JP2014232829A - Method for manufacturing silicon wafer for solar batteries - Google Patents
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Abstract
Description
本発明は、太陽電池用シリコンウエハーの製造方法に関する。 The present invention relates to a method for producing a silicon wafer for solar cells.
ウェハ内に様々な結晶面方位を持つ多結晶シリコンウエハーは、単結晶シリコンウエハーに比して安価であるため、大面積の太陽電池用基板としての利用が期待されている。 Polycrystalline silicon wafers having various crystal plane orientations within the wafer are less expensive than single crystal silicon wafers, and are expected to be used as large-area solar cell substrates.
ところで、単結晶シリコンウエハーの粗面化（表面テクスチャー構造の形成）は、異方性エッチングによりピラミッド形状の形成が可能なため、硫酸、硝酸および弗酸の混合物（混酸）をエッチャントとして使用する異方性エッチング方法が提案されている（特許文献１）。しかしながら、多結晶シリコンウエハーは、単結晶シリコンウエハーと異なり、異方性エッチングが出来ないため、等方性エッチングによる微細孔形状の形成による粗面化が行われる。そして、従来、パターン膜を介してプラズマによる等方性エッチングについての数多くの提案がなされている（特許文献２〜５）。しかしながら、斯かる方法は、前期の湿式エッチングに比して操作性に劣る。 By the way, the roughening of a single crystal silicon wafer (formation of a surface texture structure) can form a pyramid shape by anisotropic etching. An isotropic etching method has been proposed (Patent Document 1). However, since the polycrystalline silicon wafer cannot be anisotropically etched unlike the single crystal silicon wafer, the surface is roughened by forming a fine hole shape by isotropic etching. Conventionally, many proposals for isotropic etching by plasma via a pattern film have been made (Patent Documents 2 to 5). However, such a method is inferior in operability as compared with the previous wet etching.
さらに、シリコン太陽電池のコスト削減として、多結晶シリコンインゴットのスライス方法を遊離砥粒ワイヤーソー方式から加工時間がより少ない固定砥粒ワイヤーソー方式に変更する試みがなされている。しかしながら、固定砥粒ワイヤーソー方式を採用した多結晶シリコンウエハーの表面は、切断痕が少なくて比較的滑らかである。そのため、湿式エッチングによる十分な粗面化は困難である。そこで、多結晶シリコンウエハーの表面をサンドブラスト処理した後に湿式エッチングを行う方法も検討されつつある。 Furthermore, as a cost reduction of the silicon solar cell, an attempt has been made to change the slicing method of the polycrystalline silicon ingot from the free abrasive wire saw method to the fixed abrasive wire saw method with less processing time. However, the surface of the polycrystalline silicon wafer adopting the fixed abrasive wire saw method is relatively smooth with few cut marks. Therefore, it is difficult to sufficiently roughen the surface by wet etching. Therefore, a method of performing wet etching after the surface of the polycrystalline silicon wafer is sandblasted is also being studied.
因に、固定砥粒ワイヤーソー方式を採用した多結晶シリコンウエハーの表面粗さは、後述する立体的表面粗さ（三次元表面粗さ）で表すと１．０〜１．３である。これに対し、遊離砥粒ワイヤーソー方式を採用した多結晶シリコンウエハーの表面粗さは、上記の立体的表面粗さ（三次元表面粗さ）で表すと１．５〜１．９である。 Incidentally, the surface roughness of the polycrystalline silicon wafer adopting the fixed abrasive wire saw method is 1.0 to 1.3 in terms of the three-dimensional surface roughness (three-dimensional surface roughness) described later. On the other hand, the surface roughness of the polycrystalline silicon wafer adopting the free abrasive wire saw method is 1.5 to 1.9 in terms of the above-mentioned three-dimensional surface roughness (three-dimensional surface roughness).
