JP4994568B2 - Silica glass crucible - Google Patents
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- JP4994568B2 JP4994568B2 JP2003405059A JP2003405059A JP4994568B2 JP 4994568 B2 JP4994568 B2 JP 4994568B2 JP 2003405059 A JP2003405059 A JP 2003405059A JP 2003405059 A JP2003405059 A JP 2003405059A JP 4994568 B2 JP4994568 B2 JP 4994568B2
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 60
- 230000002093 peripheral effect Effects 0.000 claims description 5
- 239000011148 porous material Substances 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 description 19
- 239000013078 crystal Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000000465 moulding Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000002109 crystal growth method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000001175 rotational moulding Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- -1 silicon alkoxide Chemical class 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Description
本発明はシリカガラスルツボに係わり、特にシリコン単結晶引き上げに用いた際の変形を抑制したシリカガラスルツボに関する。 The present invention relates to a silica glass crucible, and more particularly to a silica glass crucible that suppresses deformation when used for pulling a silicon single crystal.
半導体デバイスの基板に用いられるシリコン単結晶は、一般にチョクラルスキー法（ＣＺ法）で製造されており、このＣＺ法はシリカガラスルツボ内に多結晶シリコン原料を装填し、この装填されたシリコン原料を周囲から加熱して溶融し、上方から吊り下げた種結晶をシリコン融液に接触させて引き上げるものである。 A silicon single crystal used for a substrate of a semiconductor device is generally manufactured by the Czochralski method (CZ method). In this CZ method, a polycrystalline silicon raw material is loaded into a silica glass crucible, and the loaded silicon raw material Is melted by heating from the surroundings, and the seed crystal suspended from above is brought into contact with the silicon melt and pulled up.
従来、シリカガラスルツボは、一般にアーク溶融法により製造され、内表面側に透明シリカガラスからなる透明層を有し、この外周側に多数の閉気孔を含んだ不透明シリカガラスからなる不透明層を有する２層の構造をなしている。 Conventionally, a silica glass crucible is generally manufactured by an arc melting method, and has a transparent layer made of transparent silica glass on the inner surface side, and has an opaque layer made of opaque silica glass including many closed pores on the outer peripheral side. It has a two-layer structure.
一方、引き上げられるシリコン単結晶の大口径化に伴い、シリカガラスルツボは年々大型化しており、このルツボの大型化により、多結晶シリコンの装填量を増大させることができ、スループットの向上をもたらす反面、溶融の長時間化、加熱用カーボンヒータの大出力化といった厳しい環境下で使用されている。その結果、単結晶製造中のシリカガラスルツボの変形問題が顕著になり、このため、シリカガラスルツボの粘性を高める工夫や、シリカ質原料の粘性を補うために直胴部の厚さを増加させる方法が採られている。 On the other hand, silica glass crucibles are getting larger year by year as the diameter of the silicon single crystal to be pulled is increased, and this larger crucible can increase the amount of polycrystalline silicon loaded, leading to improved throughput. It is used in harsh environments such as longer melting times and higher output of heating carbon heaters. As a result, the problem of deformation of the silica glass crucible during the production of single crystals becomes prominent. For this reason, the device for increasing the viscosity of the silica glass crucible and the thickness of the straight body portion to increase the viscosity of the siliceous material are increased. The method is taken.
特許文献１には、シリカガラスルツボの直胴部を構成するシリカ質原料英の粘性率と、その直胴部の厚さとに一定の関係を持たせて規定しシリカガラスルツボの変形を防ぐ単結晶成長方法が提案されている。しかしながら、特許文献１のシリカガラスルツボは、全体が透明層または不透明層の粘性率を用い、あるいは２層シリカガラスルツボにあっては、各層の平均粘性率を算出して、これを全体の粘性率と規定するシリカガラスルツボの変形防止に関する提案であり、粘性率が低い材料を用いた場合には、シリカガラスルツボの直胴部の厚さを増大せしめる必要があり、そうすると当該直胴部の自重による沈み込みによる変形等があり、決して十分な解決には至っておらず、２層の構造のシリカガラスルツボにおいては、大型化したシリカガラスルツボの変形を防止することができない。 Patent Document 1 discloses a simple method for preventing the deformation of the silica glass crucible by providing a certain relationship between the viscosity of the siliceous raw material constituting the straight body portion of the silica glass crucible and the thickness of the straight body portion. A crystal growth method has been proposed. However, the silica glass crucible of Patent Document 1 uses the viscosity of a transparent layer or an opaque layer as a whole, or in the case of a two-layer silica glass crucible, the average viscosity of each layer is calculated and this is used as the overall viscosity. If a material with a low viscosity is used, it is necessary to increase the thickness of the straight barrel portion of the silica glass crucible. There is deformation due to subduction due to its own weight, and it has never been a sufficient solution, and in a silica glass crucible having a two-layer structure, deformation of an enlarged silica glass crucible cannot be prevented.
