JP2000281444A - Cylindrical graphite material and its production - Google Patents

Cylindrical graphite material and its production

Info

Publication number
JP2000281444A
JP2000281444A JP11085430A JP8543099A JP2000281444A JP 2000281444 A JP2000281444 A JP 2000281444A JP 11085430 A JP11085430 A JP 11085430A JP 8543099 A JP8543099 A JP 8543099A JP 2000281444 A JP2000281444 A JP 2000281444A
Authority
JP
Japan
Prior art keywords
graphite material
cylindrical
packing
coke
furnace
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.)
Pending
Application number
JP11085430A
Other languages
Japanese (ja)
Inventor
Masahiro Yasuda
正弘 安田
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.)
Ibiden Co Ltd
Original Assignee
Ibiden 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 Ibiden Co Ltd filed Critical Ibiden Co Ltd
Priority to JP11085430A priority Critical patent/JP2000281444A/en
Publication of JP2000281444A publication Critical patent/JP2000281444A/en
Pending legal-status Critical Current

Links

Abstract

PROBLEM TO BE SOLVED: To obtain a cylindrical graphite material having a large diameter and having reduced variations in properties between various parts by placing carbonaceous members between ungraphitized materials to make the thickness of a packing coke layer uniform in a graphitization process of cylindrical materials in an Acheson-type furnace. SOLUTION: This method is suitable for obtaining a cylindrical graphite material having a diameter of >=500 mm, an unevenness in resistivity of <=5% and an unevenness in thermal expansion coefficient of <=5% in a plane perpendicular to the axis. The graphitization is carried out by placing a fired article to be graphitized in an Acheson- type rectangular furnace made of refractory bricks using coke grains as a packing material, followed by directly energizing them in the direction of furnace length to perform graphitization by resistance heating. By placing carbonaceous members 4 together with packing coke 2 between cylindrical materials 1 to be graphitized and by energizing electrodes 3, an electric current uniformly flows through the layer of packing coke 2 and a graphite material having uniform characteristics is obtained. The graphite material shows excellent soaking property in a single crystal puller and a heater because the resistivity is uniform over the entire length and in all directions. homogeneous.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、半導体製造装置用
黒鉛部材、原子炉用黒鉛部材、HIP用黒鉛部材として
使用される大きな直径を有する円柱状黒鉛部材及びその
製造方法に関する。
The present invention relates to a graphite member having a large diameter used as a graphite member for a semiconductor manufacturing apparatus, a graphite member for a nuclear reactor, a graphite member for a HIP, and a method for manufacturing the same.

【0002】[0002]

【従来技術】従来より黒鉛の製造方法は石油コークス等
のフィラーと、ピッチ等のバインダーとを混合し、これ
を所定の形状に成形して得た成型品を焼成後、溶融ピッ
チ等の含浸剤を含浸、更に、熱処理を施して黒鉛化する
ことよりなる。そして、黒鉛化に際してはアチェソン炉
が使用されている。アチェソン炉は耐火レンガ製の長方
形の炉で円柱状の焼成した黒鉛原料を直立状に並べ、そ
の間隙にコークス粒をパッキング材として炉詰めし、こ
れに炉長方向に直接通電し抵抗加熱することによって製
造している。この状態の平面図を図2に示す。図2にお
いて、1は円柱状黒鉛素材、2はパッキングコークス、
3は電極である。しかして、最近大型の半導体ウェハー
の製造を始めとして、大型の円柱形状の黒鉛材の需要が
高まっている。大型の円柱形状の黒鉛材の製造方法につ
いても一般に上述の黒鉛材の製造方法と変わるところが
ないが、直径の大きい黒鉛原料をアチェソン炉によっ
て、黒鉛化すると、均一な製品が得にくいという欠点が
あった。即ち、図2に示したような状態で通電すると、
パッキングコークス層の薄い部位では抵抗は小さく、ま
たパッキング層の厚い部位では抵抗は大きくなるため電
流は一様に流れず、電流の流れやすい部位では黒鉛化度
は高く、電流の流れにくい部位では黒鉛化度は低く、そ
の為均質な黒鉛製品は得られなかったのである。従来の
製品として直径が500mm以上の黒鉛では、その製品
の部位により熱膨張係数をはじめとして、その特性が1
0%以上のバラツキが生じ、直径の大きい製品になるに
したがって、そのバラツキは大きくなった。
2. Description of the Related Art Conventionally, graphite has been produced by mixing a filler such as petroleum coke and a binder such as pitch, forming the mixture into a predetermined shape, firing the molded product, and then impregnating an impregnating agent such as a molten pitch. And then heat-treated to graphitize. An Acheson furnace is used for graphitization. The Acheson furnace is a rectangular furnace made of refractory bricks, arranging cylindrical fired graphite raw materials in an upright position, filling the gap with coke particles as a packing material, and directing electricity to the furnace length direction to conduct resistance heating. It is manufactured by. FIG. 2 shows a plan view of this state. In FIG. 2, 1 is a columnar graphite material, 2 is packing coke,
3 is an electrode. Recently, there has been an increasing demand for large columnar graphite materials, including the production of large semiconductor wafers. Although the method for producing a large columnar graphite material is generally the same as the above-described method for producing a graphite material, there is a disadvantage in that if a graphite material having a large diameter is graphitized in an Acheson furnace, it is difficult to obtain a uniform product. Was. That is, when electricity is supplied in the state shown in FIG.
The resistance is small in the thin part of the packing coke layer, and the resistance is large in the thick part of the packing layer, so the current does not flow uniformly.The graphitization degree is high in the part where the current flows easily, and the graphite is in the part where the current does not easily flow. The degree of conversion was low, and a homogeneous graphite product could not be obtained. In the case of graphite having a diameter of 500 mm or more as a conventional product, its characteristics, such as the coefficient of thermal expansion, depend on the part of the product.
A variation of 0% or more occurred, and the variation became larger as the product became larger in diameter.

