JPH0432018B2 - - Google Patents
Info
- Publication number
- JPH0432018B2 JPH0432018B2 JP17732586A JP17732586A JPH0432018B2 JP H0432018 B2 JPH0432018 B2 JP H0432018B2 JP 17732586 A JP17732586 A JP 17732586A JP 17732586 A JP17732586 A JP 17732586A JP H0432018 B2 JPH0432018 B2 JP H0432018B2
- Authority
- JP
- Japan
- Prior art keywords
- glass
- less
- content
- oxygen
- ppm
- 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
Links
- 239000011521 glass Substances 0.000 claims description 43
- 239000007789 gas Substances 0.000 claims description 13
- 229910052760 oxygen Inorganic materials 0.000 claims description 13
- 239000006060 molten glass Substances 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 229910018068 Li 2 O Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 description 13
- 239000000126 substance Substances 0.000 description 10
- 238000002834 transmittance Methods 0.000 description 8
- 230000007423 decrease Effects 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- 238000010309 melting process Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 150000002823 nitrates Chemical class 0.000 description 3
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000004031 devitrification Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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
- C03C3/12—Silica-free oxide glass compositions
- C03C3/16—Silica-free oxide glass compositions containing phosphorus
- C03C3/17—Silica-free oxide glass compositions containing phosphorus containing aluminium or beryllium
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)
Description
〔発明の目的〕
（産業上の利用分野）
本発明は一般のカメラおよびVTRカメラ等の
色補正用フイルタガラスに使用される近赤外線吸
収ガラスおよびその製造方法に関する。
（従来の技術）
従来、一般のカメラおよびVTRカメラ等の色
補正用フイルタガラスに適用されるリン酸塩系近
赤外線吸収ガラスは、原料の一部にH3PO4を用
いるが、これが溶融過程において分解して
2H3PO4→P2O5＋3H2Oとなる。このP2O5はガラ
ス網目を形成し、H2Oは気体となつて外部へ放
出されるが、H2Oの一部はガラス内に残存して
含水ガラスとなる。この残存したH2Oはガラス
網目を切断し、ガラス構造を弱くして耐水性など
の化学的耐久性を低下させる。この化学的耐久性
が弱いため、フイルタガラスは使用時間の経過に
伴い表面が風化現象を生じ、透過率特性が著しく
低下する。
また、CuO成分の原料としてCu2+イオンの結
合状態のものを用いる。ガラスの高温溶融時に
Cu2+イオンはエネルギー状態の安定なCu+イオン
へ移行しやすくなる。Cu2+イオンがCu+イオンへ
移行すると、ガラスは400nｍ付近の透過率が低
下してしまう。この対策として原料中に硝酸塩や
硫酸塩を導入し、溶融過程で硝酸塩や硫酸塩が分
解し、酸素を発生させて酸化雰囲気を醸成し、
Cu2+イオンがCuu+イオンへ移行するのを防止す
る。しかし、この方法では硝酸塩や硫酸塩の分解
反応が、原料溶融工程におけるバツチフリーの状
態までに終了してしまい、ガラスを清澄、均質化
する工程では酸素の放出がなくなり、Cu2+イオ
ンの一部がCu+イオンへ移行し、可視光の短波長
側の透過率が低下する。
（発明が解決しようとする問題点）
本発明は上記事情を考慮してなされたもので、
400nｍ付近の波長域を効率よく透過し、近赤外
線のシヤープカツト特性が良好で、かつすぐれた
化学的耐久性を有する近赤外線吸収ガラスおよび
その製造方法を提供することを目的とする。
〔発明の構成〕
（問題点を解決するための手段）
本発明は上記の目的を達成するために、ガラス
溶融工程において酸素を含む乾燥気体を溶融ガラ
ス中に導入することにより、ガラス中のH2O含
有率を100ppm以下に制限し、かつCu2+イオンを
安定化したものである。すなわち、重量百分率で
P2O555〜85％、Ａ2O35〜15％、CaO，MgO，
BaO，ZnOの１種または２種以上の合量２〜15
％、Li2O，Na2O，K2Oの合量0.1〜８％、
CuO0.2〜10％を含み、かつH2Oの含有率が
100ppm以下となる近赤外線吸収ガラスである。
また前記組成からなるガラスを溶融する工程にお
いて、15モル％の酸素を含み、かつH2Oの含有
率が100ppm以下となる乾燥気体を溶融ガラス中
に導入することを特徴とする近赤外線吸収ガラス
の製造方法である。前記乾燥気体は誘爆性・有毒
性の気体を除けば特に限定されないが一般に不活
性の気体が適当している。
本発明のガラス組成を前記範囲に限定した理由
を説明する。
P2O5はガラス網目を構成する主成分であるが
