JP2814805B2 - Quartz glass substrate for polysilicon TFT LCD - Google Patents
Quartz glass substrate for polysilicon TFT LCDInfo
- Publication number
- JP2814805B2 JP2814805B2 JP3327149A JP32714991A JP2814805B2 JP 2814805 B2 JP2814805 B2 JP 2814805B2 JP 3327149 A JP3327149 A JP 3327149A JP 32714991 A JP32714991 A JP 32714991A JP 2814805 B2 JP2814805 B2 JP 2814805B2
- Authority
- JP
- Japan
- Prior art keywords
- quartz glass
- glass substrate
- temperature
- less
- polysilicon tft
- 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.)
- Expired - Fee Related
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/06—Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2201/00—Glass compositions
- C03C2201/06—Doped silica-based glasses
- C03C2201/08—Doped silica-based glasses containing boron or halide
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2201/00—Glass compositions
- C03C2201/06—Doped silica-based glasses
- C03C2201/20—Doped silica-based glasses containing non-metals other than boron or halide
- C03C2201/23—Doped silica-based glasses containing non-metals other than boron or halide containing hydroxyl groups
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Compositions (AREA)
- Liquid Crystal (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、ポリシリコンＴＦＴ式
ＬＣＤ用石英ガラス基板に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a quartz glass substrate for a polysilicon TFT type LCD.
【０００２】[0002]
【従来の技術】石英ガラスは、透明なガラス材料の中で
は最も耐熱性が高く、また熱膨張率が極めて小さく寸法
安定性に優れていること、更に化学的な耐久性に優れて
いることのために、近年、ポリシリコンＴＦＴ式ＬＣＤ
用の基板材料として、特にビデオカメラのビューファイ
ンダー等に用いられる小型のポリシリコンＴＦＴ用とし
て用いられている。ポリシリコンＴＦＴの製造方法は一
般的には、製造温度レベルにより、（１）高温プロセス
法（最高プロセス温度約１０００℃程度）、（２）中温
プロセス法（最高プロセス温度約７００℃程度）、
（３）低温プロセス法（最高プロセス温度約５００℃程
度）の３種類に大別される。2. Description of the Related Art Quartz glass has the highest heat resistance among transparent glass materials, has a very small coefficient of thermal expansion, has excellent dimensional stability, and has excellent chemical durability. Recently, polysilicon TFT type LCD
Used as a substrate material for small-sized polysilicon TFTs used in viewfinders of video cameras and the like. In general, polysilicon TFTs are manufactured in the following manners depending on the manufacturing temperature level: (1) high-temperature process (maximum process temperature of about 1000 ° C.);
(3) It is roughly classified into three types: a low-temperature process method (a maximum process temperature of about 500 ° C.).
【０００３】一般的に、テレビやディスプレー等の大面
積ＴＦＴの場合、製造コスト面からプロセスの低温化の
方向での開発が、現在盛んに進められている。ところが
一方、ビデオカメラのビューファインダー用等の小型の
ポリシリコンＴＦＴについては、高温プロセスを採用し
た場合、従来のＬＳＩ製造ラインを大幅に変更すること
無く製造することができるため、ＬＳＩ製造で培われた
信頼性の高いプロセス技術を有効活用でき、高歩留まり
で高品質のＴＦＴを製造できるメリットが有るため、高
温プロセスでの製造が主流となっている。In general, in the case of large-area TFTs such as televisions and displays, developments in the direction of lowering the process are being actively pursued from the viewpoint of manufacturing costs. On the other hand, small polysilicon TFTs for video camera viewfinders and the like can be manufactured without significant changes in conventional LSI manufacturing lines when a high-temperature process is adopted. In addition, there is a merit that a high-reliability process technology can be effectively used and a high-quality TFT can be manufactured with a high yield. Therefore, a high-temperature process is mainly used.
【０００４】この場合の問題点は、基板材料であるガラ
スの耐熱性にあり、かかる観点から石英ガラスが用いら
れるのが通常である。しかしながら、石英ガラスの耐熱
性も、その種類・製造方法によりかなり差異を有してお
り、一般的にはいわゆる溶融石英ガラスが耐熱性という
観点からは最も優れており、徐冷点（ガラスの粘度が１
０13ポアズを示す温度）で１１７０〜１２２０℃程度で
ある。A problem in this case is the heat resistance of glass as a substrate material, and quartz glass is usually used from such a viewpoint. However, the heat resistance of the quartz glass is also best has a viscosity of annealing point (glass has a considerable difference is generally so-called fused silica glass from the viewpoint of heat resistance by the type and manufacturing method Is 1
0 13 is approximately 1,170-1,220 ° C. in temperature) which indicates the port A's.
