JP5846877B2 - Glass processing method and optical element manufacturing method - Google Patents
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- 239000011521 glass Substances 0.000 title claims description 163
- 230000003287 optical effect Effects 0.000 title claims description 48
- 238000004519 manufacturing process Methods 0.000 title claims description 28
- 238000003672 processing method Methods 0.000 title claims description 24
- 238000000034 method Methods 0.000 claims description 84
- 239000007788 liquid Substances 0.000 claims description 75
- 230000008569 process Effects 0.000 claims description 44
- 238000000465 moulding Methods 0.000 claims description 42
- 229910019142 PO4 Inorganic materials 0.000 claims description 37
- 239000000463 material Substances 0.000 claims description 35
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 34
- 239000010452 phosphate Substances 0.000 claims description 34
- 238000012545 processing Methods 0.000 claims description 26
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 24
- 229910052698 phosphorus Inorganic materials 0.000 claims description 24
- 239000011574 phosphorus Substances 0.000 claims description 24
- 238000004140 cleaning Methods 0.000 claims description 19
- 238000005406 washing Methods 0.000 claims description 15
- 239000005303 fluorophosphate glass Substances 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000007853 buffer solution Substances 0.000 claims description 6
- 238000010828 elution Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 239000006174 pH buffer Substances 0.000 claims 1
- 235000021317 phosphate Nutrition 0.000 description 32
- 238000005498 polishing Methods 0.000 description 24
- 230000008859 change Effects 0.000 description 18
- 230000004075 alteration Effects 0.000 description 13
- 239000006061 abrasive grain Substances 0.000 description 7
- 238000007654 immersion Methods 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000000156 glass melt Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000006060 molten glass Substances 0.000 description 5
- 241000239290 Araneae Species 0.000 description 4
- 238000003754 machining Methods 0.000 description 4
- 239000005304 optical glass Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- -1 Na 2 HPO 4 Chemical class 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000007667 floating Methods 0.000 description 3
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 3
- 239000005365 phosphate glass Substances 0.000 description 3
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000003384 imaging method Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000007517 polishing process Methods 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 241000511976 Hoya Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- DWYMPOCYEZONEA-UHFFFAOYSA-L fluoridophosphate Chemical compound [O-]P([O-])(F)=O DWYMPOCYEZONEA-UHFFFAOYSA-L 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
Landscapes
- Surface Treatment Of Glass (AREA)
- Cleaning By Liquid Or Steam (AREA)
Description
本発明はガラスの表面処理方法およびガラス製の光学素子の製造方法に関する。 The present invention relates to a glass surface treatment method and a glass optical element manufacturing method.
フツリン酸塩ガラスなどのリン酸塩含有ガラスは、光学レンズ、プリズム、光フィルターなどの光学素子の材料として有用であるものの、硬度が低く、化学的にも反応しやすいため、研磨精度に限界がある、研磨時間に長時間を要するといった問題がある。 Phosphate-containing glass such as fluorophosphate glass is useful as a material for optical elements such as optical lenses, prisms, and optical filters, but has low hardness and is easy to react chemically. There is a problem that the polishing time takes a long time.
このような問題を解決するための手段として、特許文献１に開示されている方法が提案されている。
この方法は、研磨液のｐHをガラスのｐHに近似させる操作を行い、その後に、この研磨液を使用してガラス表面を研磨し、ガラス表面の線状傷の幅を７μｍ以下に抑えたガラス製品を作製する。
As a means for solving such a problem, a method disclosed in Patent Document 1 has been proposed.
In this method, an operation is performed in which the pH of the polishing liquid is approximated to the pH of glass, and then the glass surface is polished using this polishing liquid, and the width of linear scratches on the glass surface is suppressed to 7 μm or less. Make a product.
ところで、近年の撮像機器の高精細化に伴い、極めて高品位な表面を有する光学素子が必要とされている。従来、ガラスの硬度が低いために研磨によって表面に生じた潜傷が、研磨液によって顕在化しないよう特許文献１に記載の方法を用いれば良かったが、光学機器の高精細化により、光学素子製造プロセスにおけるガラス表面の変質を防止する技術が必要になってきた。 By the way, with recent high-definition imaging devices, an optical element having an extremely high-quality surface is required. Conventionally, it was sufficient to use the method described in Patent Document 1 so that latent scratches generated on the surface due to polishing due to the low hardness of the glass would not be manifested by the polishing liquid. A technique for preventing the glass surface from being altered during the manufacturing process has become necessary.
本発明は上記問題を解決し、リン酸塩含有ガラスの表面変質を抑制しつつ、前記ガラスを精密加工または洗浄するガラスの処理方法を提供すること、および、前記処理方法を用いて高品位な表面を有するリン酸塩含有ガラス製の光学素子を製造する方法を提供することを目的とする。 The present invention solves the above problems, provides a glass processing method for precisely processing or cleaning the glass while suppressing surface alteration of the phosphate-containing glass, and high-quality using the processing method. It aims at providing the method of manufacturing the optical element made from the phosphate containing glass which has a surface.
上記課題を解決するにあたり、本件発明者は鋭意検討した結果、次の知見を得た。
（ｉ）研磨、洗浄で使用する液体のｐHは、ガラス表面の潜傷の潜在化に影響するものの
、単に、液体のｐH調整のみでガラス表面の変質を抑制することは困難である。
（ii）ガラス表面の変質は、リン酸塩含有ガラスのネットワークを構成するリン酸塩の鎖
状構造が液体によりアタックされ、リン酸塩が液体に溶出し、鎖状構造が破壊されることによって生じると考えられる。
（iii）リン酸塩の液体への溶出を抑制することができれば、ガラスの鎖状構造が維持され、表面変質を防止することが可能となる。
In order to solve the above-mentioned problems, the present inventor obtained the following knowledge as a result of intensive studies.