55％未満では波長400nｍ付近の透過率が低下し、
85％超えると化学的耐久性が低下する。
Al2O3はガラスの化学的耐久性を向上させるた
めの不可欠の成分であるが、５％未満では化学的
耐久性が劣化し、15％を超えると紫外域の透過率
が低下し、かつガラスの溶融性が悪化する。
CaO，MgO，BaO，ZnOはその１種または２
種以上の合量が、２％未満では化学的耐久性が低
下し、かつ成形性がわるくなり、15％を超えると
CuO成分による赤外線シヤープカツト性能を阻害
する。Li2O，Na2O，K2Oはその合量が８％を超
えると化学的耐久性が著しく低下する。
CuOは着色剤として添加され近赤外線シヤープ
カツトのための必須成分であるが、0.2％未満で
は近赤外線の十分な吸収効果が得られず、10％を
超えるとガラスの安定性が低下し失透現象をおこ
す。
本発明のガラスは1050〜1450℃の温度で溶融す
るが、1050℃以下ではガラスの粘度が高く十分な
溶融、脱泡が行なわれず、1450℃を超えるとガラ
スの各成分が揮発しやすくなりガラスが不均質と
なる。溶融時に溶融ガラスに導入する乾燥気体の
酸素含有率が15モル％未満では、十分な酸化雰囲
気を確保することができない。
（作 用）
ガラス溶融工程において、酸素を15モル％以上
含み、かつH2Oの含有率が100ppm以下なる乾燥
気体を溶融ガラス中に導入することにより、溶融
ガラス中に入つた酸素によつてCu2+イオンがCu+
イオンへ移行することなく安定し、近赤外線のシ
ヤープカツト特性と可視域の短波長側の透過率が
向上する。さらに、溶融ガラス中に溶存している
H2Oが排出され、ガラス構造内に取り込まれる
H2Oが減少して化学的耐久性が向上する。
（実施例）
本発明の実施例について、図面に示すガラス溶
融装置を参照して説明する。
炉体１内の基台２上には溶融ガラス３を収容す
る石英るつぼ４が載置され、石英るつぼ４の外周
には加熱用電気抵抗ヒータ５が配設されている。
炉体１の側壁を貫通して石英るつぼ４内の溶融ガ
ラス３に挿入された石英ガラス製導管６は、炉外
側において酸素と窒素との混合気体供給装置（図
示しない）に連結されている。このように構成さ
れたガラス溶融装置において、重量百分率で
P2O560〜80％、Al2O311〜15％、CaO＋MgO1〜
10％、BaO0〜５％、ZnO0〜２％、
Li2O＋Na2O＋K2O0.5〜７％、CuO0.5〜８％の
組成となるように調合されたバツチを石英るつぼ
４に収容し、電気抵抗ヒータ５に通電して加熱
し、1350℃または1400℃の温度で５時間溶融す
る。この溶融開始２時間後に酸素を20〜40モル％
含有した窒素との混合気体を、供給装置から導管
６を介して溶融ガラス３中に、毎分0.5の速度
で１時間または毎分１の速度で、30分間導入す
る。H2Oを含まない気体を得るために、液体酸
素および液体窒素から生成された気体を使用し、
混合気体のH2O含有率は100ppm以下に調整す
る。
このようにして得られた本発明ガラスを次表に
示す。表中、ガラス組成は重量百分率で示し、耐
水性は日本光学硝子工業会法によつて示す。また
700nｍの透過率は肉厚１mmのガラス試料を用い
て測定し、H2Oの含有率は赤外分光透過率にて
−OH基の吸収量から求めた。
[Object of the Invention] (Industrial Application Field) The present invention relates to a near-infrared absorbing glass used for color correction filter glass in general cameras and VTR cameras, and a method for manufacturing the same. (Prior art) Phosphate-based near-infrared absorbing glass, which is conventionally applied to color correction filter glass for general cameras and VTR cameras, uses H 3 PO 4 as a part of the raw material, but this disassembled in
2H 3 PO 4 →P 2 O 5 +3H 2 O. This P 2 O 5 forms a glass network, and H 2 O is released as a gas to the outside, but a portion of the H 2 O remains within the glass and becomes hydrous glass. This remaining H 2 O cuts the glass network, weakening the glass structure and reducing chemical durability such as water resistance. Due to this weak chemical durability, the surface of the filter glass undergoes a weathering phenomenon over time, resulting in a significant decrease in transmittance characteristics. Further, as a raw material for the CuO component, one in which Cu 2+ ions are bonded is used. During high temperature melting of glass
Cu 2+ ions are more likely to transition to Cu + ions, which have a stable energy state. When Cu 2+ ions shift to Cu + ions, the transmittance of glass in the vicinity of 400 nm decreases. As a countermeasure to this, nitrates and sulfates are introduced into the raw materials, and during the melting process, the nitrates and sulfates decompose, generating oxygen and creating an oxidizing atmosphere.