【０００５】これに対し、合成石英ガラスからなる基板
は、ガラス中に含まれる泡・異物等の品質面からははる
かに優れているが、一方、一般に合成石英ガラスの徐冷
点は１０５０〜１１２０℃程度であって溶融石英ガラス
に比較し１００〜１５０℃程度低く、耐熱性がより低い
ので、ポリシリコンＴＦＴ製造上合成石英ガラスからな
る基板には問題があった。On the other hand, a substrate made of synthetic quartz glass is far superior in terms of the quality of bubbles and foreign matter contained in the glass, but the annealing point of synthetic quartz glass is generally 1050 to 1050. 1120 ° C. about a was compared to fused silica 10 0 to 0.99 ° C. about low, since the lower heat resistance, there is a problem in a substrate made of polysilicon TFT manufacturing synthetic silica glass.
【０００６】また、一般に石英ガラスは、ＴＦＴ製造工
程等で用いられるプラズマエッチング等の真空紫外光の
照射によって、２３０〜３００ｎｍの波長範囲に吸収を
伴う構造欠陥を生成することが知られている。これらの
構造欠陥の中には蛍光発光を伴うものがあり、これらの
蛍光発光のためにカラー液晶表示素子を作成した場合に
は色調を損ねるといった実用上の問題を有していた。Further, it is generally known that quartz glass generates structural defects accompanied by absorption in a wavelength range of 230 to 300 nm by irradiation with vacuum ultraviolet light such as plasma etching used in a TFT manufacturing process or the like. Some of these structural defects are accompanied by fluorescent light emission, and when a color liquid crystal display element is produced for such fluorescent light emission, there is a practical problem that the color tone is impaired.
【０００７】[0007]
【発明が解決しようとする課題】本発明の目的は、前述
の問題点を解消し、ビューファインダー等に用いられる
ポリシリコンＴＦＴ式ＬＣＤ製造用に適した、耐熱性に
優れ、蛍光発光の実質的に無いポリシリコンＴＦＴ式Ｌ
ＣＤ用石英ガラス基板を提供するにある。The object of the present invention is to solve the above is to solve the problems described above, suitable for a polysilicon TFT type LCD production used in the viewfinder over like, excellent in heat resistance, substantial fluorescence emission Polysilicon TFT type L
It is to provide a quartz glass substrate for CD.
【０００８】[0008]
【課題を解決するための手段】本発明は前述の課題を解
決するべくなされたものであり、ハロゲン含有量が１０
ｐｐｍ以下、ＯＨ含有量が１００ｐｐｍ以下、重金属お
よびアルカリ金属の含有量の総計が１ｐｐｍ以下であっ
て、徐冷点が１１５０℃以上であることを特徴とするポ
リシリコンＴＦＴ式ＬＣＤ用石英ガラス基板を提供する
ものである。SUMMARY OF THE INVENTION The present invention has been made to solve the above-mentioned problems, and has a halogen content of 10%.
ppm or less, an OH content of 100 ppm or less, a total content of heavy metals and alkali metals of 1 ppm or less, and a slow cooling point of 1150 ° C. or more. To provide.
【０００９】また本発明は、上記ポリシリコンＴＦＴ式
ＬＣＤ用石英ガラス基板において、基板面内の屈折率の
変動幅が５×１０-6以下であることを特徴とするポリシ
リコンＴＦＴ式ＬＣＤ用石英ガラス基板を提供するもの
である。The present invention also provides a quartz glass substrate for a polysilicon TFT type LCD, wherein the variation range of the refractive index in the substrate surface is 5 × 10 -6 or less. A glass substrate is provided.
【００１０】また本発明は、上記ポリシリコンＴＦＴ式
ＬＣＤ用石英ガラス基板において、該石英ガラス基板を
プラズマエッチング処理したとき、該処理の前後での波
長２３０〜３００ｎｍの範囲の吸光係数の増加が、０．
００５ｃｍ-1以下であることを特徴とするポリシリコン
ＴＦＴ式ＬＣＤ用石英ガラス基板を提供するものであ
る。Further, the present invention provides the above-mentioned quartz glass substrate for a polysilicon TFT type LCD, wherein when the quartz glass substrate is subjected to plasma etching treatment, an increase in the extinction coefficient in a wavelength range of 230 to 300 nm before and after the treatment is caused by: 0.
