JP2011123185A - Silicon material for infrared transmitting members, and infrared transmitting member - Google Patents

Silicon material for infrared transmitting members, and infrared transmitting member Download PDF

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JP2011123185A
JP2011123185A JP2009279522A JP2009279522A JP2011123185A JP 2011123185 A JP2011123185 A JP 2011123185A JP 2009279522 A JP2009279522 A JP 2009279522A JP 2009279522 A JP2009279522 A JP 2009279522A JP 2011123185 A JP2011123185 A JP 2011123185A
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infrared transmitting
silicon
transmitting member
infrared
polycrystalline silicon
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JP5437039B2 (en
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Koji Tsuzukibashi
浩司 続橋
Hiroshi Ikeda
洋 池田
Masahiro Kanai
昌弘 金井
Saburo Wakita
三郎 脇田
Tetsuya Tojo
哲也 東条
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Mitsubishi Materials Corp
Mitsubishi Materials Electronic Chemicals Co Ltd
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Mitsubishi Materials Electronic Chemicals Co Ltd
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    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/02Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of crystals, e.g. rock-salt, semi-conductors
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    • C01B33/00Silicon; Compounds thereof
    • C01B33/02Silicon
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/02Silicon
    • C01B33/037Purification
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B28/00Production of homogeneous polycrystalline material with defined structure
    • C30B28/04Production of homogeneous polycrystalline material with defined structure from liquids
    • C30B28/06Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/06Silicon
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B13/00Optical objectives specially designed for the purposes specified below
    • G02B13/14Optical objectives specially designed for the purposes specified below for use with infrared or ultraviolet radiation

Abstract

<P>PROBLEM TO BE SOLVED: To provide a silicon material for an infrared transmitting member which secures transmittance for infrared of around 9 μm wavelength and can be used for wide range of wavelength, and to provide an infrared transmitting member made of the silicon material. <P>SOLUTION: A silicon material for an infrared transmitting member used for a material of infrared transmitting members such as an infrared transmitting lens, prism, or the like, includes a polycrystalline silicon. The resistivity of the polycrystalline silicon is 1 Ωcm or more and the oxygen concentration is less than 1.0×10<SP>18</SP>atoms/cc. <P>COPYRIGHT: (C)2011,JPO&INPIT

Description

本発明は、赤外線レーザ装置等において、赤外線を透過するレンズ部材やプリズム部材等の赤外線透過部材の素材として使用される赤外線透過部材用シリコン材料及びこの赤外線透過部材用シリコン材料からなる赤外線透過部材に関するものである。   The present invention relates to a silicon material for an infrared transmitting member used as a material for an infrared transmitting member such as a lens member or a prism member that transmits infrared in an infrared laser device and the like, and an infrared transmitting member made of the silicon material for the infrared transmitting member. Is.

赤外線レーザ装置等において、赤外線レーザ光を透過するレンズ部材やプリズム部材等の赤外線透過部材は、例えば特許文献1に示すように、ゲルマニウム、シリコン等の半導体結晶材料を用いたものが提供されている。また、フッ化カルシウム(CaF2)やジンクセレン(ZnSe)といった化合物結晶材料も使用されている。これらの材料は、その屈折率や透過率等を考慮して、用途に併せて適宜選択して使用されることになる。   In an infrared laser device or the like, an infrared transmitting member such as a lens member or a prism member that transmits infrared laser light is provided using a semiconductor crystal material such as germanium or silicon as shown in Patent Document 1, for example. . In addition, compound crystal materials such as calcium fluoride (CaF2) and zinc selenium (ZnSe) are also used. These materials are appropriately selected and used according to the application in consideration of the refractive index and transmittance.

ここで、ゲルマニウムは、波長2〜20μmの赤外線を透過し、屈折率が約4程度と比較的大きく、波長による屈折率の変化が少ないといった特性を有する材料であり、レンズ部材として適している。
しかしながら、ゲルマニウムは、埋蔵量も少なく比較的高価な材料であるため、レンズ部材やプリズム部材等の赤外線透過部材として広く使用することができないといった問題があった。また、温度が100℃程度を超えると透過率が低下することが知られており、温度が上昇する環境下では使用できなかった。
Here, germanium is a material that transmits infrared rays having a wavelength of 2 to 20 μm, has a relatively large refractive index of about 4 and has a small change in refractive index depending on the wavelength, and is suitable as a lens member.
However, germanium has a problem that it cannot be widely used as an infrared transmitting member such as a lens member or a prism member because it is a relatively expensive material with a small reserve. Further, it is known that the transmittance decreases when the temperature exceeds about 100 ° C., and cannot be used in an environment where the temperature increases.