【0003】[0003]

【発明が解決しようとする課題】本発明者は上記の問題
を解決すべく種々検討した結果、本発明を完成したもの
で、本発明の目的は直径の大きな円柱状黒鉛の製造方法
において、各部位における特性にバラツキの少ない黒鉛
材を製造する方法及びバラツキの少ない黒鉛材を提供す
ることである。
The present inventors have conducted various studies to solve the above problems, and as a result, have completed the present invention. An object of the present invention is to provide a method for producing a columnar graphite having a large diameter. It is an object of the present invention to provide a method for producing a graphite material having less variation in properties at a site and a graphite material having less variation.

【0004】[0004]

【課題を解決するための手段】本願の請求項1の発明の
要旨はアチェソン炉により円柱状素材を黒鉛化する工程
において、素材間に炭素質部材を設置し、パッキングコ
ークス層の厚さを略均一にすることを特徴とする黒鉛材
の製造方法あり、請求項2の発明の要旨は請求項1記載
の方法によって得られた直径500mm以上の円柱状黒
鉛材であって、軸に垂直な面内の比抵抗、熱膨張係数の
バラツキが5%以内であることを特徴とする円柱状黒鉛
材である。即ち、本発明は黒鉛素材間に炭素質部材を設
置してあるので各素材間の間隔はほぼ均一になり、その
結果、パッキングコークス層内を電流が均一に流れるの
で、均一な黒鉛材が得られるのである。
The gist of the invention of claim 1 of the present application is that in the step of graphitizing a cylindrical material by an Acheson furnace, a carbonaceous member is provided between the materials and the thickness of the packing coke layer is reduced. There is provided a method for producing a graphite material characterized by being uniform. The gist of the invention of claim 2 is a columnar graphite material having a diameter of 500 mm or more obtained by the method of claim 1, wherein the surface is perpendicular to the axis. A variation of the specific resistance and the coefficient of thermal expansion within 5%. That is, in the present invention, since the carbonaceous members are provided between the graphite materials, the intervals between the materials become substantially uniform, and as a result, the current flows uniformly in the packing coke layer, so that a uniform graphite material is obtained. It is done.