An object of the present invention is to provide a quartz glass substrate for a polysilicon TFT type LCD, which is not more than 005 cm -1 .
【００１１】本発明において、石英ガラス基板に含有さ
れるハロゲン量は、１０ｐｐｍ以下であり、１０ｐｐｍ
を超えるハロゲンが含有される場合には、耐熱性が低下
する。また、ＯＨ含有量は、１００ｐｐｍ以下であり、
特には５０ｐｐｍ以下であることが好ましい。１００ｐ
ｐｍを超えるＯＨ量を含有する場合には、ハロゲンと同
じく耐熱性が低下する。[0011] In the present invention, the halogen content contained in the quartz glass substrate state, and are less 10 ppm, 10 ppm
If more than halogen is contained, heat resistance decreases
I do . In addition, OH content of state, and are less than 100ppm,
In particular, it is preferably at most 50 ppm. 100p
When containing OH content of more than pm, like heat resistance is lowered and a halogen.
【００１２】重金属およびアルカリ金属の含有量につい
ては、その総和が１ｐｐｍ以下であり、１ｐｐｍを超え
て含有する場合には、短波長領域での分光透過率の低下
をもたらす。また、徐冷点とはガラスの粘度が１０13 ポ
アズを示す温度であるが、これは１１５０℃以上であ
り、かかる温度以上の徐冷点を有すれば、ポリシリコン
ＴＦＴ作成上のプロセス温度としておよそ１０００℃を
採用することが可能となる。[0012] For the content of heavy metals and the alkali metals, the sum Ri der below 1ppm, when content exceeds 1ppm is to cod also a decrease in the spectral transmittance in a short wavelength region. The viscosity of the glass is the annealing point 10 13 po
Is a temperature showing the as-which 1150 ° C. or higher der
Ri, if it has more than such a temperature of the anneal point, that Do is possible to employ a roughly 1000 ° C. As the process temperature on the creation polysilicon TFT.
【００１３】また、光学的な均質性を得るためには、面
内の屈折率の変動幅が５×１０-6以下であることが好ま
しい。かかる変動幅を超える場合には、光学的な均質性
を確保することが困難となるため好ましくない。Further, in order to obtain optical homogeneity, it is preferable that the variation range of the in-plane refractive index is 5 × 10 −6 or less. Exceeding such a fluctuation range is not preferable because it becomes difficult to ensure optical homogeneity.
【００１４】また、前記プラズマエッチング処理前後で
の波長２３０〜３００ｎｍの範囲の吸光係数の増加は、
０．００５ｃｍ-1以下であることが好ましい。ここに、
吸光係数αは、透過光量をＩ、入射光量をＩo 、反射率
をＲ、ガラス基板の厚みをｔ（ｃｍ）とした時に、 Ｉ／Ｉo ＝（１−Ｒ）2 ・ｅｘｐ（−α・ｔ） で定義される値である。The increase in the extinction coefficient in the wavelength range of 230 to 300 nm before and after the plasma etching treatment is as follows:
It is preferably 0.005 cm -1 or less. here,
The extinction coefficient α is I / I o = (1−R) 2 · exp (−α), where I is the amount of transmitted light, I o is the amount of incident light, R is the reflectance, and t (cm) is the thickness of the glass substrate. -The value defined by t).
【００１５】ここに、吸光係数の増加が、０．００５ｃ
ｍ-1以下であれば、これに伴う蛍光発光も、入射光量の
１０万分の１から１００万分の１程度となり、実用上の
問題を生じない。かかる範囲を逸脱する場合には、色調
の変化や着色等を引き起こし好ましくない。Here, the increase in the extinction coefficient is 0.005 c
If it is less than m −1 , the resulting fluorescence emission will also be about 1 / 100,000 to 1 / 100,000 of the incident light amount, and will not cause a practical problem. When departing from the above range is not preferable cause pull the color change or coloring or the like.
