014-03-05
CN103634953B (zh) 2015-06-10
EP2701458A1 (en) 2014-02-26
JP5508487B2 (ja) 2014-05-28
CN103634953A (zh) 2014-03-12
JP2014041784A (ja) 2014-03-06

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