これに対して、シリコンは、太陽電池や半導体基板として広く使用されており、ゲルマニウムに比べて安価に入手することができる材料である。また、前述のゲルマニウムと同様に、屈折率が3.5程度と比較的大きく、波長による屈折率の変化が少ないため、レンズ部材を構成するのに適している。   On the other hand, silicon is widely used as a solar cell or a semiconductor substrate, and is a material that can be obtained at a lower cost than germanium. Further, similar to the above-described germanium, the refractive index is relatively large as about 3.5 and the change in the refractive index due to the wavelength is small, so that it is suitable for constituting a lens member.

特開2001−141993号公報JP 2001-141993 A

ところで、前述のシリコンにおいては、波長1.2〜6μmの赤外線に対しては透過率が高いものの、波長9μm程度において大きな吸収ピークを有することが知られている。このため、シリコンは、波長1.2〜6μmといった狭い波長領域の赤外線に対する赤外線透過部材の素材としてのみ使用されていた。   By the way, it is known that the above-mentioned silicon has a large absorption peak at a wavelength of about 9 μm, although it has a high transmittance for infrared rays having a wavelength of 1.2 to 6 μm. For this reason, silicon has been used only as a material for an infrared transmitting member for infrared rays having a narrow wavelength range of 1.2 to 6 μm.

なお、特許文献1には、レンズ部材の肉厚を薄くすることによって波長8〜12μmの赤外線の吸収を抑制することが開示されているが、やはり、波長9μm前後の赤外線については大部分が吸収されてしまうことになる。また、レンズ部材の形状も、フレネルレンズ等に限定されることになる。よって、波長8〜12μmの赤外線の赤外線透過部材としてシリコンを広く使用することはできない。   Patent Document 1 discloses that the absorption of infrared rays having a wavelength of 8 to 12 μm is suppressed by reducing the thickness of the lens member. However, most of infrared rays having a wavelength of around 9 μm are absorbed. It will be done. Further, the shape of the lens member is also limited to a Fresnel lens or the like. Therefore, silicon cannot be widely used as an infrared ray transmitting member for infrared rays having a wavelength of 8 to 12 μm.

また、赤外線透過部材の素材として使用されるシリコンとしては、いわゆる単結晶シリコンが用いられている。これは、透過する赤外線が結晶粒界において散乱することを防止するためである。しかしながら、この単結晶シリコンの製造には、多くの労力と時間が必要となるため、生産効率が悪く、製造コストも増加することになる。さらに、製出される単結晶シリコンの大きさに制限があるため、大口径のレンズ部材等を製出することができないといった問題があった。   As silicon used as a material for the infrared transmitting member, so-called single crystal silicon is used. This is to prevent the transmitted infrared rays from being scattered at the crystal grain boundaries. However, since the production of this single crystal silicon requires a lot of labor and time, the production efficiency is poor and the production cost increases. Furthermore, since the size of single crystal silicon to be produced is limited, there is a problem that a large-diameter lens member or the like cannot be produced.

本発明は、上述した状況に鑑みてなされたものであって、波長9μm前後(8〜12μm)の赤外線に対しても透過率が確保でき、広範囲な波長領域で使用可能な赤外線透過部材の素材として使用される赤外線透過部材用シリコン材料、及び、この赤外線透過部材用シリコン材料からなる赤外線透過部材を提供することを目的とする。   The present invention has been made in view of the above-described circumstances, and can provide a transmittance for infrared rays having a wavelength of about 9 μm (8 to 12 μm), and can be used in a wide wavelength range. It is an object to provide a silicon material for an infrared transmitting member used as an infrared transmitting member and an infrared transmitting member made of the silicon material for an infrared transmitting member.