【００１６】かかる石英ガラス基板の製造方法として
は、上記の項目を満足していれば特に制約はないが、例
えば、予めガラス形成原料を加熱加水分解して得られる
石英ガラス微粒子を基材に堆積・成長させた多孔質石英
ガラス体を透明ガラス化する温度以下の温度域で水蒸気
分圧の低い雰囲気中に一定時間加熱保持した後、透明ガ
ラス化温度に昇温加熱して透明ガラス化して石英ガラス
体とする方法により作成することが可能である。The method of manufacturing such a quartz glass substrate is not particularly limited as long as the above-mentioned items are satisfied. For example, quartz glass fine particles obtained by heating and hydrolyzing a glass-forming raw material are previously deposited on a substrate.・ After heating and maintaining the grown porous quartz glass body in an atmosphere with a low partial pressure of water vapor for a certain period of time in a temperature range not higher than the temperature at which the vitreous quartz is vitrified, the temperature is raised to the vitrification temperature and heated to clear vitrification to form quartz. It can be made by a method of forming a glass body.
【００１７】用いられるガラス形成原料としては、ガス
化可能な原料であれば特に制限されるものではないが、
ＳｉＣｌ4 、ＳｉＨＣｌ3 、ＳｉＨ2 Ｃｌ2 、Ｓｉ（Ｃ
Ｈ3）Ｃｌ3 等の塩化物、ＳｉＦ4 、ＳｉＨＦ3 、Ｓｉ
Ｈ2 Ｆ2 等のフッ化物、ＳｉＢｒ4 、ＳｉＨＢｒ3 等の
臭化物、ＳｉＩ4 の沃化物等のハロゲン化珪素化合物が
作業性やコストの面から好ましい。多孔質石英ガラス体
は、これらのガラス形成原料を通常の酸水素火炎中で加
水分解し、基材上に堆積させて形成される。このように
して得られた多孔質石英ガラス体は、ついで低水蒸気分
圧雰囲気下で一定時間加熱保持された後、透明ガラス化
温度まで昇温されて透明ガラス化して石英ガラスとな
る。The glass forming raw material used is not particularly limited as long as it is a gasizable raw material.
SiCl 4 , SiHCl 3 , SiH 2 Cl 2 , Si (C
H 3 ) chlorides such as Cl 3 , SiF 4 , SiHF 3 , Si
Fluoride such as H 2 F 2 , bromide such as SiBr 4 and SiHBr 3 , and silicon halide compound such as iodide of SiI 4 are preferable in terms of workability and cost. The porous quartz glass body is formed by hydrolyzing these glass forming raw materials in an ordinary oxyhydrogen flame and depositing them on a substrate. The porous quartz glass body thus obtained is then heated and held for a certain period of time in a low steam partial pressure atmosphere, and then heated to a transparent vitrification temperature to be vitrified to form quartz glass.
【００１８】すなわち、例えば、多孔質石英ガラス体は
雰囲気制御可能な電気炉内に予め装着された後、一定の
昇温速度で加熱される。ついで所定の温度に到達の後、
乾燥ガスを雰囲気中に導入し、多孔質石英ガラス体が接
する雰囲気を置換することにより雰囲気中の水蒸気分圧
を所定値以下に低減させる。その水蒸気分圧としては、
０．００２ｍｍＨｇ以下であることが好ましく、これを
超える場合には最終的に得られる石英ガラス中のＯＨ量
を低減させることが困難なため好ましくない。That is, for example, after the porous quartz glass body is previously mounted in an electric furnace whose atmosphere can be controlled, it is heated at a constant heating rate. Then, after reaching the predetermined temperature,
By introducing a dry gas into the atmosphere and replacing the atmosphere in contact with the porous quartz glass body, the partial pressure of water vapor in the atmosphere is reduced to a predetermined value or less. As the water vapor partial pressure,
Preferably 0.002mmHg or less, it
If it exceeds, it is not preferable because it is difficult to reduce the OH content in the finally obtained quartz glass.
【００１９】また加熱保持する温度域としては、８００
〜１２５０℃の範囲内が好ましく、この温度域未満の温
度では実質的な効果が得られず、またこの温度域を超え
る温度では多孔質石英ガラス体の表面の透明ガラス化が
進行するため、多孔質石英ガラス体内部を所望の低水蒸
気分圧雰囲気に置換することができず好ましくない。The temperature range for heating and holding is 800
Is preferably in the range of to 1250 ° C., no substantial effect is obtained at temperatures below this temperature range, also exceed this temperature range
That since at temperatures vitrification of the surface of the porous quartz glass body proceeds is not preferable not possible to replace the porous quartz glass body portion to a desired low water vapor partial pressure atmosphere.