(I) Although the pH of the liquid used for polishing and cleaning affects the latent latent potential on the glass surface, it is difficult to suppress alteration of the glass surface simply by adjusting the pH of the liquid.
(Ii) The alteration of the glass surface is caused by the chain structure of the phosphate constituting the phosphate-containing glass network being attacked by the liquid, the phosphate eluting into the liquid, and the chain structure being destroyed. It is thought to occur.
(Iii) If elution of phosphate into the liquid can be suppressed, the chain structure of the glass can be maintained and surface alteration can be prevented.
以上の知見に基づき完成した本発明は、上記課題を解決するための手段として、
（１）リン酸塩含有ガラスの表面に液体を接触させて前記表面を精密加工する精密加工工程または液体を用いてリン酸塩含有ガラスを洗浄する洗浄工程の少なくとも一方の処理工程を備えるガラスの処理方法において、
予め前記液体にリン酸塩を溶解することにより、前記ガラス中のリン成分の前記液体への溶出を抑制しつつ、前記処理工程を行うことを特徴とするガラスの処理方法、
（２）前記処理工程後のガラス表面のヘイズが１％以下となるように、前記液体に溶解するリンの濃度を調整する上記（１）項に記載のガラスの処理方法、
（３）前記処理工程が洗浄工程であって、洗浄工程前後のガラスの質量変化量が０．０１％以下となるように、前記液体に溶解するリンの濃度を調整する上記（１）または（２）項に記載のガラスの処理方法、
（４）前記液体がｐＨの緩衝液であることを特徴とする上記（１）〜（３）項のいずれか１項に記載のガラスの処理方法
（５）フツリン酸塩ガラスを処理することを特徴とする上記（１）〜（４）項のいずれか１項に記載のガラスの処理方法、
（６）リン酸塩含有ガラスからなるプレス成形用ガラス素材の製造方法において、
上記（１）〜（５）項のいずれか１項に記載の方法によりガラスを処理する処理工程を備えるプレス成形用ガラス素材の製造方法、
（７）リン酸塩含有ガラスからなる光学素子の製造方法において、
上記（１）〜（５）項のいずれか１項に記載の方法によりガラスを処理する処理工程を備える光学素子の製造方法、
を提供する。
The present invention completed based on the above knowledge, as a means for solving the above problems,
(1) A glass comprising at least one processing step of a precision processing step in which a liquid is brought into contact with the surface of a phosphate-containing glass to precisely process the surface or a cleaning step in which the phosphate-containing glass is washed with a liquid. In the processing method,
A glass treatment method characterized by performing the treatment step while suppressing elution of the phosphorus component in the glass into the liquid by dissolving phosphate in the liquid in advance.
(2) The glass processing method according to (1), wherein the concentration of phosphorus dissolved in the liquid is adjusted so that the haze of the glass surface after the processing step is 1% or less,
(3) The treatment step is a washing step, and the concentration of phosphorus dissolved in the liquid is adjusted so that the mass change amount of the glass before and after the washing step is 0.01% or less (1) or ( The glass processing method according to item 2),
(4) The glass treatment method according to any one of (1) to (3) above, wherein the liquid is a pH buffer solution (5) treating a fluorophosphate glass. The glass processing method according to any one of the above items (1) to (4),
(6) In the manufacturing method of the glass material for press molding which consists of phosphate containing glass,
The manufacturing method of the glass raw material for press molding provided with the process process which processes glass by the method of any one of said (1)-(5) term,
(7) In the method for producing an optical element made of phosphate-containing glass,
The manufacturing method of an optical element provided with the process process of processing glass by the method of any one of said (1)-(5) term,
I will provide a.
本発明によれば、リン酸塩含有ガラスの表面変質を抑制しつつ、前記ガラスを精密加工または洗浄するガラスの処理方法を提供すること、および、前記処理方法を用いて高品位な表面を有するリン酸塩含有ガラス製の光学素子を製造する方法を提供することができる。 According to the present invention, it is possible to provide a glass processing method for precisely processing or cleaning the glass while suppressing surface alteration of the phosphate-containing glass, and to have a high-quality surface using the processing method. A method for producing an optical element made of phosphate-containing glass can be provided.
（ガラスの処理方法）
まず、本発明のガラスの処理方法について詳説する。
本発明のガラスの処理方法は、リン酸塩含有ガラスの表面に液体を接触させて前記表面を精密加工する精密加工工程または液体を用いてリン酸塩含有ガラスを洗浄する洗浄工程の少なくとも一方の処理工程を備えるガラスの処理方法において、
予め前記液体にリン酸塩を溶解することにより、前記ガラス中のリン成分の前記液体への溶出を抑制しつつ、前記処理工程を行うことを特徴とする。
(Glass processing method)
First, the glass processing method of the present invention will be described in detail.
The glass processing method according to the present invention includes at least one of a precision processing step in which a liquid is brought into contact with the surface of the phosphate-containing glass and the surface is precisely processed or a cleaning step in which the phosphate-containing glass is cleaned with the liquid. In the processing method of glass provided with a processing process,
It is characterized in that the treatment step is performed while suppressing elution of the phosphorus component in the glass into the liquid by dissolving phosphate in the liquid in advance.
