JP2009051678A - Method for manufacturing sapphire substrate - Google Patents
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Abstract
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本発明は、サファイア基板の製造方法に関し、特に、サファイア基板に3−5族元素の化合物半導体、窒化ガリウム(GaN)などの窒化物系化合物半導体を育成して発光ダイオード(LED)、レーザーダイオード(LD)、トランジスタ(FET)などのデバイス得るために用いるサファイア基板の製造方法に関する。 The present invention relates to a method for manufacturing a sapphire substrate, and in particular, grows a compound semiconductor of a group 3-5 element, a nitride compound semiconductor such as gallium nitride (GaN) on a sapphire substrate, and a light emitting diode (LED), a laser diode ( The present invention relates to a method for manufacturing a sapphire substrate used to obtain devices such as LD) and transistors (FET).
従来、サファイア単結晶インゴットからウエハー形状の基板へと加工するプロセスとしては、インゴットの円筒研削加工、オリフラ加工、ウエハースライス、ウエハー外周研削加工、表面研削、表面仕上げ加工及び洗浄の一連の工程を経る事になる。 Conventionally, as a process for processing from a sapphire single crystal ingot to a wafer-shaped substrate, a series of processes of ingot cylindrical grinding, orientation flat processing, wafer slicing, wafer peripheral grinding, surface grinding, surface finishing and cleaning are performed. It will be a thing.
まず、インゴットの円筒研削加工工程で、単結晶の直径が求められるウエハーの外径になるように調整する。次に、オリフラ加工工程で、円筒研削されたインゴットにウエハーの結晶方位や表裏を識別するために用いられるオリエンテーションフラットなどの切りかき状の形状を形成する。これらの加工には、ダイヤモンド固定砥石を用いた研削加工を用いるのが一般的である。 First, in the cylindrical grinding process of the ingot, adjustment is performed so that the diameter of the single crystal becomes the required outer diameter of the wafer. Next, in the orientation flat processing step, a notched shape such as an orientation flat used for identifying the crystal orientation and the front and back of the wafer is formed on the cylindrically-ground ingot. In these processes, a grinding process using a diamond fixed grindstone is generally used.
次に、ウエハースライス工程で、インゴットから所望の厚さのウエハーを多数枚切り出す。 Next, in the wafer slicing step, a number of wafers having a desired thickness are cut out from the ingot.
その後、スライスされたウエハーにはさらに種々の加工を施す。すなわち、ウエハー外周研削加工工程で、ウエハーの側面を所望の形状に加工する。この加工は、ベベリング加工と呼ばれ、この後に行うウエハー両面ラップ加工や、表面仕上げ加工の際に、ウエハーの割れやウエハーのエッジからのスクラッチを低減する効果がある。また、このウエハーを基板として用いるエピタキシャル成長の際に基板の周辺部の異常成長を防いだり、デバイス形成工程における温度サイクルや反りなどによる歪による割れを防いだりする役割も有している。例えば、ヘキ開性が強く機械的な強度も弱いGaAsなどの半導体の加工プロセスでは、歩留まり低下を防止する効果が大きく必須の工程である。しかしながら、硬度が非常に高くヘキ開性も弱く頑丈なサファイアでは、ベベリング加工が施されない場合も多い。 Thereafter, the sliced wafer is further processed in various ways. That is, the side surface of the wafer is processed into a desired shape in the wafer outer periphery grinding process. This process is called a beveling process, and has the effect of reducing wafer cracks and scratches from the wafer edge during wafer double-sided lapping and surface finishing. In addition, the epitaxial growth using this wafer as a substrate also prevents abnormal growth in the peripheral portion of the substrate, and also prevents cracking due to distortion due to temperature cycles and warpage in the device formation process. For example, in a processing process of a semiconductor such as GaAs having a high cleavage property and a low mechanical strength, an effect of preventing a decrease in yield is a large and indispensable step. However, sapphire, which has a very high hardness and a low cleaving ability, is often not beveled.