上記課題を解決するために、本発明に係る赤外線透過部材用シリコン材料は、赤外線を透過するレンズやプリズム等の赤外線透過部材の素材として使用される赤外線透過部材用シリコン材料であって、多結晶シリコンからなり、この多結晶シリコンの抵抗率が1Ωcm以上、かつ、酸素濃度が1.0×1018atoms/cc未満とされていることを特徴としている。 In order to solve the above-described problems, the silicon material for an infrared transmitting member according to the present invention is a silicon material for an infrared transmitting member used as a material for an infrared transmitting member such as a lens or prism that transmits infrared rays, and is polycrystalline. The polycrystalline silicon is characterized by having a resistivity of 1 Ωcm or more and an oxygen concentration of less than 1.0 × 10 18 atoms / cc.

この構成の赤外線透過部材用シリコン材料は、抵抗率が1Ωcm以上、かつ、酸素濃度が1.0×1018atoms/cc未満とされている。ここで、波長9μm前後(8〜12μm)の赤外線の吸収については、シリコン結晶内に含有される酸素に起因するものである。よって、酸素濃度を1.0×1018atoms/cc未満とすることにより、波長9μm前後(8〜12μm)の赤外線の吸収を抑えることが可能となり、広範囲な波長領域で使用可能な赤外線透過部材の素材として使用できることになる。なお、酸素濃度は、5.0×1017atoms/cc未満とすることが好ましく、さらに1.0×1016atoms/cc未満とすることが好ましい。 The silicon material for an infrared transmitting member having this configuration has a resistivity of 1 Ωcm or more and an oxygen concentration of less than 1.0 × 10 18 atoms / cc. Here, the absorption of infrared rays having a wavelength of around 9 μm (8 to 12 μm) is caused by oxygen contained in the silicon crystal. Therefore, by setting the oxygen concentration to less than 1.0 × 10 18 atoms / cc, it is possible to suppress absorption of infrared rays having a wavelength of about 9 μm (8 to 12 μm), and an infrared transmitting member usable in a wide wavelength range. It can be used as a material. Note that the oxygen concentration is preferably less than 5.0 × 10 17 atoms / cc, and more preferably less than 1.0 × 10 16 atoms / cc.

また、前述の波長9μm前後(8〜12μm)の赤外線の吸収については、抵抗率と相関関係があることが知られている、すなわち、抵抗率が大きくなると、赤外線の吸収係数が低くなるのである。よって、多結晶シリコンの抵抗率を1Ωcm以上に規定することにより、波長9μm前後(8〜12μm)の赤外線の吸収を確実に抑制することができるのである。   Further, it is known that the absorption of infrared rays having a wavelength of about 9 μm (8 to 12 μm) has a correlation with the resistivity, that is, when the resistivity increases, the absorption coefficient of the infrared rays decreases. . Therefore, by limiting the resistivity of polycrystalline silicon to 1 Ωcm or more, it is possible to reliably suppress the absorption of infrared rays having a wavelength of around 9 μm (8 to 12 μm).

さらに、多結晶シリコンで構成されているので、単結晶シリコンよりも酸素濃度を比較的容易に低減することができ、前述のように赤外線の吸収を抑制することが可能となる。なお、この赤外線透過部材用シリコン材料においては、内部に結晶粒界が存在することになるが、出力の比較的低い赤外線レーザであれば、結晶粒界における散乱による影響を特に考慮する必要はない。   Furthermore, since it is made of polycrystalline silicon, the oxygen concentration can be reduced relatively easily as compared with single crystal silicon, and infrared absorption can be suppressed as described above. In this silicon material for an infrared transmitting member, there are crystal grain boundaries inside. However, if the infrared laser has a relatively low output, it is not necessary to consider the influence of scattering at the crystal grain boundaries. .

ここで、前記多結晶シリコンの平均結晶粒径が、3mm以上20mm以下とされていることが好ましい。
この場合、多結晶シリコンの平均結晶粒径が3mm以上とされているので、この赤外線透過部材用シリコン材料を用いて赤外線透過部材を成形した際に、赤外線透過部材内部に存在する結晶粒界の数が少なくなり、赤外線の散乱を抑制することができる。よって、赤外線レーザが高出力の場合であっても、この赤外線透過部材用シリコン材料を用いることが可能となる。
また、多結晶シリコンの平均結晶粒径が20mm以下とされているので、比較的容易にこの多結晶シリコンを製出することができる。
Here, it is preferable that the average crystal grain size of the polycrystalline silicon is 3 mm or more and 20 mm or less.
In this case, since the average crystal grain size of polycrystalline silicon is 3 mm or more, when an infrared transmitting member is formed using this silicon material for infrared transmitting member, the grain boundary existing inside the infrared transmitting member The number is reduced, and scattering of infrared rays can be suppressed. Therefore, even when the infrared laser has a high output, it is possible to use the silicon material for the infrared transmitting member.
Further, since the average crystal grain size of polycrystalline silicon is 20 mm or less, this polycrystalline silicon can be produced relatively easily.