本発明は、上記実情に鑑みなされたものであり、その目的は、シリコンウエハーとして多結晶シリコンインゴットを固定砥粒ワイヤーソー方式でスライスして得た多結晶シリコンウエハーを使用し、エッチング法として湿式エッチングを採用し、しかも、サンドブラスト処理などの前処理を必要とせず、ウエハーの表面を十分に粗面化し得る、太陽電池用シリコンウエハーの製造方法を提供することにある。 The present invention has been made in view of the above circumstances, and its purpose is to use a polycrystalline silicon wafer obtained by slicing a polycrystalline silicon ingot by a fixed abrasive wire saw method as a silicon wafer, and wet as an etching method. An object of the present invention is to provide a method for producing a silicon wafer for solar cells, which employs etching and does not require a pretreatment such as a sandblasting process and can sufficiently roughen the surface of the wafer.
本発明者らは、鋭意検討を重ねた結果、硫酸、硝酸および弗酸を使用して所定の濃度に調節された混酸をエッチャントとして使用することにより、上記の目的を容易に達成し得るとの知見を得た。 As a result of intensive studies, the present inventors have found that the above object can be easily achieved by using a mixed acid adjusted to a predetermined concentration using sulfuric acid, nitric acid and hydrofluoric acid as an etchant. Obtained knowledge.
本発明は、上記の知見に基づき完成されたものであり、その要旨は、レーザーマイクロスコープを利用して測定される立体的表面粗さが１．０〜１．３の多結晶シリコンウエハーの表面を、硫酸濃度が５５〜８５重量％、硝酸濃度が４〜２１重量％、弗酸濃度が２〜１０重量％、水分濃度が２〜１４重量％（但し、これらの合計量は１００重量％）であり、水／硫酸の重量比率は０．２０以下であるエッチャントで等方性エッチングすることを特徴とする太陽電池用基板の製造方法に存する。 The present invention has been completed based on the above findings, and the gist thereof is the surface of a polycrystalline silicon wafer having a three-dimensional surface roughness of 1.0 to 1.3 measured using a laser microscope. The sulfuric acid concentration is 55 to 85% by weight, the nitric acid concentration is 4 to 21% by weight, the hydrofluoric acid concentration is 2 to 10% by weight, and the water concentration is 2 to 14% by weight (the total amount is 100% by weight). In the method of manufacturing a solar cell substrate, isotropic etching is performed with an etchant having a water / sulfuric acid weight ratio of 0.20 or less.
本発明によれば、前述の課題が達成される。 According to the present invention, the aforementioned problems are achieved.
以下、本発明を詳細に説明する。 Hereinafter, the present invention will be described in detail.
本発明においては、シリコンウエハーとして多結晶シリコンインゴットを固定砥粒ワイヤーソー方式でスライスして得た多結晶シリコンウエハーを使用する。多結晶シリコンは、ウェハ内に様々な結晶面方位を持つ、すなわち、隣り合う結晶の方向がばらばらで単結晶のように全体の原子の並び方が一定していない特徴を有する。固定砥粒ワイヤーソー方式（例えば芯線にダイヤモンド砥粒を固定したワイヤーソーを使用する方式）でスライスした場合、そのスライス面は、前述のとおり、切断痕が少なくて比較的滑らかであり、レーザーマイクロスコープを利用して測定される立体的表面粗さが１．０〜１．３であることによって特徴付けられる。 In the present invention, a polycrystalline silicon wafer obtained by slicing a polycrystalline silicon ingot by a fixed abrasive wire saw method is used as the silicon wafer. Polycrystalline silicon has various crystal plane orientations in a wafer, that is, the direction of adjacent crystals is different and the arrangement of atoms as a whole is not constant like a single crystal. When sliced by a fixed abrasive wire saw method (for example, a method using a wire saw in which diamond abrasive grains are fixed to the core wire), the slice surface is relatively smooth with few cutting marks, as described above. It is characterized by a three-dimensional surface roughness measured using a scope of 1.0 to 1.3.