次に、表面研削工程で、ウエハーの厚さの調整や平行度、平坦度などの加工精度を得る。ここで、基板材料の硬度に応じて研磨材や研磨方式を選択し高精度加工を行う。 Next, in the surface grinding process, processing accuracy such as wafer thickness adjustment, parallelism, and flatness is obtained. Here, an abrasive and a polishing method are selected according to the hardness of the substrate material, and high-precision processing is performed.
最後に、表面仕上げ加工及び洗浄工程により、窒化物半導体のエピタキシャル成長に適した、平坦で歪やキズのない清浄な表面状態を有する基板を得る。 Finally, a substrate having a clean surface state that is flat and free from strain and scratches, suitable for epitaxial growth of nitride semiconductors, is obtained by a surface finishing process and a cleaning process.
近年基板の大口径化が求められているが、基板の径が大きくなるに従いエピタキシャル成長以降のデバイス作製工程においてサファイア基板に発生する反りにより、基板の割れ不良が増加し、歩留まりを大きく下げることが推定されている。すなわち、エピタキシャル成長では、サファイア基板には、基板そのものの反りと、基板とエピタキシャル膜との熱膨張係数の大きな差による反対向きの反りとにより合成された力がかかることになり、基板の大口径化と共にこの力が大きくなるからである。 In recent years, there has been a demand for a larger substrate diameter. However, as the substrate diameter increases, warpage that occurs in the sapphire substrate in the device fabrication process after epitaxial growth increases the number of defects in the substrate, and it is estimated that the yield will be greatly reduced. Has been. In other words, in epitaxial growth, the sapphire substrate is subjected to a combined force due to the warpage of the substrate itself and the warpage in the opposite direction due to the large difference in the thermal expansion coefficient between the substrate and the epitaxial film. This is because this power increases.
このため、シリコン、GaAsなどの基板と同様に、ウエハー側面を研削加工しウエハー強度を向上させて、後工程である表面仕上げ加工の際やエピタキシャル成長の際に、ウエハーの割れやウエハーのエッジからのスクラッチを低減することが要求されるようになってきている(特許文献1参照)。
本発明は上記問題点に鑑みて成されたものであり、基板が大口径化したとしても、エピタルシャル成長以降のデバイス作製工程で反りによる割れを生じないサファイア基板の製造方法の提供を目的とする。 The present invention has been made in view of the above problems, and an object of the present invention is to provide a method for manufacturing a sapphire substrate that does not cause cracking due to warpage in a device manufacturing process after epitaxial growth even when the substrate has a large diameter. .
本発明者は前記目的を達成すべく種々の検討を試みた結果、サファイア基板の反りを特定の範囲に調整すればよいことを見いだして本発明に至った。 As a result of various studies to achieve the above object, the present inventor has found that the warpage of the sapphire substrate may be adjusted to a specific range, and has reached the present invention.
すなわち、本発明は、サファイア単結晶インゴットの円筒研削加工、オリフラ加工、ウエハースライス、ウエハー外周研削加工、表面研削、表面仕上げ加工及び洗浄工程工程からなるサファイア基板の製造方法において、アニール工程を表面研削工程の前または後に設け、またはアニール工程を表面研削工程の間に設け、その後表面仕上げ加工工程に入るものである。 That is, the present invention relates to a method of manufacturing a sapphire substrate comprising cylindrical grinding, orientation flat processing, wafer slicing, wafer peripheral grinding, surface grinding, surface finishing and cleaning process steps of a sapphire single crystal ingot. It is provided before or after the process, or an annealing process is provided during the surface grinding process, and then the surface finishing process is entered.