なお、特許文献２には、シリカガラスルツボの原料として、シリカ質原料中の不純物を規定することにより、１４５０℃における粘度が１０１０ポイズ以上にした天然シリカ質原料を用い、変形を抑制するシリカガラスルツボが提案されているが、単に１４５０℃における粘性率を規制しただけでは、大型化したシリカガラスルツボの変形を防止することが、十分に達成できなかった。
本発明は上述した事情を考慮してなされたもので、直胴部の厚さを増加させることなく、大口径の単結晶を引き上げても変形が少ないシリカガラスルツボを提供することを目的とする。 The present invention has been made in consideration of the above-described circumstances, and an object thereof is to provide a silica glass crucible with little deformation even when a large-diameter single crystal is pulled up without increasing the thickness of the straight body portion. .
本発明者は、内表面側に透明シリカガラスからなる透明層を有し、この外周側に多数の閉気孔を含んだ不透明シリカガラスからなる不透明層を有する２層の構造を有するシリカガラスルツボにおいて、両層に同一原料を使用した場合、気泡を有する不透明層の粘度が約２０％低下するため、透明層部分と不透明層部分に粘度差が生じ、この粘度差が大きいほど変形を起こし易いことをつきとめ、不透明層の粘度を透明層の粘度に近づけることにより、粘度差を解消し変形を抑制することが可能となるとの知見を得、本発明を完成させるに至った。 In the silica glass crucible having a two-layer structure having a transparent layer made of transparent silica glass on the inner surface side and an opaque layer made of opaque silica glass containing a number of closed pores on the outer peripheral side. When the same raw material is used for both layers, the viscosity of the opaque layer having bubbles is reduced by about 20%, so that a difference in viscosity occurs between the transparent layer portion and the opaque layer portion, and the larger the viscosity difference, the easier the deformation. As a result, the inventors have found that it is possible to eliminate the viscosity difference and suppress deformation by bringing the viscosity of the opaque layer closer to the viscosity of the transparent layer, and the present invention has been completed.
すなわち、上記目的を達成するため、内表面側に透明シリカガラスからなる透明層を有し、この外周側に多数の閉気孔を含んだ不透明シリカガラスからなる不透明層を有するシリカガラスルツボにおいて、前記透明層の厚さを１としたとき、４〜６の厚さの前記不透明層を有し、前記不透明層は、不透明層の金属不純物濃度および／もしくはＯＨ基濃度により、粘度が調整されて、１３５０℃における粘度が１１．０ポイズ以上であり、かつ透明層のたわみ量に対し、±１５％以内のたわみ量を有することを特徴とするシリカガラスルツボが提供される。これにより、直胴部の厚さを増加させることなく、大口径の単結晶を引き上げても変形が少ないシリカガラスルツボが実現される。 That is, in order to achieve the above object, in the silica glass crucible having the transparent layer made of transparent silica glass on the inner surface side and the opaque layer made of opaque silica glass containing a large number of closed pores on the outer peripheral side, When the transparent layer has a thickness of 1, the opaque layer has a thickness of 4 to 6, and the opaque layer has a viscosity adjusted by the metal impurity concentration and / or OH group concentration of the opaque layer, There is provided a silica glass crucible having a viscosity at 1350 ° C. of 11.0 poise or more and having a deflection amount within ± 15% with respect to the deflection amount of the transparent layer. As a result, a silica glass crucible with little deformation is realized even if the single crystal having a large diameter is pulled up without increasing the thickness of the straight body portion.
好適な一例では、前記透明層が合成シリカ質原料を溶融した層であり、前記不透明層が天然シリカ質原料を溶融した層からなる。 In a preferred example, the transparent layer is a layer obtained by melting a synthetic siliceous material, and the opaque layer is a layer obtained by melting a natural siliceous material.
本発明に係わるシリカガラスルツボによれば、直胴部の厚さを増加させることなく、大口径の単結晶を引き上げても変形が少ないシリカガラスルツボを提供することができる。 According to the silica glass crucible according to the present invention, it is possible to provide a silica glass crucible with little deformation even when a single crystal having a large diameter is pulled up without increasing the thickness of the straight body portion.