上記の立体的表面粗さは、レーザーマイクロスコープ（例えば、ＫＥＹＥＮＣＨ社製「ＶＫ−９７００」）を使用し、測定時倍率：３，０００倍、観察視野：６，５１２μｍ２の条件下で、シリコンウエハーの凹凸表面の表面積を計測し、その値を観察視野で除した値として定義される。 The above three-dimensional surface roughness was measured using a laser microscope (for example, “VK-9700” manufactured by KEYENCH) under the conditions of magnifying power: 3,000 times and observation field of view: 6,512 μm 2. It is defined as the value obtained by measuring the surface area of the uneven surface of the wafer and dividing the value by the observation field.
レーザーマイクロスコープ：ＫＥＹＥＮＣＨ社製「ＶＫ−９７００」は、短波長レーザ光源」と「白色光源」を用いた２Ｗａｙ光源方式を採用し、この２つの光により、カラー超深度・レーザ超深度・高低画像を構築するために必要な、色・光量・高さの情報を得ることができる装置である。この装置においては、レーザ光源は点光源のため、Ｘ−Ｙスキャン光学系を介して観察視野内を１０２４×７６８ピクセルに分割してスキャンし、各ピクセルごとの反射光を受光素子で検出する。そして、対物レンズをＺ軸方向に駆動し、スキャンを繰り返すことにより各ピクセルのＺ軸位置ごとの反射光量を取得する。これにより、３次元で凹凸を測定することが出来、凹凸表面の立体的表面粗さを把握することが出来る。しかも、最も反射光量の高いＺ軸位置を焦点として、高さ情報と反射光量を検出することが出来る。これにより、全体に焦点の合った光量超深度画像と高低画像（情報）が得られる。 Laser microscope: “VK-9700” manufactured by KEYENCH employs a two-way light source system using a short-wavelength laser light source and a white light source. It is a device that can obtain the information of color, light quantity, and height necessary for constructing. In this apparatus, since the laser light source is a point light source, the observation field is divided into 1024 × 768 pixels and scanned through an XY scanning optical system, and the reflected light for each pixel is detected by a light receiving element. Then, the objective lens is driven in the Z-axis direction, and scanning is repeated to obtain the reflected light amount for each Z-axis position of each pixel. Accordingly, the unevenness can be measured in three dimensions, and the three-dimensional surface roughness of the uneven surface can be grasped. In addition, height information and the amount of reflected light can be detected with the Z-axis position having the highest amount of reflected light as a focal point. Thereby, an ultra-deep light amount image and a high / low image (information) focused on the whole are obtained.
本発明においては、上記の装置を使用した３次元計測として、測定時倍率：３，０００倍の画像上に任意で指定した領域（但し観察視野：６，５１２μｍ２）における対象物の表面積を測定し、その値を観察視野で除した値を立体的表面粗さと定義している。 In the present invention, as a three-dimensional measurement using the above-described apparatus, the surface area of an object is measured in an arbitrarily designated area (observation field of view: 6,512 μm 2 ) on an image having a measurement magnification of 3,000 times. The value obtained by dividing the value by the observation field is defined as the three-dimensional surface roughness.
多結晶シリコン基板は、ｐ型多結晶シリコン基板であってもよく、ｎ型多結晶シリコン基板であってもよい。この場合、シリコン基板に含まれる不純物は、例えば、ｐ型の場合、ホウ素やアルミニウムなどであり、ｎ型の場合、リン、砒素、アンチモンなどである。多結晶シリコン基板がｐ型多結晶シリコン基板またはｎ型多結晶シリコン基板の場合、不純物の濃度は、特に限定されないが、例えば、１０１３／ｃｍ３〜１０２１／ｃｍ３である。 The polycrystalline silicon substrate may be a p-type polycrystalline silicon substrate or an n-type polycrystalline silicon substrate. In this case, the impurity contained in the silicon substrate is, for example, boron or aluminum in the case of p-type, and phosphorus, arsenic, antimony or the like in the case of n-type. When the polycrystalline silicon substrate is a p-type polycrystalline silicon substrate or an n-type polycrystalline silicon substrate, the concentration of impurities is not particularly limited, but is, for example, 10 13 / cm 3 to 10 21 / cm 3 .