前述のように、ガラス表面の変質はガラス中のリン成分がガラス表面から液体に溶出し、ガラスの鎖状構造が破壊されることによって生じると考えられる。そこで、ガラス中のリン成分が液体に溶出しないよう、予め液体にリン酸塩を溶解し、液体に溶解しているリンの濃度を高める。 As described above, the alteration of the glass surface is considered to be caused by the phosphorus component in the glass eluting from the glass surface into the liquid and the chain structure of the glass being destroyed. Therefore, in order to prevent the phosphorus component in the glass from eluting into the liquid, the phosphate is dissolved in the liquid in advance, and the concentration of phosphorus dissolved in the liquid is increased.
処理工程が精密加工工程の場合、液体は例えば加工液に相当する。精密加工工程としては、研磨工程、高精度な切削工程、研削工程などを例示することができる。研磨工程における加工液は、研磨液あるいは研磨スラリーとも呼ばれ、砥粒を含む液体、すなわち、研磨砥粒を分散させた液体である。また上記処理工程が洗浄工程の場合、液体は例えば洗浄液に相当する。 When the treatment process is a precision machining process, the liquid corresponds to, for example, a machining liquid. Examples of the precision machining process include a polishing process, a highly accurate cutting process, and a grinding process. The processing liquid in the polishing process is also called a polishing liquid or a polishing slurry, and is a liquid containing abrasive grains, that is, a liquid in which polishing abrasive grains are dispersed. Moreover, when the said process process is a washing | cleaning process, a liquid corresponds to a washing | cleaning liquid, for example.
加工液、例えば研磨液としては、ＣｅＯ2を主な砥粒とする市販の研磨材を水に分散した液等を使用することができる。 As the processing liquid, for example, a polishing liquid, a liquid obtained by dispersing a commercially available abrasive containing CeO 2 as main abrasive grains in water can be used.
加工液のリンの濃度を調整する物質としては、可溶性のリン酸塩、例えば、Ｎａ2ＨＰＯ4、ＮａＨ2ＰＯ4、Ｋ2ＨＰＯ4、ＫＨ2ＰＯ4等を使用すればよい。 Soluble phosphates such as Na 2 HPO 4 , NaH 2 PO 4 , K 2 HPO 4 , KH 2 PO 4, etc. may be used as substances for adjusting the concentration of phosphorus in the processing liquid.
洗浄液としては、軟硝材用の洗浄用として市販されている各種洗浄液や、純水に水溶性のリン酸塩を溶解した水溶液などを使用すればよい。 As the cleaning liquid, various cleaning liquids commercially available for cleaning soft glass materials, aqueous solutions in which water-soluble phosphates are dissolved in pure water, or the like may be used.
洗浄液中に溶解するリンの濃度を調整する物質としては、液体に対し可溶性のリン酸塩、例えば、Ｎａ2ＨＰＯ4、ＮａＨ2ＰＯ4、Ｋ2ＨＰＯ4、ＫＨ2ＰＯ4等を使用すればよい。 As a substance for adjusting the concentration of phosphorus dissolved in the washing liquid, phosphates soluble in the liquid, for example, Na 2 HPO 4 , NaH 2 PO 4 , K 2 HPO 4 , KH 2 PO 4, etc. may be used. Good.
上記加工液、洗浄液は、ｐＨの緩衝液としての役割も果たす。このようなｐＨの緩衝液を使用することにより、ガラスの処理に伴う液体のｐＨ変化が生じにくくなり、リン成分の溶出抑制効果をより安定的に得ることができる。 The processing solution and the cleaning solution also serve as a pH buffer solution. By using such a buffer solution having a pH, it becomes difficult to cause a pH change of the liquid accompanying the glass treatment, and the phosphorus component elution suppressing effect can be more stably obtained.
本発明の好ましい態様は、前記精密加工工程後のガラス表面のヘイズが１％以下（以下、ヘイズ基準値という）となるように、前記液体に溶解するリンの濃度を調整する方法である。 A preferred embodiment of the present invention is a method for adjusting the concentration of phosphorus dissolved in the liquid so that the haze of the glass surface after the precision processing step is 1% or less (hereinafter referred to as haze reference value).
ヘイズは、日本光学硝子工業会規格ＪＯＧＩＳの「光学ガラスの化学的耐久性の測定方法（表面法）０７-1975」のヘイズＨに相当し、前記規格で定められた方法によって測定される。ヘイズが１％以下の面とすることにより、前記面を光学機能面とし、高精細な光学機器に搭載可能な光学素子を得ることができる。なお、ヘイズ基準値を０．７％とすることが好ましく、０．５％とすることがより好ましい。なお、光学機能面として、光学素子の制御対象の光を屈折させる面、反射させる面、透過させる面、回折させる面などを例示することができる。 The haze corresponds to the haze H of “Measurement Method of Chemical Durability of Optical Glass (Surface Method) 07-1975” of Japan Optical Glass Industry Association Standard JOGIS, and is measured by the method defined in the above standard. By setting the haze to a surface of 1% or less, an optical element that can be mounted on a high-definition optical device by using the surface as an optical functional surface can be obtained. The haze reference value is preferably 0.7%, more preferably 0.5%. Examples of the optical function surface include a surface that refracts light to be controlled by the optical element, a surface that reflects light, a surface that transmits light, and a surface that diffracts light.
リンの濃度の調整は次のように行ってもよい。まず、リン酸塩溶液を作り、この溶液を使用して試験的に処理工程を行い、処理工程後のガラス表面のヘイズを測定する。ヘイズ測定値がヘイズ基準値よりも大きい場合、液体中に溶解するリンの濃度を高め、さらに試験的に処理工程を行い、ガラス表面のヘイズ測定を繰り返す。このようにしてヘイズがヘイズ基準値以下になった時点で、実際に処理工程で使用する液体に溶解するリン酸の濃度を決めてもよい。 The concentration of phosphorus may be adjusted as follows. First, a phosphate solution is prepared, a treatment process is performed on a trial basis using this solution, and the haze of the glass surface after the treatment process is measured. When the haze measurement value is larger than the haze reference value, the concentration of phosphorus dissolved in the liquid is increased, and further a treatment process is performed on a trial basis to repeat the haze measurement on the glass surface. In this way, when the haze becomes equal to or less than the haze reference value, the concentration of phosphoric acid that is actually dissolved in the liquid used in the treatment process may be determined.