【００２０】また、この温度域であれば、加熱処理の方
法としては、一定温度に保持してもよく、またこの温度
域内を所定の時間の範囲内で昇温させながら処理しても
よい。またこの温度域での保持時間は、保持温度に依存
するため一概に規定することはできないが１〜３０時間
程度が好ましく、これ未満の場合には、実質的な効果が
なく、またこれより長時間かけた場合にもその効果は変
わらないために生産効率等を考慮に入れると好ましくな
い。Further, if this temperature range, as the method of heat treatment, rather it may also be held at a constant temperature, also be treated while warming the temperature range within a predetermined time
Not good. Also, the holding time in this temperature range depends on the holding temperature and cannot be specified unconditionally, but is preferably about 1 to 30 hours, and if it is less than this, there is no substantial effect and the holding time is longer. Even if it takes time, the effect does not change, so it is not preferable to take production efficiency and the like into consideration.
【００２１】また、乾燥ガスとしては、窒素、ヘリウ
ム、アルゴン等を通常用いることができるが、乾燥ガス
として使用できれば必ずしもこれらのガスに限定される
ものではない。ついでこのような加熱処理の後、多孔質
石英ガラス体は透明ガラス化温度まで昇温されて透明ガ
ラス化される。透明ガラス化温度としては、１３５０〜
１５００℃の範囲から採用することが好ましい。更に、
加熱処理と透明ガラス化処理は、それぞれ別の加熱装置
で行われてもよいが、その場合には、移送時に水分が吸
着したりすることを防止する等の処置を講じることが好
ましい。したがって、さらに好ましい実施態様として
は、加熱処理とガラス化を同一の設備で行うことが好ま
しい。As the dry gas, nitrogen, helium, argon or the like can be usually used, but it is not necessarily limited to these gases as long as it can be used as the dry gas. Then, after such heat treatment,
Quartz glass body is transparent glass <br/> las reduction is heated to a transparent vitrification temperature. The transparent vitrification temperature is 1350-
It is preferable to adopt from the range of 1500 ° C. Furthermore,
Heat treatment and vitrification process, it may also be carried out in separate heating devices bur, in that case, it is preferable to take measures such as water at the time of transfer to prevent or adsorption. Therefore, as a more preferred embodiment, it is preferable to perform the heat treatment and the vitrification in the same facility.
【００２２】こうして得られた石英ガラス体を軟化点以
上の温度に加熱し、所望の形状に成形加工を行い石英ガ
ラスインゴットを製造する。成形加工の温度域は、１６
５０〜１８００℃の範囲から選択することが好ましい。
１６５０℃未満の温度では石英ガラスの粘度が高いた
め、実質的に自重変形が行われず、またＳｉ０2 の結晶
相であるクリストバライトの成長がおこりいわゆる失透
が生じるため好ましくなく、１８００℃を超える温度で
は、ＳｉＯ2 の昇華が無視できなくなり好ましくない。
また、石英ガラス体の自重変形を行わせる方向は、特に
規定されないが多孔質石英ガラス体の成長方向と同一で
あることが好ましい。The quartz glass body thus obtained is heated to a temperature equal to or higher than the softening point and formed into a desired shape to produce a quartz glass ingot. The temperature range of the forming process is 16
It is preferable to select from the range of 50 to 1800 ° C.
At a temperature lower than 1650 ° C., the viscosity of quartz glass is high, so that its own weight is not substantially deformed, and cristobalite, which is a crystal phase of SiO 2 , grows and so-called devitrification occurs. In this case, sublimation of SiO 2 cannot be ignored, which is not preferable.
The direction in which the quartz glass body undergoes its own weight deformation is not particularly limited, but is preferably the same as the growth direction of the porous quartz glass body.
【００２３】こうして得られる石英ガラスインゴット
は、さらに研削加工、スライス加工、研磨加工を経て、
基板とされる。なお、透過率の改善のために、必要に応
じてスライスした基板を水素を含む雰囲気中で熱処理し
てもよい。The quartz glass ingot thus obtained is further subjected to grinding, slicing, and polishing.