以下、本発明に係わるシリカガラスルツボの一実施形態について添付図面を参照して説明する。 Hereinafter, an embodiment of a silica glass crucible according to the present invention will be described with reference to the accompanying drawings.
図１は本発明に係わるシリカガラスルツボの縦断面図である。 FIG. 1 is a longitudinal sectional view of a silica glass crucible according to the present invention.
図１に示すように、本発明に係わるシリカガラスルツボ１は、内表面側に透明シリカガラスからなる透明層２と、この外周側に多数の閉気孔を含んだ不透明シリカガラスからなる不透明層３を有する２層構造であり、透明層２の厚さを１としたとき、不透明層３の厚さは４〜６であり、この不透明層３は、その１３５０℃における粘度が１１．０ポイズ以上であり、かつ透明層２のたわみ量に対し、±１５％以内のたわみ量を有する。
As shown in FIG. 1, a silica glass crucible 1 according to the present invention includes a
通常、不透明層の方が透明層に対して厚く形成され不透明層が耐変形性の支配的要因になっており、不透明層の厚さは、透明層の厚さを１としたとき、不透明層の厚さが４未満では、十分な耐変形性が得られず、６を超えると、特にルツボのストレート部の重量が大きくなり、ストレート部の内側への沈み込みの問題が生じる。 Usually, the opaque layer is formed to be thicker than the transparent layer, and the opaque layer is a dominant factor for deformation resistance. The thickness of the opaque layer is defined as 1 when the thickness of the transparent layer is 1. If the thickness is less than 4, sufficient deformation resistance cannot be obtained, and if it exceeds 6, the weight of the straight portion of the crucible becomes particularly large, which causes a problem of sinking into the straight portion.
また、不透明層の粘度が１１．０ポイズ未満では、十分な耐変形性が得られず、さらに、不透明層のたわみ量が透明層のたわみ量に対し、±１５％以内の範囲外では、変形量が大きくなり十分な耐変形性が得られない。 In addition, when the viscosity of the opaque layer is less than 11.0 poise, sufficient deformation resistance cannot be obtained. Further, when the amount of deflection of the opaque layer is outside the range of ± 15% relative to the amount of deflection of the transparent layer, deformation is not possible. The amount increases and sufficient deformation resistance cannot be obtained.
不透明層のたわみ量が透明層のたわみ量に対し、より好ましくは、±５％以内である。 More preferably, the amount of deflection of the opaque layer is within ± 5% of the amount of deflection of the transparent layer.
なお、上記たわみ量は、図２に示すように、幅５ｍｍ、厚さ２ｍｍ、長さ５０ｍｍのシリカガラスを片持ちはり状に固定台に溶接し、１３５０℃で２時間放置したときの先端のたわみ距離と定義する。 Note that, as shown in FIG. 2, the amount of deflection described above is obtained by welding a silica glass having a width of 5 mm, a thickness of 2 mm, and a length of 50 mm to a fixed base in a cantilever shape and leaving it at 1350 ° C. for 2 hours. It is defined as the deflection distance.
本発明に係わるシリカガラスルツボは、一般的な回転モールド法などにより製造される。例えば、複数の貫通孔が穿設されたルツボ成形用型を高速で回転させ、これに水晶等の不透明層用シリカ質原料、例えばシリコンアルコキシドもしくは四塩化珪素の加水分解により得られる透明層用シリカ質原料粉の順で、特性あるいは種類の異なるシリカ質原料を供給する。供給された不透明層用シリカ質粉は、遠心力によってルツボ成形用型の内面側に押圧されルツボ成形体の外層として形成され、透明層用シリカ質原料は内層として形成される。ルツボ成形用型内を減圧し、アーク電極に通電して成形体の内側から加熱し、成形体を溶融して、内層が透明層のシリカガラスルツボを製造する。また、適宜、減圧を止めることで、内層が透明、外層が不透明のシリカガラスルツボを製造することができる。 The silica glass crucible according to the present invention is manufactured by a general rotational molding method or the like. For example, a transparent layer silica obtained by rotating a crucible molding die having a plurality of through holes at high speed and hydrolyzing a siliceous raw material for an opaque layer such as quartz, for example, silicon alkoxide or silicon tetrachloride. Silica raw materials with different characteristics or types are supplied in the order of raw material powder. The supplied siliceous powder for opaque layer is pressed against the inner surface side of the crucible molding die by centrifugal force to form an outer layer of the crucible molded body, and the siliceous raw material for transparent layer is formed as an inner layer. The inside of the crucible molding die is depressurized, the arc electrode is energized and heated from the inside of the molded body, and the molded body is melted to produce a silica glass crucible whose inner layer is a transparent layer. Further, by appropriately stopping the decompression, a silica glass crucible having an inner layer that is transparent and an outer layer that is opaque can be manufactured.