本発明の好ましい他の態様は、前記処理工程が洗浄工程であって、洗浄工程前後のガラスの質量変化量が０．０１％以下（以下、質量変化量基準値という）となるように、前記液体に溶解するリンの濃度を調整する方法である。ガラスの質量変化量を質量変化量基準値以下にすることで、ガラス表面の変質をより確実に抑制することができる。 In another preferred embodiment of the present invention, the treatment step is a washing step, and the mass change amount of the glass before and after the washing step is 0.01% or less (hereinafter referred to as a mass change amount reference value). This is a method for adjusting the concentration of phosphorus dissolved in a liquid. By making the mass change amount of the glass equal to or less than the mass change amount reference value, it is possible to more reliably suppress the alteration of the glass surface.
質量変化量は、処理工程前のガラスの質量Ｍｂを精密に測定し、質量を測定したガラスを試験的に処理し、処理工程後の質量Ｍａを精密に測定し、（Ｍｂ−Ｍａ）／Ｍｂから求める。質量変化量が質量変化量基準値以下となった時点で、実際に処理工程で使用する液体中のリンの濃度、すなわち、液体に溶解するリンの濃度を決めてもよい。 The amount of mass change is determined by precisely measuring the mass Mb of the glass before the treatment step, treating the glass whose mass was measured experimentally, measuring the mass Ma after the treatment step, and (Mb−Ma) / Mb. Ask from. When the mass change amount becomes equal to or less than the mass change amount reference value, the concentration of phosphorus in the liquid actually used in the treatment process, that is, the concentration of phosphorus dissolved in the liquid may be determined.
なお、本発明における処理工程としては、精密加工工程のみでもよいし、洗浄工程のみでもよいし、精密加工工程および洗浄工程でもよい。なお、上記液体中においてリン酸塩含有ガラス製の光学素子を使用するという応用もある。このようにすることで、光学素子表面の変質を抑制することができる。 In addition, as a process process in this invention, only a precision processing process may be sufficient, a cleaning process only may be sufficient, and a precision processing process and a washing process may be sufficient. There is also an application in which an optical element made of phosphate-containing glass is used in the liquid. By doing in this way, alteration of the optical element surface can be suppressed.
リン酸塩含有ガラスの代表的なものは、モル％表示で、Ｐ2Ｏ5に換算したリンの含有量が、Ｂ2Ｏ3に換算したホウ素の含有量やＳｉＯ2に換算したケイ素の含有量よりも多いリン酸塩ガラスである。Ｐ2Ｏ5に換算したリンの含有量は、例えば１０％以上である。 The typical phosphate-containing glass is expressed in mol%, the phosphorus content converted to P 2 O 5 is the boron content converted to B 2 O 3 and the silicon content converted to SiO 2. More phosphate glass than the amount. The phosphorus content converted to P 2 O 5 is, for example, 10% or more.
リン酸塩ガラスの中でも、高屈折率高分散化のためにＮｂ2Ｏ5、ＴｉＯ2、Ｂｉ2Ｏ3およびＷＯ3を合計で１０モル％以上含有するガラスは、リン酸塩ガラスの中でも比較的、化学的耐久性が優れているが、Ｎｂ2Ｏ5、ＴｉＯ2、Ｂｉ2Ｏ3およびＷＯ3の合計含有量が１０モル％未満のガラスは化学的耐久性が低く、リン成分の液体への溶出がおきやすい。したがって、本発明は、Ｎｂ2Ｏ5、ＴｉＯ2、Ｂｉ2Ｏ3およびＷＯ3の合計含有量が１０モル％未満のリン酸塩含有ガラスの処理に好適である。 Among phosphate glasses, a glass containing Nb 2 O 5 , TiO 2 , Bi 2 O 3 and WO 3 in total of 10 mol% or more in order to achieve high refractive index and high dispersion is a comparison among phosphate glasses. Is excellent in chemical and chemical durability, but glass having a total content of Nb 2 O 5 , TiO 2 , Bi 2 O 3 and WO 3 of less than 10 mol% has low chemical durability and is a liquid of phosphorus component Elution is likely to occur. Therefore, the present invention is suitable for processing a phosphate-containing glass having a total content of Nb 2 O 5 , TiO 2 , Bi 2 O 3 and WO 3 of less than 10 mol%.
表面変質がおこりやすいガラスとしてフツリン酸塩ガラスがある。したがって、フツリン酸塩ガラスの処理に、本発明は特に好適である。 Fluorophosphate glass is a glass that easily undergoes surface alteration. Therefore, the present invention is particularly suitable for the treatment of fluorophosphate glass.
フツリン酸塩ガラスは、Ｐ5+以外にカチオン成分としてＡｌ3+、アルカリ金属、アルカリ土類金属などを含むことができる。 The fluorophosphate glass can contain Al 3+ , alkali metal, alkaline earth metal and the like as a cation component in addition to P 5+ .
また、フツリン酸塩ガラスに、近赤外線吸収剤としてＣｕイオンを添加し、近赤外線吸収フィルター用ガラスとしてもよい。 Moreover, it is good also as glass for near-infrared absorption filters by adding Cu ion as a near-infrared absorber to fluorophosphate glass.