さらに、前記多結晶シリコンが、一方向凝固法によって製出されたものであることが好ましい。
この場合、一方向凝固法によって多結晶シリコンを製出しているので、固液界面において、固体側から液体側へと不純物が排出されることになり、純度の高い多結晶シリコンを得ることができる。よって、赤外線透過部材用シリコン材料中の酸素濃度を確実に低減させることができ、赤外線の吸収を抑えることができる。また、一方向凝固であることから、凝固方向に向くように柱状晶が成長することになり、結晶粒径を比較的大きくすることが可能となる。
Furthermore, it is preferable that the polycrystalline silicon is produced by a unidirectional solidification method.
In this case, since polycrystalline silicon is produced by the unidirectional solidification method, impurities are discharged from the solid side to the liquid side at the solid-liquid interface, and high-purity polycrystalline silicon can be obtained. . Therefore, the oxygen concentration in the silicon material for an infrared transmitting member can be reliably reduced, and infrared absorption can be suppressed. In addition, since it is unidirectionally solidified, columnar crystals grow in the direction of solidification, and the crystal grain size can be made relatively large.

また、前記多結晶シリコンに、B又はAlがドーピングされていてもよい。
この場合、シリコンにB又はAlがドーピングすることで抵抗率を調整することが可能となり、多結晶シリコンの抵抗率を確実に1Ωcm以上とすることができる。
The polycrystalline silicon may be doped with B or Al.
In this case, the resistivity can be adjusted by doping silicon with B or Al, and the resistivity of the polycrystalline silicon can be reliably set to 1 Ωcm or more.

本発明に係る赤外線透過部材は、前述の赤外線透過部材用シリコン材料を用いて製造されたことを特徴としている。
この構成の赤外線透過部材においては、抵抗率が1Ωcm以上、かつ、酸素濃度が1.0×1018atoms/cc未満とされた多結晶シリコンによって構成されているので、波長9μm前後の赤外線の吸収を抑えることが可能となり、広範囲な波長の赤外線を透過可能となる。
The infrared transmitting member according to the present invention is manufactured using the aforementioned silicon material for infrared transmitting member.
Since the infrared transmitting member having this configuration is made of polycrystalline silicon having a resistivity of 1 Ωcm or more and an oxygen concentration of less than 1.0 × 10 18 atoms / cc, it absorbs infrared rays having a wavelength of about 9 μm. Can be suppressed, and infrared rays having a wide range of wavelengths can be transmitted.

このように、本発明によれば、波長9μm前後(8〜12μm)の赤外線に対しても透過率が確保でき、広範囲な波長領域で使用可能な赤外線透過部材の素材として使用される赤外線透過部材用シリコン材料、及び、この赤外線透過部材用シリコン材料からなる赤外線透過部材を提供することができる。   As described above, according to the present invention, the infrared transmission member can be used as a material for an infrared transmission member that can secure a transmittance even for infrared rays having a wavelength of around 9 μm (8 to 12 μm) and can be used in a wide wavelength range. It is possible to provide an infrared transmitting member made of the silicon material and the silicon material for the infrared transmitting member.

本発明の実施形態である赤外線透過部材用シリコン材料からなるレンズ部材の概略説明図である。It is a schematic explanatory drawing of the lens member which consists of a silicon material for infrared rays transmissive members which is an embodiment of the present invention. 多結晶シリコンの平均結晶粒径の測定方法を示す説明図である。It is explanatory drawing which shows the measuring method of the average crystal grain diameter of a polycrystalline silicon. 本発明の実施形態である赤外線透過部材用シリコン材料である多結晶シリコンの製造装置の概略説明図である。It is a schematic explanatory drawing of the manufacturing apparatus of the polycrystalline silicon which is the silicon material for infrared rays transmissive members which is embodiment of this invention.