It is a substrate. In order to improve the transmittance, but it may also be heat-treated substrate sliced if necessary in an atmosphere containing hydrogen.
【００２４】以上のような工程を経て得られる石英ガラ
スは、石英ガラス中に含有されるＯＨ量が１００ｐｐｍ
以下であり、該ガラス中のＯＨ量の変動幅がほとんどの
領域において±５ｐｐｍ以内であって均質性に優れる石
英ガラスである。The quartz glass obtained through the above steps has an OH content of 100 ppm in the quartz glass.
Or less, a silica glass having excellent homogeneity is within ± 5 ppm variation width of the OH content is have you to most areas of the glass.
【００２５】また、本発明の石英ガラスは、ガラス形成
原料として高純度な合成原料が使用可能なこと、溶融工
程を経ないためルツボ等からの不純物の混入がないこと
等から、鉄、ニッケル等の重金属元素やナトリウム、カ
リウム等のアルカリ金属元素の不純物総量が１ｐｐｍ以
下と極めて高純度であり、これをポリシリコンＴＦＴ製
造用に供した場合、高温処理を経ても不純物がシリコン
膜その他の部位に拡散してその部位を劣化させることが
ない。In addition, the quartz glass of the present invention can be used as a raw material for forming a glass, because a high-purity synthetic raw material can be used and no impurities are mixed in from a crucible because it does not go through a melting step. The total amount of impurities of heavy metal elements and alkali metal elements such as sodium and potassium is extremely high as 1 ppm or less, and when this is used for the production of polysilicon TFTs, the impurities remain in the silicon film and other parts even after high temperature treatment. It does not diffuse and degrade the site .
【００２６】以下、本発明の詳細についてさらに実施例
により説明するが、当然のことながら本発明の内容はこ
れら実施例に限定されるものではない。Hereinafter, the present invention will be described in further detail with reference to Examples, but it goes without saying that the present invention is not limited to these Examples.
【００２７】[0027]
【実施例】［実施例１］ 公知の方法により、ＳｉＣｌ4 を酸水素火炎中で加熱加
水分解させて形成した直径３５ｃｍ、長さ１００ｃｍの
多孔質石英ガラス体を室温で雰囲気制御可能な電気炉内
に設置した。ついで露点温度−７０℃の窒素ガスで電気
炉内雰囲気を置換した後、露点温度−７０℃の窒素ガス
を流しながら５００℃／ｈｒの昇温速度で１０００℃ま
で昇温した。EXAMPLES Example 1 By a known method, a porous quartz glass body having a diameter of 35 cm and a length of 100 cm formed by heating and hydrolyzing SiCl 4 in an oxyhydrogen flame can control the atmosphere at room temperature. Installed in the furnace. Then, after replacing the atmosphere in the electric furnace with a nitrogen gas having a dew point of -70 ° C, the temperature was raised to 1000 ° C at a rate of 500 ° C / hr while flowing a nitrogen gas having a dew point of -70 ° C.
【００２８】引き続き昇温速度を５０℃／ｈｒとし、１
２５０℃まで昇温して、その温度で１０ｈｒ保持した。
こうして得られた熱処理済みの多孔質石英ガラス体を透
明ガラス化のための炉内最高温度が１４５０℃に制御さ
れた電気炉内上部に設置し、炉内を露点温度が−７０℃
のヘリウムガスで置換した後、８０ｃｍ／ｈｒの速度で
下降させながら最高温度域を通過させて透明ガラス化を
行った。Subsequently, the temperature was raised at a rate of 50 ° C./hr.
The temperature was raised to 250 ° C. and maintained at that temperature for 10 hours.
The heat-treated porous quartz glass body thus obtained is placed in an upper part of an electric furnace controlled at a maximum furnace temperature of 1450 ° C. for transparent vitrification, and the furnace has a dew point temperature of −70 ° C.
After the helium gas was replaced with the helium gas, the glass was passed through the highest temperature range while being lowered at a speed of 80 cm / hr to perform vitrification.
【００２９】こうして得られた透明石英ガラスを、カー
ボン製発熱体を有する電気炉内で、軟化点以上の１７５
０℃に加熱して自重変形を行わせ、１７０ｍｍφ×４０
０ｍｍの円柱インゴット形状に成形した。こうして得ら
れた石英ガラスインゴットの長手方向の中心部より、１
７０ｍｍφ×５７ｍｍの石英ガラスインゴットを切り出
し、形状を揃えるために円筒研削を行い、１６０ｍｍφ
とした後、精密干渉計（ＺｙｇｏIV）により屈折率分布
を評価した。The transparent quartz glass thus obtained was placed in an electric furnace having a heating element made of carbon at a temperature of 175 ° C. or above the softening point.