精密加工工程の後、加工液がガラス表面に残存しないよう洗浄することが好ましく、この洗浄工程に本発明の処理方法を適用することが望ましい。 After the precision processing step, it is preferable to wash so that the processing liquid does not remain on the glass surface, and it is desirable to apply the treatment method of the present invention to this cleaning step.
洗浄工程後、液体がガラス表面に残存しないよう、ガラス表面を乾燥させることが望ましい。 After the cleaning process, it is desirable to dry the glass surface so that no liquid remains on the glass surface.
このようにして、フツリン酸塩ガラスからなるガラス物品を処理し、クモリ、ヤケなどの表面変質のないガラス物品を得ることができる。 In this way, a glass article made of a fluorophosphate glass can be processed to obtain a glass article free from surface alteration such as spider and burn.
ここでガラス物品としては、加熱、軟化、プレス成形してプレス成形品を作製するためのプレス成形用ガラス素材、あるいは、レンズ、プリズム、回折格子、ミラー、光学フィルターなどの各種の光学素子を例示することができる。 Here, examples of glass articles include glass materials for press molding for producing press-molded products by heating, softening, and press molding, or various optical elements such as lenses, prisms, diffraction gratings, mirrors, and optical filters. can do.
これらのガラス物品は、高品位な表面を有することが求められている。特に、光学機器の高精細化に伴い、光学素子には極めて高品位な光学機能面が求められている。本発明によれば、表面変質を防止し、高品位な面を有するガラス物品を処理する方法を提供することができる。 These glass articles are required to have a high quality surface. In particular, along with the increase in definition of optical equipment, optical elements are required to have extremely high quality optical functional surfaces. ADVANTAGE OF THE INVENTION According to this invention, the method of processing the glass article which prevents surface alteration and has a high quality surface can be provided.
（プレス成形用ガラス素材の製造方法）
次に本発明のプレス成形用ガラス素材の製造方法について詳説する。
(Method for producing glass material for press molding)
Next, the manufacturing method of the glass material for press molding of this invention is explained in full detail.
リン酸塩含有ガラスからなるプレス成形用ガラス素材の製造方法において、
上記ガラスの処理方法によりガラスを処理する処理工程を備えるプレス成形用ガラス素材の製造方法。
In the manufacturing method of the glass material for press molding made of phosphate-containing glass,
The manufacturing method of the glass raw material for press molding provided with the process process which processes glass with the said processing method of glass.
前述のように、プレス成形用ガラス素材は、加熱、軟化、プレス成形してプレス成形品を作製するためのガラス素材である。プレス成形用ガラス素材の中でも精密プレス成形に供されるガラス素材には、高品位な表面が求められる。精密プレス成形は、プレス成形によりダイレクトに光学素子を成形する方法で、プレス成形型の成形面をガラスに精密に転写し光学機能面を形成する方法である。プレス成形後、光学機能面を機械的に加工しないため、ガラス素材の表面が光学素子の表面として残る。表面が変質したガラス素材を精密プレス成形すると光学素子表面に変質層が残るため、精密プレス成形用ガラス素材（以下、プリフォームともいう。）の表面変質を抑制する必要がある。
通常の加工方法の場合、得られたガラス表面のリン成分濃度はガラス内部のリン濃度より低下するが、本方法による加工によって得られたガラス表面のリン成分濃度は変化が抑えられる特徴も有しており、安定したガラス特性を容易に得ることができる。
As described above, the glass material for press molding is a glass material for producing a press-molded product by heating, softening, and press molding. Among the glass materials for press molding, a glass material used for precision press molding requires a high-quality surface. Precision press molding is a method of directly molding an optical element by press molding, and is a method of precisely transferring a molding surface of a press mold to glass to form an optical functional surface. Since the optical functional surface is not mechanically processed after press molding, the surface of the glass material remains as the surface of the optical element. If a glass material having a modified surface is precision press-molded, a modified layer remains on the surface of the optical element, and therefore it is necessary to suppress surface modification of the glass material for precision press molding (hereinafter also referred to as a preform).
In the case of ordinary processing methods, the phosphorous component concentration on the glass surface obtained is lower than the phosphorous concentration inside the glass, but the phosphorous component concentration on the glass surface obtained by processing by this method also has the feature that the change can be suppressed. Therefore, stable glass characteristics can be easily obtained.
本発明のプレス成形用ガラス素材の製造方法によれば、上記本発明のガラスの処理方法により、リン酸塩含有ガラスを精密加工および／または洗浄するので、化学的耐久性の低いガラスでも表面変質のないプレス成形用ガラス素材を製造することができる。 According to the method for producing a glass material for press molding according to the present invention, the phosphate-containing glass is precisely processed and / or washed by the glass processing method according to the present invention. It is possible to produce a glass material for press molding without any material.
次に、プレス成形用ガラス素材を製造方法の態様について説明する。 Next, the aspect of the manufacturing method of the glass material for press molding is demonstrated.
第一の態様は、リン酸塩含有ガラスからなるガラス塊を研削、研磨してプレス成形用ガラス素材を製造する際、精密加工工程に相当する研磨工程に上記本発明の処理方法を用いる方法である。ガラス塊を丸め加工して球状化し、球状化したガラスの表面を研磨して球状ガラスを作製し、表面を洗浄し、その後に乾燥させて清浄な表面を有するプレス成形用ガラス素材を作製する。上記プロセスにおいて、研磨工程後のガラスの洗浄工程に、上記本発明の処理方法を用いてもよい。
なお、ガラス塊を丸め加工、球状化、洗浄後の乾燥については、公知の方法を用いればよい。
The first aspect is a method of using the processing method of the present invention in a polishing step corresponding to a precision processing step when a glass material for press molding is produced by grinding and polishing a glass lump made of phosphate-containing glass. is there. The glass lump is rounded to form a spheroid, the surface of the spheroidized glass is polished to produce a spherical glass, the surface is washed, and then dried to produce a glass material for press molding having a clean surface. In the above process, the processing method of the present invention may be used for the glass cleaning step after the polishing step.