以下に、本発明の実施形態である赤外線透過部材用シリコン材料、及び、この赤外線透過部材用シリコン材料からなるレンズ部材(赤外線透過部材)について添付した図面を参照にして説明する。
本実施形態である赤外線透過部材用シリコン材料は、図1に示すように、赤外線を透過して集光するレンズ部材10として使用されるものである。このようなレンズ部材10においては、赤外線の透過率が良好であること、及び、屈折率が大きく、かつ、波長に対して安定していることが重要な特性となる。
Hereinafter, a silicon material for an infrared transmitting member according to an embodiment of the present invention and a lens member (infrared transmitting member) made of the silicon material for an infrared transmitting member will be described with reference to the accompanying drawings.
As shown in FIG. 1, the silicon material for an infrared transmitting member according to this embodiment is used as a lens member 10 that transmits infrared rays and collects them. In such a lens member 10, it is important that the infrared transmittance is good, the refractive index is large, and the wavelength member is stable with respect to the wavelength.

また、本実施形態である赤外線透過部材用シリコン材料は、一方向凝固法によって形成された多結晶シリコンで構成されている。すなわち、複数の柱状晶が下部から上方に向けて延びた構造とされているのである。   In addition, the silicon material for an infrared transmitting member according to the present embodiment is composed of polycrystalline silicon formed by a unidirectional solidification method. That is, it has a structure in which a plurality of columnar crystals extend upward from the lower part.

この多結晶シリコンの抵抗率が1Ωcm以上とされている。ここで、多結晶シリコンの抵抗率の測定は、4探針法(JIS H 0602:シリコン単結晶及びシリコンウェーハの4探針法による抵抗率測定方法)によって測定した。   The resistivity of this polycrystalline silicon is set to 1 Ωcm or more. Here, the resistivity of the polycrystalline silicon was measured by a four-probe method (JIS H 0602: a resistivity measurement method by a four-probe method of a silicon single crystal and a silicon wafer).

また、酸素濃度が1.0×1018atoms/cc未満とされている。この酸素濃度の測定は、FT−IR法(JEIDA−61:赤外吸収によるシリコン中の格子間酸素原子濃度の標準測定、JEITA EM−3503(旧JEIDA―56):赤外吸収によるシリコン結晶中の置換型炭素原子濃度の標準測定)によって測定した。
なお、酸素濃度は、5.0×1017atoms/cc未満とすることが好ましく、さらに1.0×1016atoms/cc未満とすることが好ましい。
The oxygen concentration is less than 1.0 × 10 18 atoms / cc. This oxygen concentration is measured by the FT-IR method (JEIDA-61: standard measurement of interstitial oxygen atom concentration in silicon by infrared absorption, JEITA EM-3503 (former JEIDA-56): in silicon crystal by infrared absorption. (Standard measurement of substitutional carbon atom concentration).
Note that the oxygen concentration is preferably less than 5.0 × 10 17 atoms / cc, and more preferably less than 1.0 × 10 16 atoms / cc.

さらに、この多結晶シリコンの平均結晶粒径は、3mm以上20mm以下に設定されている。ここで、結晶粒径の測定は、以下に示すような方法で実施する。
図2に示すように、多結晶シリコンインゴット1の高さ方向(一方向凝固方向)で下側部分、中央部分、上側部分をスライスして測定試料2,3,4を採取する。これら各測定試料の表面組織を観察し、基準直線Sに対して交差する結晶粒界6の数をカウントする。この基準直線Sに交差する結晶粒界6の数で当該基準直線Sの長さを除することで、各測定試料の平均結晶粒径を求める。そして、これら各測定試料の測定結果から、多結晶シリコンインゴット1の平均結晶粒径を算出する。
なお、本実施形態では、多結晶シリコンインゴット1の大きさが、680mm×680mmの正方形断面をなし、高さ(一方向凝固方向の長さ)が300mmとされており、底面から10mm部分、150mm部分、290mm部分から測定試料2,3,4を採取した。そして、680mm×680mmの測定試料表面に、その一辺に平行に680mmの基準直線Sを設けて、平均結晶粒径を測定した。
Furthermore, the average crystal grain size of this polycrystalline silicon is set to 3 mm or more and 20 mm or less. Here, the crystal grain size is measured by the following method.
As shown in FIG. 2, measurement samples 2, 3, and 4 are obtained by slicing the lower portion, the center portion, and the upper portion in the height direction (one-direction solidification direction) of the polycrystalline silicon ingot 1. The surface texture of each measurement sample is observed, and the number of crystal grain boundaries 6 intersecting the reference straight line S is counted. By dividing the length of the reference line S by the number of crystal grain boundaries 6 intersecting the reference line S, the average crystal grain size of each measurement sample is obtained. Then, the average crystal grain size of the polycrystalline silicon ingot 1 is calculated from the measurement results of these measurement samples.
In the present embodiment, the size of the polycrystalline silicon ingot 1 is a square section of 680 mm × 680 mm, the height (the length in the unidirectional solidification direction) is 300 mm, the 10 mm portion from the bottom, 150 mm Samples 2, 3, and 4 were collected from the 290 mm portion. Then, a standard straight line S of 680 mm was provided on the surface of the measurement sample of 680 mm × 680 mm in parallel with one side, and the average crystal grain size was measured.