多結晶シリコン基板の厚さは、特に限定されないが、通常１００〜３００μｍである。１００μｍ以上とすることにより、シリコン基板が十分な強度を有することができ、３００μｍ以下とすることにより、太陽電池などを低コストで製造することができる。多結晶シリコン基板の大きさは、特に限定されないが、例えば１２６ｍｍ×１２６ｍｍ又は１５６ｍｍ×１５６ｍｍである。 The thickness of the polycrystalline silicon substrate is not particularly limited, but is usually 100 to 300 μm. By setting it as 100 micrometers or more, a silicon substrate can have sufficient intensity | strength, and a solar cell etc. can be manufactured at low cost by setting it as 300 micrometers or less. The size of the polycrystalline silicon substrate is not particularly limited, but is, for example, 126 mm × 126 mm or 156 mm × 156 mm.
本発明においては、硫酸、硝酸および弗酸の混合物をエッチャントとして使用する。エッチャントの調製に使用する原料の酸としては、各種の濃度のものを使用することが出来る。硫酸原料としては、希硫酸、濃硫酸、発煙硫酸などが挙げられる。濃硫酸とは９６〜９８重量％硫酸、発煙硫酸とは濃硫酸に過剰の三酸化硫黄を吸収させたものである。硝酸としては、希硝酸、濃硝酸、発煙硝酸などが挙げられる。濃硝酸とは７０〜９８重量％硝酸、発煙硝酸とは濃硝酸に気体の二酸化窒素を吹き込んだものである。原料弗酸としては、弗酸の他に弗化水素ガス（無水弗酸）を使用することが出来る。 In the present invention, a mixture of sulfuric acid, nitric acid and hydrofluoric acid is used as an etchant. As the raw material acid used for the preparation of the etchant, those having various concentrations can be used. Examples of the sulfuric acid raw material include dilute sulfuric acid, concentrated sulfuric acid, fuming sulfuric acid and the like. Concentrated sulfuric acid is 96-98% by weight sulfuric acid, and fuming sulfuric acid is concentrated sulfuric acid in which excess sulfur trioxide is absorbed. Examples of nitric acid include dilute nitric acid, concentrated nitric acid, and fuming nitric acid. Concentrated nitric acid is 70 to 98% by weight nitric acid, and fuming nitric acid is obtained by blowing gaseous nitrogen dioxide into concentrated nitric acid. As the raw material hydrofluoric acid, hydrogen fluoride gas (anhydrous hydrofluoric acid) can be used in addition to hydrofluoric acid.
本発明において、エッチャントの組成は次のように調節される。すなわち、硫酸濃度は５５〜８５重量％、好ましくは６０〜８０重量％、硝酸濃度は４〜２１重量％、好ましくは１０〜２１重量％、弗酸濃度は２〜１０重量％、好ましくは２〜５重量％、水分濃度は２〜１４重量％、好ましくは７〜１４重量％（但し、これらの合計量は１００重量％）である。また、水／硫酸の重量比率は０．２０以下であることが重要である。 In the present invention, the composition of the etchant is adjusted as follows. That is, the sulfuric acid concentration is 55 to 85 wt%, preferably 60 to 80 wt%, the nitric acid concentration is 4 to 21 wt%, preferably 10 to 21 wt%, and the hydrofluoric acid concentration is 2 to 10 wt%, preferably 2 to 2 wt%. 5% by weight and water concentration is 2 to 14% by weight, preferably 7 to 14% by weight (however, the total amount is 100% by weight). It is also important that the water / sulfuric acid weight ratio is 0.20 or less.