In addition, what is necessary is just to use a well-known method about the rounding process of a glass lump, spheroidization, and drying after washing | cleaning.
第二の態様は、リン酸塩含有ガラスの融液を作製し、プレス成形用ガラス素材一個分に相当する量のガラス融液を、浮上させながらガラス素材に成形し、作製したガラス素材を上記本発明の処理方法により洗浄する方法である。
例えば、ガラス原料を熔融容器内に入れて、加熱、熔融し、得られた熔融物を清澄、均質化してガラス融液、すなわち、熔融ガラスを作製する。熔融容器に取り付けたガラス流出パイプからガラス融液を流出し、プレス成形用ガラス素材一個分に相当する量のガラス融液を公知の方法で分離する。分離して得た熔融ガラス塊を浮上しながら成形する際も、公知の方法を用いればよい。
In the second aspect, a phosphate-containing glass melt is prepared, and an amount of glass melt corresponding to one glass material for press molding is formed into a glass material while floating, and the produced glass material is the above This is a method of cleaning by the treatment method of the present invention.
For example, a glass raw material is put in a melting vessel, heated and melted, and the obtained melt is clarified and homogenized to produce a glass melt, that is, a molten glass. A glass melt is flowed out from a glass outflow pipe attached to a melting vessel, and an amount of glass melt corresponding to one glass material for press molding is separated by a known method. A known method may be used when forming the molten glass lump obtained by separation while floating.
上記方法によれば、熔融ガラス塊を浮上状態で成形するので、ガラス素材の全表面が自由表面となり、精密プレス成形用ガラス素材として好適なガラス素材を得ることができる。成形後、本発明の処理方法を用いてガラス素材を洗浄し、乾燥させた後、必要に応じてガラス素材の表面に炭素膜などをコートしてもよい。このような膜は、精密プレス成形の際、ガラスとプレス成形型との融着を防止し、ガラスがプレス成形面に沿って移動する際、潤滑層としての機能を果たす。 According to the said method, since a molten glass lump is shape | molded in a floating state, the whole surface of a glass raw material turns into a free surface, and a glass raw material suitable as a glass material for precision press molding can be obtained. After molding, the glass material may be washed and dried using the treatment method of the present invention, and then the surface of the glass material may be coated with a carbon film or the like as necessary. Such a film prevents fusion between the glass and the press mold during precision press molding, and functions as a lubricating layer when the glass moves along the press molding surface.
ガラス素材表面の変質を防止することにより、ガラス素材表面へのコートの付着性改善効果が得られる。また、ガラス素材表面の変質を防止することは、精密プレス成形の際、ガラスとプレス成形型との融着を防止する上からも好ましい。 By preventing alteration of the surface of the glass material, an effect of improving the adhesion of the coat to the surface of the glass material can be obtained. Moreover, it is preferable to prevent the surface of the glass material from being deteriorated from the viewpoint of preventing fusion between the glass and the press mold during precision press molding.
（光学素子の製造方法）
次に本発明の光学素子の製造方法について詳説する。
(Optical element manufacturing method)
Next, the manufacturing method of the optical element of the present invention will be described in detail.
本発明の光学素子の製造方法は、リン酸塩含有ガラスからなる光学素子の製造方法において、上記ガラスの処理方法によりガラスを処理する処理工程を備える光学素子の製造方法である。 The manufacturing method of the optical element of this invention is a manufacturing method of an optical element provided with the process process which processes glass by the processing method of the said glass in the manufacturing method of the optical element which consists of phosphate containing glass.
本発明の第一の態様は、光学素子の形状に近似する光学素子ブランクを成形し、該光学素子ブランクを少なくとも研磨する工程を備え、本発明の処理方法により前記研磨を行う方法である。光学素子ブランクの作製方法としては、熔融ガラス塊をプレス成形して作製する方法、プレス成形用ガラス素材を加熱、軟化し、プレス成形して作製する方法、ガラスブロックを機械加工して作製する方法などの公知の方法を例示することができる。上記研磨工程の後、得られた光学素子の洗浄を本発明の処理方法により行うことが、ガラス表面の変質を防止する上から好ましい。 A first aspect of the present invention is a method of forming an optical element blank that approximates the shape of an optical element, and at least polishing the optical element blank, and performing the polishing by the processing method of the present invention. As a method for producing an optical element blank, a method for producing a molten glass lump by press molding, a method for heating and softening a glass material for press molding, press molding, and a method for producing a glass block by machining Examples of such known methods can be given. After the polishing step, the obtained optical element is preferably washed by the treatment method of the present invention from the viewpoint of preventing the glass surface from being altered.
本発明の第二の態様は、プレス成形用ガラス素材を加熱し、該加熱したガラス素材を精密プレス成形して光学素子を作製し、本発明の処理方法により前記光学素子を洗浄する工程を有する方法である。精密プレス成形には公知の方法を用いればよい。 The second aspect of the present invention includes the steps of heating a glass material for press molding, producing an optical element by precision press molding the heated glass material, and washing the optical element by the processing method of the present invention. Is the method. A known method may be used for precision press molding.