次に、本実施形態である赤外線透過部材用シリコン材料を構成する多結晶シリコンインゴットの製造方法について説明する。この多結晶シリコンは、図3に示す多結晶シリコン製造装置20を用いて製造されることになる。
この多結晶シリコン製造装置20は、シリコン融液Lが貯留されるルツボ21と、このルツボ22が載置されるチルプレート22と、このチルプレート22を下方から支持する床下ヒータ23と、ルツボ21の上方に配設された天井ヒータ24と、を備えている。また、ルツボ21の周囲には、断熱材25が設けられている。
Next, the manufacturing method of the polycrystalline silicon ingot which comprises the silicon | silicone material for infrared rays transparent members which is this embodiment is demonstrated. This polycrystalline silicon is manufactured using the polycrystalline silicon manufacturing apparatus 20 shown in FIG.
The polycrystalline silicon manufacturing apparatus 20 includes a crucible 21 in which the silicon melt L is stored, a chill plate 22 on which the crucible 22 is placed, an underfloor heater 23 that supports the chill plate 22 from below, and a crucible 21. And a ceiling heater 24 disposed above. A heat insulating material 25 is provided around the crucible 21.

ここで、ルツボ21は、水平断面形状が角形(四角形)又は丸形(円形)をなすシリカ製とされている。
また、チルプレート22は、中空構造とされており、供給パイプ26を介して内部にArガスが供給される構成とされている。
Here, the crucible 21 is made of silica whose horizontal cross-sectional shape is square (square) or round (circular).
The chill plate 22 has a hollow structure, and Ar gas is supplied to the inside through a supply pipe 26.

この多結晶シリコン製造装置20により多結晶シリコンインゴットを作製する際には、まず、ルツボ21内にシリコン原料を装入する。このシリコン原料を、天井ヒータ24と床下ヒータ23とに通電して加熱して溶解する。これにより、ルツボ21内には、シリコン融液Lが貯留されることになる。   When producing a polycrystalline silicon ingot by the polycrystalline silicon manufacturing apparatus 20, first, a silicon raw material is charged into the crucible 21. This silicon raw material is melted by energizing and heating the ceiling heater 24 and the underfloor heater 23. As a result, the silicon melt L is stored in the crucible 21.

次に、床下ヒータ23への通電を停止し、チルプレート22の内部に供給パイプ26を介してArガスを供給する。これにより、ルツボ21の底部を冷却する。さらに、天井ヒータ24への通電を徐々に減少させることにより、シリコン融液Lは、ルツボ21の底部から冷却されて下部から上方に向けて一方向凝固することになる。これにより、下部から上方に向けて延びる柱状晶からなす多結晶シリコンインゴットが製出される。   Next, energization of the underfloor heater 23 is stopped, and Ar gas is supplied into the chill plate 22 through the supply pipe 26. Thereby, the bottom part of the crucible 21 is cooled. Furthermore, by gradually reducing the energization to the ceiling heater 24, the silicon melt L is cooled from the bottom of the crucible 21 and solidifies in one direction from the lower part upward. As a result, a polycrystalline silicon ingot made of columnar crystals extending upward from the lower part is produced.