このようなシリカガラスルツボの製造工程において、内層である透明層及び外層である不透明層のいずれにも天然原料（水晶）を用い、かつ、透明層の原料がＡｌ≦８ｐｐｍであるとき、不透明層の原料はＡｌ≧１５ｐｐｍであるものを用いるのが好ましく、あるいは、透明層の原料がＮａ＋Ｋ（アルカリ金属）≦０．５ｐｐｍであるとき、不透明層の原料はＮａ＋Ｋ≦０．１ｐｐｍであるものを用いるのが好ましい。 In the production process of such a silica glass crucible, when a natural raw material (quartz) is used for both the transparent layer as the inner layer and the opaque layer as the outer layer, and the raw material of the transparent layer is Al ≦ 8 ppm, the opaque layer It is preferable to use a material of Al ≧ 15 ppm, or when the transparent layer material is Na + K (alkali metal) ≦ 0.5 ppm, the opaque layer material is Na + K ≦ 0.1 ppm. Is preferred.
また、本発明に係わるシリカガラスルツボは、透明層が合成シリカ質原料の溶融した層、不透明層が天然シリカ質原料を溶融した層であるのが好ましい。これにより、直胴部の厚さを増加させることなく、大口径の単結晶を引き上げてもより顕著に変形を抑制できる。さらに、その直胴部の厚さは、沈み込み変化をより抑制するためには、８〜１６ｍｍであるのが好ましい。 In the silica glass crucible according to the present invention, the transparent layer is preferably a layer in which a synthetic siliceous material is melted, and the opaque layer is a layer in which a natural siliceous material is melted. Thereby, even if it pulls up the single crystal of a large diameter, without increasing the thickness of a straight body part, a deformation | transformation can be suppressed more notably. Furthermore, the thickness of the straight body portion is preferably 8 to 16 mm in order to further suppress the subsidence change.
上記のように本実施形態のシリカガラスルツボは、同一原料を使用した場合、透明層の厚さ及びたわみ量に対し、不透明層の厚さ及びたわみ量を特定の値に規定し、かつ不透明層の粘度を透明層の粘度に近づけることにより、粘度差を解消し、直胴部の厚さを増加させることなく、単結晶引き上げ時の変形を抑制することができる。また、透明層が合成シリカ質原料、不透明層が天然シリカ質原料を使用した場合、透明層の厚さ及びたわみ量に対し、不透明層の厚さ及びたわみ量を特定の値に規定し、不透明層の原料と透明層の原料のＡｌの含有量を制御して粘度差を解消し、直胴部の厚さを増加させることなく、単結晶引き上げ時の変形を抑制することができる。 As described above, when the same raw material is used, the silica glass crucible of this embodiment defines the thickness and the amount of deflection of the opaque layer to a specific value with respect to the thickness and the amount of deflection of the transparent layer, and the opaque layer. By making the viscosity close to that of the transparent layer, the difference in viscosity can be eliminated, and deformation during pulling of the single crystal can be suppressed without increasing the thickness of the straight body portion. In addition, when the transparent layer uses a synthetic siliceous raw material and the opaque layer uses a natural siliceous raw material, the thickness and the amount of deflection of the opaque layer are regulated to specific values with respect to the thickness and the amount of deflection of the transparent layer. By controlling the Al content of the raw material of the layer and the raw material of the transparent layer, the difference in viscosity can be eliminated, and deformation during pulling of the single crystal can be suppressed without increasing the thickness of the straight body part.