Heat to 0 ° C to deform under its own weight, 170 mm φ × 40
It was formed into a 0 mm cylindrical ingot shape. From the center in the longitudinal direction of the quartz glass ingot thus obtained, 1
70 mm cut out quartz glass ingot phi × 57 mm, subjected to cylindrical grinding to align the shape, 160 mm phi
After that, the refractive index distribution was evaluated using a precision interferometer (Zygo IV).
【００３０】またＯＨ量およびその分布は、１７０ｍｍ
φ×４００ｍｍ石英ガラスインゴットより屈折率分布を
評価した部分のすぐ隣の場所より、２ｍｍ厚みのガラス
板を切り出し日本分光社製簡易ＦＴＩＲ装置により３７
００ｃｍ-1の吸収により定量した。Ｃｌ含有量は得られ
た石英ガラスをアルカリ溶融したのち、イオンクロマト
グラフィー法により定量した。また、徐冷点は、サンプ
ルサイズ２．４ｍｍ×５ｍｍ×６０ｍｍのサンプルを切
り出し、スパン５２ｍｍで、ビームベンディング法によ
り測定した。結果を表１に示す。The OH content and its distribution are 170 mm
A glass plate having a thickness of 2 mm was cut out from a place immediately adjacent to the portion where the refractive index distribution was evaluated from a φ × 400 mm quartz glass ingot, and was cut out with a simple FTIR apparatus manufactured by JASCO Corporation.
Quantified by absorption at 00 cm -1 . The Cl content was determined by ion chromatography after melting the obtained quartz glass with alkali. The annealing point was measured by cutting out a sample having a sample size of 2.4 mm × 5 mm × 60 mm and measuring the span at 52 mm by the beam bending method. Table 1 shows the results.
【００３１】また、上記の石英ガラスインゴットからサ
ンプルを切り出し、１００％水素雰囲気中で１０００
℃、１４時間の熱処理をした後、研磨して３０ｍｍの厚
さに整えた後透過率を測定した。ついで、東京応化製ド
ライエッチャー（Ｓ−６００）を用い、酸素／四塩化炭
素プラズマ（０．３５ｔｏｒｒ、２００Ｗ）中で５分間
のプラズマエッチング処理を行い、透過率を測定した。
プラズマエッチング処理前後での２３０〜３００ｎｍの
範囲での透過率の減少は０．５％であり、この値から換
算して吸光係数の増加は、０．００２ｃｍ-1であった。Further, a sample was cut out from the above quartz glass ingot and 1000% in a 100% hydrogen atmosphere.
After heat treatment at 14 ° C. for 14 hours, the resultant was polished to a thickness of 30 mm, and the transmittance was measured. Next, using a dry etcher (S-600) manufactured by Tokyo Ohka, a plasma etching treatment was performed in oxygen / carbon tetrachloride plasma (0.35 torr, 200 W) for 5 minutes, and the transmittance was measured.
The decrease in transmittance in the range of 230 to 300 nm before and after the plasma etching treatment was 0.5%, and the increase in the extinction coefficient calculated from this value was 0.002 cm -1 .
【００３２】［実施例２］ 実施例１と同一の方法で作成した石英ガラスインゴット
からサンプルを切りだし、水素雰囲気の水素濃度が３０
％であること以外は実施例１と同様の後処理を行い、プ
ラズマエッチング前後での透過率の変化を測定したとこ
ろ、透過率の減少は１％であり、この値から換算して吸
光係数の増加は０．００４ｃｍ-1であった。Example 2 A sample was cut out from a quartz glass ingot prepared in the same manner as in Example 1, and the hydrogen concentration in a hydrogen atmosphere was 30%.
%, The same post-treatment as in Example 1 was performed, and the change in transmittance before and after plasma etching was measured. The decrease in transmittance was 1%. The increase was 0.004 cm -1 .