そして、前記表面研削工程において、この加工後の平均表面粗さを0.9μm以下とする。そのために使用する砥粒を粒径平均#240〜320の範囲で選択する。#240より小さい番手を用いるとラップレートが低く、生産性が悪い問題が生じる。また#320番より大きな番手を用いると、必要とする粗さ0.9μm以下の基板を得られない。従って本条件でラップ加工を行う事より、均一な表面粗さ、安定したラップレート、厚さばらつきの少ない基板が得る事が可能となる。 And in the said surface grinding process, the average surface roughness after this process shall be 0.9 micrometer or less. For this purpose, the abrasive grains to be used are selected in the range of average grain size # 240-320. If a count smaller than # 240 is used, the lap rate is low and the productivity is poor. Moreover, if a count larger than # 320 is used, a required substrate having a roughness of 0.9 μm or less cannot be obtained. Therefore, by performing lapping under these conditions, it is possible to obtain a substrate with uniform surface roughness, a stable wrap rate, and less thickness variation.
そして、前記アニール工程により、反り値が7μm以下の基板を得る。そのため、アニール温度を1200〜1650°C、好ましくは1400〜1650°Cとする。 And the board | substrate whose curvature value is 7 micrometers or less is obtained by the said annealing process. Therefore, the annealing temperature is set to 1200 to 1650 ° C, preferably 1400 to 1650 ° C.
このアニール工程は、前記表面研削工程で発生した基板表面の加工変質層を除去するために行う。変質層除去効果は、1200°Cから得られるが、1400°C以下だと反りに影響を与える加工変質層が十分に除去できない。また、1650°C程度までは変質層除去効果で、反りは減少するが、結晶欠陥が増加する傾向が見られる。従って、結晶欠陥を問題とせず、反り量が小さい基板が必要な際は、1650°C程度までアニール行うと良い。アニール温度を1650°C超えた場合、加工変質層の更なる除去効果はほとんど得られなく、エネルギーコストの増大を招くのみである。また、保持時間については、基板全体が前記範囲内の所望の温度に均等になる時間(好ましくは3時間以上)であればよい。 This annealing step is performed in order to remove the work-affected layer on the substrate surface generated in the surface grinding step. The effect of removing the deteriorated layer is obtained from 1200 ° C., but if it is 1400 ° C. or less, the work affected layer that affects the warp cannot be sufficiently removed. Further, up to about 1650 ° C., the warpage is reduced due to the effect of removing the deteriorated layer, but there is a tendency for crystal defects to increase. Accordingly, when a substrate with a small amount of warpage is required without causing crystal defects, annealing is preferably performed up to about 1650 ° C. When the annealing temperature exceeds 1650 ° C., a further effect of removing the work-affected layer is hardly obtained, and only increases the energy cost. Further, the holding time may be a time (preferably 3 hours or more) at which the entire substrate becomes equal to a desired temperature within the above range.
なお、アニール工程は表面研削工程の前後のいずれで行ってもよく、加工変質層の低減効果を得ることができ、反り量7μm以下のウエハーを得ることができる。
本発明により、反り量7μm以下のサファイア基板を安定的に量産できる事が可能となる。また、本発明により作製した基板を用いるデバイス工程、例えばエピタキシャル成長以降のデバイス工程において基板に発生する反り起因の割れ、スクラッチなどの不良が低減し、工程の安定化ならびに歩留まりの向上に繋がる。
Note that the annealing step may be performed either before or after the surface grinding step, so that the effect of reducing the work-affected layer can be obtained, and a wafer having a warp amount of 7 μm or less can be obtained.
According to the present invention, it is possible to stably mass-produce a sapphire substrate having a warp amount of 7 μm or less. In addition, defects such as cracks and scratches caused by warpage occurring in the substrate in a device process using the substrate manufactured according to the present invention, for example, a device process after epitaxial growth, are reduced, leading to stabilization of the process and improvement of yield.