透明層、不透明層の金属不純物濃度および／もしくはＯＨ基濃度により、粘度を調整し、また、不透明層および透明層の厚さは、シリカ質原料粉の堆積厚さおよび溶融時間により調整（全体厚さはいずれも１２ｍｍ±０．５ｍｍ）して、透明層及び不透明層が表１に示すような粘度を有する口径３２インチの天然シリカガラスルツボを作製し、これらを用いて直径１２インチの単結晶の引き上げ試験を実施した。表１に結果を示す。なお、表１中、不透明層の値は、透明層の値を１としたときの相対指数で示す。
表１からもわかるように、粘度（１１．０ポイズ以上）、不透明層の厚さ（４〜６）、不透明層のたわみ量率（±１５％以内）のいずれもが本発明範囲内である実施例１〜４は、ＤＦ率（単結晶化率）が１００％と極めて良好であり、使用後のシリカガラスルツボに変形が認められなかった。 As can be seen from Table 1, the viscosity (11.0 poise or more), the thickness of the opaque layer (4 to 6), and the deflection rate of the opaque layer (within ± 15%) are all within the scope of the present invention. In Examples 1 to 4, the DF rate (single crystallization rate) was very good at 100%, and no deformation was observed in the silica glass crucible after use.
これに対して、不透明層の厚さが２と範囲の下限外の比較例１は、ＤＦ率が５０％と極めて悪く、口元の倒れ込み及びストレート部中央付近に軽い座屈変形が発生していた。不透明層の厚さが８と範囲の上限外の比較例２はＤＦ率が６０％と極めて悪く、シリカガラスルツボの口元位置が、カーボンサセプタよりも下に沈み込んでいた。不透明層のたわみ量率が１８％と上限外の比較例３は引き上げ初期にシリカガラスルツボ口元が内側に大きく倒れ込み、引き上げ不可能であり、ＤＦ率は０であった。不透明層のたわみ量率−１８％と下限外の比較例４はＤＦ率が３５％と極めて悪く、ストレート部中央付近に大きな座屈変形が発生していた。 On the other hand, the thickness of the opaque layer was 2 and the comparative example 1 outside the lower limit of the range had a very low DF ratio of 50%, and the buckling of the mouth and light buckling deformation occurred near the center of the straight part. . In Comparative Example 2 where the thickness of the opaque layer was 8 and outside the upper limit of the range, the DF ratio was extremely poor at 60%, and the mouth position of the silica glass crucible was sinking below the carbon susceptor. In Comparative Example 3 where the deflection amount of the opaque layer was 18%, which was outside the upper limit, the silica glass crucible mouth fell greatly inward at the initial stage of pulling, and pulling was impossible, and the DF ratio was 0. In the comparative example 4 where the deflection amount rate of the opaque layer was -18% and outside the lower limit, the DF rate was extremely poor at 35%, and a large buckling deformation occurred near the center of the straight portion.
１ シリカガラスルツボ
２ 透明層
３ 不透明層
1
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| US8673163B2 (en) | 2008-06-27 | 2014-03-18 | Apple Inc. | Method for fabricating thin sheets of glass |
| EP2404228B1 (en) | 2009-03-02 | 2020-01-15 | Apple Inc. | Techniques for strengthening glass covers for portable electronic devices |
| JP5047227B2 (en) * | 2009-05-27 | 2012-10-10 | ジャパンスーパークォーツ株式会社 | Silicon single crystal manufacturing method and silicon single crystal pulling apparatus |
| US9778685B2 (en) | 2011-05-04 | 2017-10-03 | Apple Inc. | Housing for portable electronic device with reduced border region |
| US9213451B2 (en) | 2010-06-04 | 2015-12-15 | Apple Inc. | Thin glass for touch panel sensors and methods therefor |
| US8824140B2 (en) | 2010-09-17 | 2014-09-02 | Apple Inc. | Glass enclosure |
| US10781135B2 (en) | 2011-03-16 | 2020-09-22 | Apple Inc. | Strengthening variable thickness glass |
| US9725359B2 (en) | 2011-03-16 | 2017-08-08 | Apple Inc. | Electronic device having selectively strengthened glass |
| US9128666B2 (en) | 2011-05-04 | 2015-09-08 | Apple Inc. | Housing for portable electronic device with reduced border region |
| US10133156B2 (en) | 2012-01-10 | 2018-11-20 | Apple Inc. | Fused opaque and clear glass for camera or display window |
| US8773848B2 (en) | 2012-01-25 | 2014-07-08 | Apple Inc. | Fused glass device housings |
| US9946302B2 (en) * | 2012-09-19 | 2018-04-17 | Apple Inc. | Exposed glass article with inner recessed area for portable electronic device housing |
| US9459661B2 (en) | 2013-06-19 | 2016-10-04 | Apple Inc. | Camouflaged openings in electronic device housings |
| JP6088666B2 (en) | 2013-12-28 | 2017-03-01 | 株式会社Sumco | Quartz glass crucible and manufacturing method thereof |
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