【0005】[0005]

【発明の実施の形態】以下、本発明について詳細に述べ
る。本発明で使用するアチェソン炉とは通常黒鉛化に使
用する黒鉛化炉であって、耐火レンガ製の長方形の炉で
あり、その大きさは長さ15m、巾2m、高さ2m程度
ある。そして、この炉の内に黒鉛材料である焼成品をコ
ークス粒をパッキング材として炉詰めし、これに炉長方
向に直接通電して抵抗加熱して黒鉛化を行うのである。
しかして、本発明は黒鉛素材間にパッキングコークスと
共に炭素質部材を設置して黒鉛素材の各部位における通
電を均一にするのである。ここで使用する炭素質部材と
しては黒鉛等の電気比抵抗がパッキングコークスの比抵
抗より小さいものが好ましく、その形状として四角柱や
円柱等であるが、特にこれらに限定されるものではな
い。そして、本発明においては炭素質部材と原料との間
隔の大きさは20cm±10cm程度とする。本発明に
おけるアチェソン炉に炭素質部材及び黒鉛化原料を設置
した状態の平面図を図1に示す。図1において、1は円
柱状黒鉛素材、2はパッキングコークス、3は電極、4
は炭素部材である。このような状態のもとに通電すると
電流は黒鉛材料中を均一に流れ、その結果、得られた黒
鉛材の各特性は均一である。
BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail. The Acheson furnace used in the present invention is a graphitization furnace usually used for graphitization, and is a rectangular furnace made of refractory brick, and its size is about 15 m in length, 2 m in width and 2 m in height. Then, in the furnace, a fired product, which is a graphite material, is packed in a furnace using coke particles as a packing material, and electricity is directly supplied to the furnace in the furnace length direction to perform resistance heating to graphitize.
Thus, in the present invention, the carbonaceous member is provided between the graphite materials together with the packing coke, and the energization in each part of the graphite material is made uniform. The carbonaceous member used herein is preferably one having a specific electrical resistance of graphite or the like smaller than that of the packing coke, and the shape thereof is, for example, a square pole or a cylinder, but is not particularly limited thereto. And, in the present invention, the size of the interval between the carbonaceous member and the raw material is about 20 cm ± 10 cm. FIG. 1 is a plan view showing a state in which a carbonaceous member and a graphitizing raw material are installed in the Acheson furnace in the present invention. In FIG. 1, 1 is a columnar graphite material, 2 is a packing coke, 3 is an electrode,
Is a carbon member. When a current is applied in such a state, the current flows uniformly in the graphite material, and as a result, each characteristic of the obtained graphite material is uniform.

【0006】[0006]

【発明の効果】請求項1の発明によれば、約1500℃
に加熱して使用される単結晶引き上げ装置やヒーターに
おいて、比抵抗が均質であるため、優れた均熱性を示
し、単結晶の品質に多大な効果をもたらす。また、熱膨
張係数が均一であるため、加熱に伴う素材内歪みが発生
しにくく、優れた耐熱衝撃性を示すことから、単結晶引
き上げ装置用部材等、高温で使用される黒鉛部材に有効
である。
According to the first aspect of the present invention, about 1500 ° C.
In a single crystal pulling apparatus and a heater which are used after being heated to a high temperature, since the specific resistance is uniform, it exhibits excellent heat uniformity and has a great effect on the quality of the single crystal. In addition, since the thermal expansion coefficient is uniform, distortion in the material due to heating is unlikely to occur, and since it exhibits excellent thermal shock resistance, it is effective for graphite members used at high temperatures, such as members for single crystal pulling equipment. is there.

【0007】[0007]

【実施例】コークス粉砕物とバインダーピッチの混練物
を再度粉砕し、冷間静水圧成形(CIP成形)にて円柱
形状に成形し、還元雰囲気にて1000℃にて焼成した
素材(1次品)を図 のような2m×2m×15mのア
チェソン炉に詰め、約2500Wにて通電し、2500
℃で加熱した。 データ 比抵抗:1次品 5×10~3 Ωcm パッキングコークス 0.2 Ωcm 炭素質部材 1.5×10~3Ωcm 電極 0.6×10~3Ωcm
EXAMPLE A kneaded material of coke pulverized material and binder pitch was pulverized again, formed into a cylindrical shape by cold isostatic pressing (CIP molding), and fired at 1000 ° C. in a reducing atmosphere (primary product). ) Is packed in a 2m × 2m × 15m Acheson furnace as shown in the figure,
Heated at ° C. Data Resistivity: primary product 5 × 10 ~ 3 Ωcm packing coke 0.2 [Omega] cm carbonaceous member 1.5 × 10 ~ 3 Ωcm electrode 0.6 × 10 ~ 3 Ωcm

【0008】[0008]

【表1】 [Table 1]

【図面の簡単な説明】[Brief description of the drawings]

【図1】本発明製造方法におけるアチェソン炉内の黒鉛
素材の配列図。
FIG. 1 is an arrangement diagram of a graphite material in an Acheson furnace in the production method of the present invention.