これらの方法によれば、少なくとも光学機能面に変質のない光学素子を製造することができる。表面変質層のない光学素子は、高精細な撮像機器に搭載する光学素子に好適である。 According to these methods, it is possible to manufacture an optical element having at least no optical function change. An optical element having no surface-affected layer is suitable for an optical element mounted on a high-definition imaging device.
光学素子としては、レンズ、プリズム、回折格子、ミラー、光学フィルターを例示することができる。 Examples of the optical element include a lens, a prism, a diffraction grating, a mirror, and an optical filter.
光学素子には、必要に応じて、反射防止膜、全反射膜、部分反射膜などをコーティングしてもよい。なお、ガラス表面の変質がないので、付着性の良好なコーティングが可能である。 If necessary, the optical element may be coated with an antireflection film, a total reflection film, a partial reflection film, or the like. In addition, since there is no alteration of the glass surface, coating with good adhesion is possible.
（実施例１）
ＨＯＹＡ株式会社製のフツリン酸塩光学ガラス（硝種名FCD100）を直径４３．７ｍｍ、厚さ５ｍｍの円盤状に加工し、円盤状ガラスの対向する２つの平面を透明に研磨しサンプルを作製した。サンプルの質量を測定したところ、２６．４３４３ｇであった。また、サンプルの２つの平面のうち、一方の平面に所定の強度を有する光を垂直に入射させ、他方の平面から出射する光の強度を測定し、ヘイズを算出したところ、０．１％であった。
Ｎａ2ＨＰＯ4、ＮａＨ2ＰＯ4、Ｋ2ＨＰＯ4、ＫＨ2ＰＯ4などのリン酸塩を使用し、純水にリン酸塩を溶解し、水溶液を作製した。水溶液中のリン、ナトリウム、カリウムの濃度は、それぞれＰ：１６０ｐｐｍ、Ｎａ：１２５ｐｐｍ、Ｋ：８３ｐｐｍである。以下、この水溶液を液体Ａということにする。このように、液体Ａにはリンだけでなく、Ｎａ、Ｋといったアルカリ金属も溶解しているので、緩衝液として機能する。
５０℃に保った液体Ａに上記ガラスサンプルを１５時間浸漬（浸漬テスト）した後、乾燥させて、上記方法により質量とヘイズを測定したところ、液体浸漬後のサンプルの質量が２６．４３３８ｇ、ヘイズは０．３％であった。サンプルの質量変化量は０．００１９％と質量変化量基準値を大幅に下回った。
なお、液体Ａは緩衝液のｐＨは７．１である。
(Example 1)
A fluorophosphate optical glass (glass type name FCD100) manufactured by HOYA Corporation was processed into a disk shape having a diameter of 43.7 mm and a thickness of 5 mm, and two opposing flat surfaces of the disk-shaped glass were transparently polished to prepare a sample. It was 26.4343g when the mass of the sample was measured. In addition, light having a predetermined intensity is vertically incident on one of the two planes of the sample, the intensity of the light emitted from the other plane is measured, and the haze is calculated to be 0.1%. there were.
A phosphate such as Na 2 HPO 4 , NaH 2 PO 4 , K 2 HPO 4 , or KH 2 PO 4 was used, and the phosphate was dissolved in pure water to prepare an aqueous solution. The concentrations of phosphorus, sodium, and potassium in the aqueous solution are P: 160 ppm, Na: 125 ppm, and K: 83 ppm, respectively. Hereinafter, this aqueous solution is referred to as liquid A. As described above, since not only phosphorus but also alkali metals such as Na and K are dissolved in the liquid A, it functions as a buffer solution.
The glass sample was immersed in a liquid A maintained at 50 ° C. for 15 hours (immersion test) and then dried, and the mass and haze were measured by the above method. The mass of the sample after liquid immersion was 26.4338 g, haze. Was 0.3%. The mass change amount of the sample was 0.0019%, which was significantly lower than the mass change amount reference value.
The liquid A has a buffer solution pH of 7.1.
次に、この液体Ａに研磨砥粒として市販のＣｅＯ2を導入、分散させ、研磨液とし、上記フツリン酸塩ガラスと同種のガラスからなるレンズブランクを研磨して球面レンズとし、このレンズを液体Ａで十分洗浄した後、乾燥させ、ヘイズを測定したところ０．３％であった。このようにして、表面にクモリやヤケといった変質層のない高品位な表面を有するレンズを作製した。 Next, commercially available CeO 2 is introduced and dispersed in the liquid A as abrasive grains, and used as a polishing liquid. A lens blank made of the same kind of glass as the fluorophosphate glass is polished to form a spherical lens. After thoroughly washing with A, it was dried and the haze measured was 0.3%. In this way, a lens having a high-quality surface without an altered layer such as spider or burn was produced on the surface.
次いで、レンズ表面に反射防止膜をコートした。レンズ表面に変質層がないことから反射防止膜の付着性は良好であった。
なお、上記レンズブランクは、プレス成形用ガラス素材を加熱、軟化し、プレス成形型を用い、周知の方法でプレス成形して得られたものである。
Next, an antireflection film was coated on the lens surface. Since there was no deteriorated layer on the lens surface, the adhesion of the antireflection film was good.
The lens blank is obtained by heating and softening a glass material for press molding, and press molding by a well-known method using a press mold.
（実施例２）
実施例１で用いた光学ガラスと同種のフツリン酸塩ガラスからなるブロックを熔融ガラスから成形し、アニールした後、切断、研削して得たガラス片を球形状に研磨し、精密プレス成形用プリフォームを作製した。研磨には、液体Ａに砥粒として市販のＣｅＯ2を導入、分散させた研磨液を用いた。
研磨後、プリフォーム表面を液体Ａにより十分洗浄し、乾燥させた。プリフォーム表面にはクモリやヤケといった変質層は認められなかった。
(Example 2)
A block made of a fluorophosphate glass of the same type as the optical glass used in Example 1 is molded from molten glass, annealed, then cut and ground, and the glass piece obtained is polished into a spherical shape to obtain a precision press molding process. A reform was made. For polishing, a polishing liquid in which commercially available CeO 2 was introduced and dispersed in the liquid A as abrasive grains was used.