【００３３】［比較例］ １２５０℃での熱処理を行わないほかは、実施例１と同
一の方法で作製した石英ガラスインゴットの屈折率分
布、ＯＨ量およびその分布幅、Ｃｌ含有量、および徐冷
点を表１に示す。Comparative Example A refractive index distribution, an OH content and its distribution width, a Cl content, and a slow cooling of a quartz glass ingot produced by the same method as in Example 1 except that the heat treatment at 1250 ° C. was not performed. The points are shown in Table 1.
【００３４】[0034]
【表１】 [Table 1]
【００３５】[0035]
【発明の効果】上述したように、本発明のポリシリコン
ＴＦＴ式ＬＣＤ用石英ガラス基板は、徐冷点が高く、耐
熱性に優れ、かつプラズマエッチング処理前後での短波
長側の吸光係数の増加が小さく、実質的に蛍光発光が無
い優れた特徴を有する。また、本発明のポリシリコンＴ
ＦＴ式ＬＣＤ用石英ガラス基板は光学的均質性にも優れ
た特徴を有する。[Effect of the Invention] As described above, polysilicon TFT type quartz glass substrate for an LCD of the present invention, high anneal points, excellent heat resistance, and the absorption light coefficient in the short wavelength side of the before and after plasma etching process It has excellent characteristics with little increase and substantially no fluorescence emission. Also, the polysilicon T of the present invention
The quartz glass substrate for the FT type LCD has a feature excellent in optical homogeneity.
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.6，ＤＢ名) C03C 3/06 G02F 1/1333 500──────────────────────────────────────────────────続 き Continued on front page (58) Field surveyed (Int. Cl. 6 , DB name) C03C 3/06 G02F 1/1333 500
Claims (3)
有量が１００ｐｐｍ以下、重金属およびアルカリ金属の
含有量の総計が１ｐｐｍ以下であって、徐冷点が１１５
０℃以上であることを特徴とするポリシリコンＴＦＴ式
ＬＣＤ用石英ガラス基板。1. A halogen content of 10 ppm or less, an OH content of 100 ppm or less, a total content of heavy metals and alkali metals of 1 ppm or less, and a slow cooling point of 115 ppm.
A quartz glass substrate for a polysilicon TFT type LCD, wherein the temperature is 0 ° C. or higher.
ガラス基板において、基板面内の屈折率の変動幅が５×
１０-6以下であることを特徴とするポリシリコンＴＦＴ
式ＬＣＤ用石英ガラス基板。2. The quartz glass substrate for a polysilicon TFT according to claim 1, wherein a variation width of the refractive index in the substrate surface is 5 ×.
Polysilicon TFT characterized by being 10 -6 or less
Quartz glass substrate for LCD.
Ｔ式ＬＣＤ用石英ガラス基板において、該石英ガラス基
板をプラズマエッチング処理したとき、該処理の前後で
の波長２３０〜３００ｎｍの範囲の吸光係数の増加が、
０．００５ｃｍ-1以下であることを特徴とするポリシリ
コンＴＦＴ式ＬＣＤ用石英ガラス基板。3. The polysilicon TF according to claim 1, wherein
In a quartz glass substrate for a T-type LCD, when the quartz glass substrate is subjected to plasma etching treatment, an increase in the extinction coefficient in a wavelength range of 230 to 300 nm before and after the treatment,
A quartz glass substrate for a polysilicon TFT type LCD, having a thickness of 0.005 cm -1 or less.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3327149A JP2814805B2 (en) | 1991-11-15 | 1991-11-15 | Quartz glass substrate for polysilicon TFT LCD |
| US07/912,776 US5330941A (en) | 1991-07-24 | 1992-07-13 | Quartz glass substrate for polysilicon thin film transistor liquid crystal display |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3327149A JP2814805B2 (en) | 1991-11-15 | 1991-11-15 | Quartz glass substrate for polysilicon TFT LCD |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05139775A JPH05139775A (en) | 1993-06-08 |
| JP2814805B2 true JP2814805B2 (en) | 1998-10-27 |
Family
ID=18195861
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3327149A Expired - Fee Related JP2814805B2 (en) | 1991-07-24 | 1991-11-15 | Quartz glass substrate for polysilicon TFT LCD |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2814805B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6376401B1 (en) | 1998-09-07 | 2002-04-23 | Tosoh Corporation | Ultraviolet ray-transparent optical glass material and method of producing same |
-
1991
- 1991-11-15 JP JP3327149A patent/JP2814805B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05139775A (en) | 1993-06-08 |
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