このとき、一方向凝固によって、酸素等の不純物が固体側から液体側へと排出されることになり、純度の高い多結晶シリコンインゴットを得ることが可能となる。よって、酸素濃度が1.0×1018atoms/cc未満となるのである。
また、凝固速度を調整することによって、結晶粒径を粗大化させることができ、多結晶シリコンの平均結晶粒径を、3mm以上20mm以下に設定することが可能となるのである。
At this time, by unidirectional solidification, impurities such as oxygen are discharged from the solid side to the liquid side, and a high-purity polycrystalline silicon ingot can be obtained. Therefore, the oxygen concentration is less than 1.0 × 10 18 atoms / cc.
Moreover, by adjusting the solidification rate, the crystal grain size can be increased, and the average crystal grain size of polycrystalline silicon can be set to 3 mm or more and 20 mm or less.

このような構成とされた本実施形態である赤外線透過部材用シリコン材料およびこの赤外線透過部材用シリコン材料から構成されたレンズ部材10によれば、多結晶シリコンからなり、酸素濃度が1.0×1018atoms/cc未満、好ましくは5.0×1017atoms/cc未満、さらに好ましくは1.0×1016atoms/cc未満とされているので、シリコン結晶内の酸素に起因する波長9μm前後(8〜12μm)の赤外線の吸収を抑制することが可能となる。 According to the silicon material for the infrared transmitting member and the lens member 10 made of this silicon material for the infrared transmitting member according to the present embodiment having such a configuration, it is made of polycrystalline silicon and has an oxygen concentration of 1.0 ×. Since it is less than 10 18 atoms / cc, preferably less than 5.0 × 10 17 atoms / cc, more preferably less than 1.0 × 10 16 atoms / cc, the wavelength is about 9 μm due to oxygen in the silicon crystal. It becomes possible to suppress absorption of infrared rays (8 to 12 μm).

また、波長9μm前後(8〜12μm)の赤外線の吸収については、抵抗率と相関関係があることが知られているが、本実施形態では、多結晶シリコンの抵抗率を1Ωcm以上としているので、波長9μm前後(8〜12μm)の赤外線の吸収を確実に抑制することができる。
したがって、波長1.2〜14μmといった広範囲な波長領域で透過率が確保されることになり、レンズ部材10等の赤外線透過部材の素材として使用することが可能となる。
In addition, it is known that the absorption of infrared rays having a wavelength of around 9 μm (8 to 12 μm) has a correlation with the resistivity, but in this embodiment, the resistivity of polycrystalline silicon is 1 Ωcm or more, Absorption of infrared rays having a wavelength of about 9 μm (8 to 12 μm) can be reliably suppressed.
Therefore, the transmittance is ensured in a wide wavelength region such as a wavelength of 1.2 to 14 μm, and it can be used as a material for an infrared transmitting member such as the lens member 10.

また、本実施形態である赤外線透過部材用シリコン材料は、多結晶シリコンとされているので、単結晶シリコンよりも酸素濃度を比較的容易に低減することができ、赤外線の吸収を抑制することが可能となる。
特に、本実施形態では、一方向凝固法によって多結晶シリコンを製出しているので、固液界面において、固体側から液体側へと不純物が排出されることになり、純度の高い多結晶シリコンを得ることができる。よって、赤外線透過部材用シリコン材料中の酸素濃度を確実に低減させることができ、赤外線の吸収を抑えることができる。また、一方向凝固であることから、凝固方向に向くように柱状晶が成長することになり、結晶粒径を比較的大きくすることが可能となる。
In addition, since the silicon material for the infrared transmitting member according to the present embodiment is made of polycrystalline silicon, the oxygen concentration can be reduced relatively easily as compared with single crystal silicon, and the absorption of infrared rays can be suppressed. It becomes possible.
In particular, in this embodiment, since polycrystalline silicon is produced by the unidirectional solidification method, impurities are discharged from the solid side to the liquid side at the solid-liquid interface. Obtainable. Therefore, the oxygen concentration in the silicon material for an infrared transmitting member can be reliably reduced, and infrared absorption can be suppressed. In addition, since it is unidirectionally solidified, columnar crystals grow in the direction of solidification, and the crystal grain size can be made relatively large.

さらに、多結晶シリコンの平均結晶粒径が、3mm以上20mm以下とされているので、この赤外線透過部材用シリコン材料で構成されたレンズ部材10内部に存在する結晶粒界の数が少なくなり、赤外線の散乱を抑制することができる。よって、赤外線レーザの出力が高い場合であっても、この赤外線透過部材用シリコン材料からなるレンズ部材10等の赤外線透過部材を使用することが可能となる。   Furthermore, since the average crystal grain size of the polycrystalline silicon is 3 mm or more and 20 mm or less, the number of crystal grain boundaries existing inside the lens member 10 made of this silicon material for infrared transmitting member is reduced, and infrared rays are reduced. Can be suppressed. Therefore, even when the output of the infrared laser is high, it is possible to use an infrared transmitting member such as the lens member 10 made of the silicon material for the infrared transmitting member.