硫酸濃度が５５重量％未満の場合はエッチング速度が遅すぎる傾向があり、８５重量％を超える場合は、硝酸、弗酸、水の適正量の配合に支障を来す。硝酸濃度が４重量％未満の場合はエッチング速度が遅すぎ、２１重量％を超える場合はエッチング速度が速すぎてコントロール困難となる傾向がある。水分濃度は特に重要である。水分濃度が２重量％未満の場合はエッチング速度が遅すぎる。すなわち、湿式エッチングでは硝酸によりシリコンウエハー表面が酸化され、生成したＳｉＯ２とＨＦの反応によりエッチングが進行するが、水の含有量が少な過ぎる場合はＨＦがイオン化せずＳｉＯ２が除去されないためエッチングが進行しない。一方、水分濃度が１４重量％を超える場合や水／硫酸の重量比率が０．２０を超える場合は硝酸の酸化力が低くなりエッチングが困難となる。 When the sulfuric acid concentration is less than 55% by weight, the etching rate tends to be too slow, and when it exceeds 85% by weight, mixing of appropriate amounts of nitric acid, hydrofluoric acid and water is hindered. When the nitric acid concentration is less than 4% by weight, the etching rate is too slow, and when it exceeds 21% by weight, the etching rate tends to be too fast and difficult to control. The moisture concentration is particularly important. When the water concentration is less than 2% by weight, the etching rate is too slow. That is, in wet etching, the surface of the silicon wafer is oxidized by nitric acid, and etching proceeds due to the reaction between the generated SiO 2 and HF. However, if the water content is too small, HF is not ionized and SiO 2 is not removed. Does not progress. On the other hand, when the water concentration exceeds 14% by weight or when the weight ratio of water / sulfuric acid exceeds 0.20, the oxidizing power of nitric acid becomes low and etching becomes difficult.
因に、スライスしたままのウエハーには、表面に機械的ダメージ(欠陥)の残った層が存在するが、上記のエッチャントによる湿式エッチングによれば、ダメージ層の除去と、表面テクスチャー構造の形成とを同じ工程で行うことが出来る。そのため、本発明においては、酸又はアルカリ等でエッチングするダメージ層の除去工程を予め行う必要はない。 Incidentally, the wafer that has been sliced has a layer with mechanical damage (defects) remaining on the surface, but according to the wet etching using the above etchant, the damage layer is removed and the surface texture structure is formed. Can be performed in the same process. For this reason, in the present invention, it is not necessary to perform in advance the step of removing the damaged layer by etching with acid or alkali.
エッチングに要する時間は、エッチャント組成および温度と、多結晶シリコン基板の厚さと所望のエッチング後の厚さとによって決められるが、例えば、ディップ式で行った場合は、通常０．１〜１０分程度であり、エッチング量は、片面で、ウェハ面内平均１〜２０μｍ程度となるエッチング量が最適である。また、エッチングの温度（エッチャントの温度）は通常０〜３０℃である。 The time required for etching is determined by the etchant composition and temperature, the thickness of the polycrystalline silicon substrate, and the desired post-etching thickness. For example, in the case of a dip method, it is usually about 0.1 to 10 minutes. In addition, the etching amount is optimally an etching amount that is about 1 to 20 μm on the wafer surface average on one side. The etching temperature (etchant temperature) is usually 0 to 30 ° C.
次に、実施例を挙げて本発明を更に詳細に説明するが、本発明はこれらに何ら制限されるものではない。なお、エッチャントの調製用酸には、９７重量％硫酸、９８重量％硝酸、５０重量％弗酸を使用した。 EXAMPLES Next, although an Example is given and this invention is demonstrated further in detail, this invention is not restrict | limited to these at all. Note that 97 wt% sulfuric acid, 98 wt% nitric acid, and 50 wt% hydrofluoric acid were used as acids for preparing the etchant.