表面研削前または後に行う、反り量を抑制するためのアニール工程は、ポリッシュ非研磨面が、表面研削加工(ラッピング加工)時の粗さを維持し、ラッピング時に受けた加工変質層除去のために行う。変質層除去効果は、1200°Cから得られるが、1400°C以下だと反りに影響を与える加工変質層が十分に除去できない。また、1650°C程度までは変質層除去効果で、反りは減少するが、結晶欠陥が増加する傾向が見られる。従って、結晶欠陥を問題とせず、反り量が小さい基板が必要な際は、1650°C程度までアニール行うと良い。アニール温度が1650°Cを超えた場合、加工変質層の更なる除去効果はほとんど得られなく、エネルギーコストの増大を招くのみである。また、保持時間については、基板全体を均等に1400°Cとするために必要な時間である。 The annealing process to suppress the amount of warpage before or after surface grinding is performed to maintain the roughness of the polished non-polished surface during surface grinding (lapping) and to remove the work-affected layer that was received during lapping. Do. The effect of removing the deteriorated layer is obtained from 1200 ° C., but if it is 1400 ° C. or less, the work-affected layer that affects the warp cannot be sufficiently removed. Further, up to about 1650 ° C., the warpage is reduced due to the effect of removing the deteriorated layer, but there is a tendency that crystal defects increase. Accordingly, when a substrate with a small amount of warpage is required without causing crystal defects, annealing is preferably performed up to about 1650 ° C. When the annealing temperature exceeds 1650 ° C., a further effect of removing the work-affected layer is hardly obtained and only increases the energy cost. In addition, the holding time is a time required to make the entire substrate uniformly 1400 ° C.
アニール工程の前もしくは後で行う両面ラッピング(表面研削)は、砥粒粒径#240〜320の範囲で行う。#240より小さい番手を用いるとラップレートが低く、生産性が悪い問題が生じる。また#320より大きな番手を用いると、必要とする粗さ0.9μm以下の基板を得られない。従って本条件(#240〜#320)でラップ加工を行う事より、均一な表面粗さ、安定したラップレート、厚さばらつきの少ない基板が得る事が可能となる。 Double-sided lapping (surface grinding) performed before or after the annealing step is performed in the range of abrasive grain size # 240-320. If a count smaller than # 240 is used, the lap rate is low and the productivity is poor. Moreover, if a count larger than # 320 is used, a required substrate having a roughness of 0.9 μm or less cannot be obtained. Therefore, by performing lapping under these conditions (# 240 to # 320), it is possible to obtain a substrate with uniform surface roughness, a stable lapping rate, and a small thickness variation.
基板端面加工においては、反り量に影響を及ぼさないと考えられる。また、ラッピング後の加工変質層除去を目的とし、平均粒径約2μmの遊離ダイヤ砥粒を用いたダイヤラッピング加工を行い、ポリッシュ研磨面を約25μm除去する。これは、前述したように、ポリッシュ研磨面が対象で、ポリッシュ非研磨面は加工が行えない。 In the substrate end face processing, it is considered that the warpage amount is not affected. For the purpose of removing the work-affected layer after lapping, diamond lapping using free diamond abrasive grains having an average particle diameter of about 2 μm is performed to remove about 25 μm of the polished surface. As described above, this is for a polished polished surface, and a polished non-polished surface cannot be processed.
また、アニールは切断(スライス)工程以降、どの工程から投入しても、加工変質層の低減効果を得る事ができ、反り値7μm以下のウエハーを得る事ができる。 In addition, annealing can be performed from any step after the cutting (slicing) step, and the effect of reducing the work-affected layer can be obtained, and a wafer having a warp value of 7 μm or less can be obtained.