以上、本発明の実施形態である赤外線透過部材用シリコン材料について説明したが、これに限定されることはなく、適宜設計変更することができる。
例えば、シリコン原料を溶融させたシリコン融液を凝固させたものとして説明したが、これに限定されることはなく、シリコン原料やシリコン融液に、ボロン(B)やアルミニウム(Al)をドーピングしてもよい。
As described above, the silicon material for an infrared transmitting member according to the embodiment of the present invention has been described, but the present invention is not limited to this, and the design can be changed as appropriate.
For example, although the silicon melt obtained by melting the silicon raw material has been described as solidified, the present invention is not limited to this, and boron (B) or aluminum (Al) is doped into the silicon raw material or the silicon melt. May be.

また、赤外線透過部材の一例として、図1に示すようなレンズ部材10(凸レンズ)を挙げて説明したが、これに限定されることはなく、凹レンズ、フレネルレンズ、メニスカスレンズ等の他のレンズ部材であってもよいし、赤外線を透過するとともに赤外線の進行方向を制御するプリズム部材等であってもよい。   Further, the lens member 10 (convex lens) as shown in FIG. 1 has been described as an example of the infrared transmitting member, but the present invention is not limited to this, and other lens members such as a concave lens, a Fresnel lens, and a meniscus lens. It may be a prism member that transmits infrared rays and controls the traveling direction of infrared rays.

さらに、図3に示す多結晶シリコン製造装置を用いて多結晶シリコンからなる赤外線透過部材用シリコン材料を製造するものとして説明したが、これに限定されることはなく、他の多結晶シリコン製造装置を用いてもよい。   Furthermore, although it demonstrated as what manufactures the silicon | silicone material for infrared rays transmissive members which consists of polycrystalline silicon using the polycrystalline silicon manufacturing apparatus shown in FIG. 3, it is not limited to this, Other polycrystalline silicon manufacturing apparatuses May be used.

10 レンズ部材
20 多結晶シリコン製造装置
21 ルツボ
10 Lens member 20 Polycrystalline silicon production device 21 Crucible

Claims (5)

赤外線を透過するレンズやプリズム等の赤外線透過部材の素材として使用される赤外線透過部材用シリコン材料であって、
多結晶シリコンからなり、この多結晶シリコンの抵抗率が1Ωcm以上、かつ、酸素濃度が1.0×1018atoms/cc未満とされていることを特徴とする赤外線透過部材用シリコン材料。
A silicon material for an infrared transmitting member used as a material for an infrared transmitting member such as a lens or prism that transmits infrared rays,
A silicon material for an infrared transmitting member, which is made of polycrystalline silicon and has a resistivity of 1 Ωcm or more and an oxygen concentration of less than 1.0 × 10 18 atoms / cc.
前記多結晶シリコンの平均結晶粒径が、3mm以上20mm以下とされていることを特徴とする請求項1に記載の赤外線透過部材用シリコン材料。   The silicon material for an infrared transmitting member according to claim 1, wherein an average crystal grain size of the polycrystalline silicon is 3 mm or more and 20 mm or less. 前記多結晶シリコンが、一方向凝固法によって製出されたものであることを特徴とする請求項1または請求項2に記載の赤外線透過部材用シリコン材料。   The silicon material for an infrared transmitting member according to claim 1 or 2, wherein the polycrystalline silicon is produced by a unidirectional solidification method. 前記多結晶シリコンに、B又はAlがドーピングされていることを特徴とする請求項1から請求項3のいずれか一項に記載の赤外線透過部材用シリコン材料。   The silicon material for an infrared transmitting member according to any one of claims 1 to 3, wherein the polycrystalline silicon is doped with B or Al. 請求項1から請求項4のいずれか一項に記載の赤外線透過部材用シリコン材料を用いて製造されたことを特徴とする赤外線透過部材。   An infrared transmitting member produced using the silicon material for an infrared transmitting member according to any one of claims 1 to 4.
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