【図2】従来方法におけるアチェソン炉内の黒鉛素材の
配列図。
FIG. 2 is an arrangement diagram of a graphite material in an Acheson furnace according to a conventional method.

【符号の説明】[Explanation of symbols]

1 円柱状黒鉛素材 2 パッキングコークス 3 電極 4 炭素部材 1 Columnar graphite material 2 Packing coke 3 Electrode 4 Carbon member

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】 アチェソン炉により円柱状素材を黒鉛化
する工程において、素材間に炭素質部材を設置し、パッ
キングコークス層の厚さを略均一にすることを特徴とす
る黒鉛材の製造方法。
1. A method for producing a graphite material, comprising: in a step of graphitizing a cylindrical material in an Acheson furnace, placing a carbonaceous member between the materials and making the thickness of a packing coke layer substantially uniform.
【請求項2】 請求項1記載の方法によって得られた直
径500mm以上の円柱状黒鉛材であって、軸に垂直な
面内の比抵抗、熱膨張係数のバラツキが5%以内である
ことを特徴とする円柱状黒鉛材。
2. A cylindrical graphite material having a diameter of 500 mm or more obtained by the method according to claim 1, wherein a variation in specific resistance and coefficient of thermal expansion in a plane perpendicular to the axis is within 5%. Characteristic columnar graphite material.
JP11085430A 1999-03-29 1999-03-29 Cylindrical graphite material and its production Pending JP2000281444A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP11085430A JP2000281444A (en) 1999-03-29 1999-03-29 Cylindrical graphite material and its production

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP11085430A JP2000281444A (en) 1999-03-29 1999-03-29 Cylindrical graphite material and its production

Publications (1)

Publication Number Publication Date
JP2000281444A true JP2000281444A (en) 2000-10-10

Family

ID=13858635

Family Applications (1)

Application Number Title Priority Date Filing Date
JP11085430A Pending JP2000281444A (en) 1999-03-29 1999-03-29 Cylindrical graphite material and its production

Country Status (1)

Country Link
JP (1) JP2000281444A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010049428A2 (en) * 2008-10-27 2010-05-06 Timcal S.A. Process for the production and treatment of graphite powders
CN108341669A (en) * 2018-03-29 2018-07-31 中钢集团新型材料(浙江)有限公司 High temperature gas cooled reactor in-pile component big specification nuclear graphite materials and preparation method
CN109081695A (en) * 2018-07-24 2018-12-25 中钢集团新型材料(浙江)有限公司 The preparation method of the molten salt reactor ultra-fine aperture nuclear graphite materials of high density large scale
JP2020147473A (en) * 2019-03-15 2020-09-17 イビデン株式会社 Manufacture support method of graphite material

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010049428A2 (en) * 2008-10-27 2010-05-06 Timcal S.A. Process for the production and treatment of graphite powders
WO2010049428A3 (en) * 2008-10-27 2010-12-29 Timcal S.A. Process for the production and treatment of graphite powders
US9102539B2 (en) 2008-10-27 2015-08-11 Imerys Graphite & Carbon Switzerland Sa Process for the production and treatment of graphite powders
CN108341669A (en) * 2018-03-29 2018-07-31 中钢集团新型材料(浙江)有限公司 High temperature gas cooled reactor in-pile component big specification nuclear graphite materials and preparation method
CN108341669B (en) * 2018-03-29 2020-12-04 中钢集团新型材料(浙江)有限公司 Large-size nuclear graphite material for high-temperature gas cooled reactor internals and preparation method thereof
CN109081695A (en) * 2018-07-24 2018-12-25 中钢集团新型材料(浙江)有限公司 The preparation method of the molten salt reactor ultra-fine aperture nuclear graphite materials of high density large scale
JP2020147473A (en) * 2019-03-15 2020-09-17 イビデン株式会社 Manufacture support method of graphite material
JP7191742B2 (en) 2019-03-15 2022-12-19 イビデン株式会社 Graphite material manufacturing support method

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