(実施例1)
本発明の実施例として、直径約φ3インチ、反り量約20μmの切断後約0.75mmt基板を最終仕上げ約0.56mmtでポリッシュ非研磨面がラッピング加工の粗さを維持し、反り量約7μmのウエハーを作製した実施例を以下に示す。
1)外周を研削したサファイア結晶は、内・外周刃カッターもしくはバンドソー及びワイヤーソーで薄く切断する。切断後の、厚さ、表面の粗さを整えるため、粒径範囲約20〜100μmのSiC遊離砥粒を用いて両面ラッピング加工を行い、両面で約139μm除去した。この時点で、反り量はラッピング加工前約25μmから加工後は約10μmとなる。
2)その後、基板外周部の端面の加工を行う。
3)端面加工後、アニールを行う。アニール温度を約1500°Cで行った場合、反り量は、約5μmとなった
4)アニール後、平均粒径約2μmの遊離ダイヤ砥粒を用いたダイヤラッピング加工を行い、ポリッシュ研磨面を約25μm除去し、最終仕上げを目的とし、平均粒径約70nmのコロイダルシルカを用いたポリッシュ加工を行い、片側約17μmを除去する。
(Example 1)
As an example of the present invention, after cutting about Φ3 inch in diameter and warping amount of about 20 μm, a substrate of about 0.75 mmt is finished to a final finish of about 0.56 mmt. Examples of manufacturing the wafers are shown below.
1) The sapphire crystal whose outer periphery is ground is cut into thin pieces with an inner / outer peripheral blade cutter or a band saw and a wire saw. In order to adjust the thickness and surface roughness after cutting, double-sided lapping was performed using SiC free abrasive grains having a particle size range of about 20 to 100 μm, and about 139 μm was removed on both sides. At this time, the warpage amount is about 25 μm before lapping and about 10 μm after processing.
2) Thereafter, the end surface of the outer peripheral portion of the substrate is processed.
3) Annealing is performed after end face processing. When the annealing temperature was about 1500 ° C, the amount of warpage was about 5 µm. 4) After annealing, diamond lapping using free diamond abrasive grains with an average grain size of about 2 µm was performed to reduce the polished surface to about 25 μm is removed, and for the final finishing, polishing using colloidal silker having an average particle diameter of about 70 nm is performed to remove about 17 μm on one side.
これらの工程により、ラッピング後の非研磨面の表面粗さを維持し、かつ、反り量を約5μm程度に抑制したウエハーを作成する事ができた。 By these steps, it was possible to produce a wafer that maintained the surface roughness of the non-polished surface after lapping and suppressed the amount of warpage to about 5 μm.
今回の実施例では、アニールをラッピング工程前に実施しているがラッピング工程後の工程に投入しても、加工変質層の低減効果を得る事ができ、反り値7μm以下のウエハーを得る事ができる。
(実施例2)
実施例1で得られたサファイア基板を窒化物半導体の成長用基板として用いたところ、割れ不良も少なくほぼ問題なく使用できた。すなわち、エピタキシャル成長工程において、本発明による基板の反り量が小さいため、基板とエピタキシャル膜の熱膨張係数による合力が抑制され、割れ低減の効果が得られたと考えられる。
In this example, annealing is performed before the lapping process, but even if it is added to the process after the lapping process, the effect of reducing the work-affected layer can be obtained, and a wafer with a warp value of 7 μm or less can be obtained. it can.
(Example 2)
When the sapphire substrate obtained in Example 1 was used as a substrate for growing a nitride semiconductor, it could be used almost without problems with few cracking defects. That is, in the epitaxial growth process, since the amount of warpage of the substrate according to the present invention is small, it is considered that the resultant force due to the thermal expansion coefficient between the substrate and the epitaxial film is suppressed and the effect of reducing cracks is obtained.
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| JP2011151151A (en) * | 2010-01-20 | 2011-08-04 | Showa Denko Kk | Method of manufacturing semiconductor wafer |
| CN104070446A (en) * | 2013-03-27 | 2014-10-01 | 株式会社迪思科 | Sapphire substrate flattening method |
| CN105525355A (en) * | 2015-11-06 | 2016-04-27 | 浙江露通机电有限公司 | In-situ annealing process for large-size sapphire crystal |
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