After polishing, the preform surface was sufficiently washed with liquid A and dried. Altered layers such as spiders and burns were not observed on the preform surface.
（実施例３）
実施例２において作製したプリフォームの表面にカーボン膜を形成し、加熱してプレス成形型を用いて精密プレス成形し、非球面レンズを作製した。精密プレス成形後、カーボン膜を酸化して除去した。
このようにして、表面にクモリやヤケといった変質層のない高品位な表面を有するレンズを作製した。またレンズは長期にわたって変質しないため、溶液中での使用も可能である。
(Example 3)
A carbon film was formed on the surface of the preform produced in Example 2, heated and precision press molded using a press mold to produce an aspheric lens. After precision press molding, the carbon film was oxidized and removed.
In this way, a lens having a high-quality surface without an altered layer such as spider or burn was produced on the surface. Further, since the lens does not change over a long period of time, it can be used in a solution.
次いで、レンズ表面に反射防止膜をコートした。レンズ表面に変質層がないことから反射防止膜の付着性は良好であった。 Next, an antireflection film was coated on the lens surface. Since there was no deteriorated layer on the lens surface, the adhesion of the antireflection film was good.
（比較例１）
純水にＮａＯＨを溶解したｐＨが７．８の水溶液（液体Ｂという）を使用した以外は、実施例１の浸漬テストと同様にしてサンプルの質量変化量とヘイズを測定した。質量変化量は０．０２２％、ヘイズは５２．１％であった。浸漬後のサンプル表面はヤケと呼ばれる変質層が一面に生じているのが目視により確認された。
液体Ｂに市販のＣｅＯ2砥粒を分散させた研磨液を使用し、上記ガラスと同種のガラスを研磨してレンズ形状に加工し、得られたレンズを液体Ｂにより洗浄、乾燥させた後、レンズ表面を観察したところ、ヤケと呼ばれる変質層が一面に生じていた。
(Comparative Example 1)
The amount of change in mass and haze of the sample were measured in the same manner as in the immersion test of Example 1, except that an aqueous solution (referred to as liquid B) having a pH of 7.8 in which NaOH was dissolved in pure water was used. The amount of mass change was 0.022%, and the haze was 52.1%. It was confirmed by visual observation that the surface of the sample after immersion had a deteriorated layer called burn.
After using a polishing liquid in which commercially available CeO 2 abrasive grains are dispersed in liquid B, polishing the same kind of glass as the glass and processing it into a lens shape, and washing and drying the obtained lens with liquid B, When the lens surface was observed, an altered layer called a burn was formed on one side.
（比較例２）
ｐＨ６．８のＨＮＯ3水溶液（液体Ｃという）を使用した以外は、実施例１の浸漬テストと同様にしてサンプルの質量変化量とヘイズを測定した。質量変化量は０．０２４％、ヘイズは５１．６％であった。浸漬後のサンプル表面はヤケと呼ばれる変質層が一面に生じているのが目視により確認された。
液体Ｃに市販のＣｅＯ2砥粒を分散させた研磨液を使用し、上記ガラスと同種のガラスを研磨してレンズ形状に加工し、得られたレンズを液体Ｃにより洗浄、乾燥させた後、レンズ表面を観察したところ、ヤケと呼ばれる変質層が一面に生じていた。
(Comparative Example 2)
The amount of change in mass and haze of the sample were measured in the same manner as in the immersion test of Example 1 except that an aqueous HNO 3 solution having pH 6.8 (referred to as liquid C) was used. The amount of mass change was 0.024%, and the haze was 51.6%. It was confirmed by visual observation that the surface of the sample after immersion had a deteriorated layer called burn.
Using a polishing liquid in which commercially available CeO 2 abrasive grains are dispersed in liquid C, polishing the same type of glass as the above glass and processing into a lens shape, and washing and drying the resulting lens with liquid C, When the lens surface was observed, an altered layer called a burn was formed on one side.
Claims (6)
前記ガラスはフツリン酸塩ガラスであり、かつ、前記液体はｐＨの緩衝液であり、
予め前記液体にリン酸塩を溶解することにより、前記ガラス中のリン成分の前記液体への溶出を抑制しつつ、前記処理工程を行うことを特徴とするガラスの処理方法。 In a glass processing method comprising at least one processing step of a precision processing step in which a liquid is brought into contact with a surface of a glass containing phosphate and the glass is cleaned with a liquid using a precision processing step.
The glass is a fluorophosphate glass, and the liquid is a pH buffer;
A method for treating glass, wherein the treatment step is performed while suppressing elution of a phosphorus component in the glass into the liquid by dissolving phosphate in the liquid in advance.
請求項１〜４のいずれか１項に記載の方法により前記ガラスを処理する処理工程を備えるプレス成形用ガラス素材の製造方法。 The method of manufacturing a glass material for press molding comprising a glass containing a phosphate,
The manufacturing method of the glass raw material for press molding provided with the process process which processes the said glass by the method of any one of Claims 1-4 .
請求項１〜４のいずれか１項に記載の方法により前記ガラスを処理する処理工程を備える光学素子の製造方法。 In the method for manufacturing an optical element made of glass which contains a phosphate,
The manufacturing method of an optical element provided with the process process which processes the said glass by the method of any one of Claims 1-4 .
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