実施例１〜４及び比較例１〜２：
サイズ１５６ｍｍ×１５６ｍｍ±０．５ｍｍ、厚さ２００μｍ±２０μｍのＰ型多結晶シリコンウエハーを、表１に示した組成のエッチャントでエッチングし、得られた凹凸表面の立体的表面粗さを測定した。上記のシリコンウエハーは、多結晶シリコンインゴットを固定砥粒ワイヤーソー方式でスライスして得られたものであり、前述の立体的表面粗さは１．１である。また、エッチング温度は２５℃、エッチング時間は６０秒とした。立体的表面粗さ測定結果を表１に示す。
Examples 1-4 and Comparative Examples 1-2:
A P-type polycrystalline silicon wafer having a size of 156 mm × 156 mm ± 0.5 mm and a thickness of 200 μm ± 20 μm was etched with an etchant having the composition shown in Table 1, and the three-dimensional surface roughness of the resulting uneven surface was measured. The silicon wafer is obtained by slicing a polycrystalline silicon ingot by a fixed abrasive wire saw method, and the above-mentioned three-dimensional surface roughness is 1.1. The etching temperature was 25 ° C. and the etching time was 60 seconds. Table 1 shows the three-dimensional surface roughness measurement results.
（１）凹凸表面の立体的表面粗さの測定：
レーザーマイクロスコープ：ＫＥＹＥＮＣＨ社製「ＶＫ−９７００」を使用し、測定時倍率：３，０００倍、観察視野：６，５１２μｍ２の条件下で、多結晶シリコンウエハーの凹凸表面の表面積を計測し、その値を観察視野で除し、立体的表面粗さ値を算出した。
(1) Measurement of three-dimensional surface roughness of uneven surface:
Laser microscope: Using “VK-9700” manufactured by KEYENCH, measuring the surface area of the concavo-convex surface of the polycrystalline silicon wafer under the conditions of the magnification at the time of measurement: 3,000 times and the viewing field: 6,512 μm 2 , The value was divided by the observation field, and the three-dimensional surface roughness value was calculated.
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| CN107971933A (en) * | 2016-10-21 | 2018-05-01 | 乐山新天源太阳能科技有限公司 | A kind of minimizing technology of polysilicon chip surface diamond wire cutting damage layer |
| JP2018535558A (en) * | 2015-11-23 | 2018-11-29 | インテグリス・インコーポレーテッド | Composition and method for selectively etching p-type doped polysilicon relative to silicon nitride |
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| WO2012102368A1 (en) * | 2011-01-27 | 2012-08-02 | 京セラ株式会社 | Solar battery element manufacturing method, solar battery element, and solar battery module |
| JP2014225633A (en) * | 2013-04-26 | 2014-12-04 | 株式会社Tkx | Silicon wafer for solar batteries, and method for manufacturing the same |
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| WO2012102368A1 (en) * | 2011-01-27 | 2012-08-02 | 京セラ株式会社 | Solar battery element manufacturing method, solar battery element, and solar battery module |
| JP2014225633A (en) * | 2013-04-26 | 2014-12-04 | 株式会社Tkx | Silicon wafer for solar batteries, and method for manufacturing the same |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2018535558A (en) * | 2015-11-23 | 2018-11-29 | インテグリス・インコーポレーテッド | Composition and method for selectively etching p-type doped polysilicon relative to silicon nitride |
| US10991809B2 (en) | 2015-11-23 | 2021-04-27 | Entegris, Inc. | Composition and process for selectively etching p-doped polysilicon relative to silicon nitride |
| CN107971933A (en) * | 2016-10-21 | 2018-05-01 | 乐山新天源太阳能科技有限公司 | A kind of minimizing technology of polysilicon chip surface diamond wire cutting damage layer |
| CN107971933B (en) * | 2016-10-21 | 2020-05-01 | 乐山新天源太阳能科技有限公司 | Method for removing diamond wire cutting damage layer on surface of polycrystalline silicon wafer |
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