Prevents Cu 2+ ions from migrating to Cuu + ions. However, in this method, the decomposition reaction of nitrates and sulfates is completed before the batch-free state is reached in the raw material melting process, and in the glass fining and homogenization process, no oxygen is released, and some of the Cu 2+ ions are removed. transfers to Cu + ions, and the transmittance of visible light on the short wavelength side decreases. (Problems to be solved by the invention) The present invention has been made in consideration of the above circumstances, and
The object of the present invention is to provide a near-infrared absorbing glass that efficiently transmits wavelengths around 400 nm, has good near-infrared sharp cutting characteristics, and has excellent chemical durability, and a method for producing the same. [Structure of the Invention] (Means for Solving the Problems) In order to achieve the above object, the present invention introduces a dry gas containing oxygen into the molten glass in the glass melting process, thereby reducing H in the glass. 2 O content is limited to 100 ppm or less and Cu 2+ ions are stabilized. i.e. in weight percentage
P2O5 55-85 %, A2O3 5-15 %, CaO, MgO,
Total amount of one or more of BaO and ZnO 2 to 15
%, total amount of Li 2 O, Na 2 O, K 2 O 0.1 to 8%,
Contains CuO0.2~10% and H2O content
It is a near-infrared absorbing glass with less than 100 ppm.
Further, in the step of melting the glass having the above composition, a drying gas containing 15 mol% of oxygen and having a H 2 O content of 100 ppm or less is introduced into the molten glass. This is a manufacturing method. The drying gas is not particularly limited except for explosive or toxic gases, but inert gases are generally suitable. The reason why the glass composition of the present invention is limited to the above range will be explained. P 2 O 5 is the main component that makes up the glass network.
If it is less than 55%, the transmittance around the wavelength of 400nm will decrease,
If it exceeds 85%, chemical durability decreases. Al 2 O 3 is an essential component for improving the chemical durability of glass, but if it is less than 5%, the chemical durability deteriorates, and if it exceeds 15%, the transmittance in the ultraviolet region decreases, and Glass meltability deteriorates. CaO, MgO, BaO, ZnO are one or two of them.
If the total amount is less than 2%, chemical durability and moldability will deteriorate, and if it exceeds 15%,
Inhibits infrared sharp cut performance by CuO component. If the total amount of Li 2 O, Na 2 O, and K 2 O exceeds 8%, the chemical durability will be significantly reduced. CuO is added as a colorant and is an essential component for near-infrared sharp cutting, but if it is less than 0.2%, a sufficient near-infrared absorption effect cannot be obtained, and if it exceeds 10%, the stability of the glass decreases and devitrification occurs. cause The glass of the present invention melts at a temperature of 1,050 to 1,450°C, but below 1,050°C, the glass has a high viscosity and sufficient melting and defoaming cannot be achieved, and when the temperature exceeds 1,450°C, each component of the glass easily volatizes, making the glass becomes heterogeneous. If the oxygen content of the dry gas introduced into the molten glass during melting is less than 15 mol%, a sufficient oxidizing atmosphere cannot be secured. (Function) In the glass melting process, by introducing a dry gas containing 15 mol% or more of oxygen and a H 2 O content of 100 ppm or less into the molten glass, the oxygen that has entered the molten glass is Cu 2+ ion becomes Cu +
It is stable without transferring to ions, and improves near-infrared sharp cut characteristics and short wavelength transmittance in the visible range. Furthermore, dissolved in the molten glass
H2O is expelled and incorporated into the glass structure
H 2 O is reduced and chemical durability is improved. (Example) An example of the present invention will be described with reference to a glass melting apparatus shown in the drawings. A quartz crucible 4 containing molten glass 3 is placed on a base 2 within the furnace body 1, and an electric resistance heater 5 for heating is arranged around the outer periphery of the quartz crucible 4.
A quartz glass conduit 6, which penetrates the side wall of the furnace body 1 and is inserted into the molten glass 3 in the quartz crucible 4, is connected to an oxygen and nitrogen gas mixture supply device (not shown) outside the furnace. In a glass melting apparatus configured in this way, the weight percentage
P2O5 60 ~80%, Al2O3 11 ~15%, CaO+MgO1~
A batch prepared to have a composition of 10%, BaO 0 to 5%, ZnO 0 to 2%, Li 2 O + Na 2 O + K 2 O 0.5 to 7%, and CuO 0.5 to 8% is placed in a quartz crucible 4, The electric resistance heater 5 is energized to heat it and melt at a temperature of 1350°C or 1400°C for 5 hours. 2 hours after the start of this melting, add 20 to 40 mol% of oxygen.
A gas mixture containing nitrogen is introduced from a feed device via conduit 6 into the molten glass 3 at a rate of 0.5 per minute for 1 hour or at a rate of 1 per minute for 30 minutes. To obtain a gas free of H 2 O, use a gas produced from liquid oxygen and liquid nitrogen,
The H 2 O content of the mixed gas is adjusted to 100 ppm or less. The glass of the present invention thus obtained is shown in the following table. In the table, the glass composition is shown in weight percentage, and the water resistance is shown in accordance with the Japan Optical Glass Industry Association method. Also
The transmittance at 700 nm was measured using a glass sample with a wall thickness of 1 mm, and the H 2 O content was determined from the amount of absorption of -OH groups in the infrared spectral transmittance.
以上のように本発明は、所定の組成を有するガ
ラスを溶融する工程において、酸素を15モル％以
上含み、かつH2Oの含有率が100ppm以上なる乾
燥気体を溶融ガラス中に導入することによりガラ
ス中のH2Oの含有率100ppm以下に制限しかつ
Cu2+イオンを安定化したリン酸塩系近赤外線吸
収ガラスおよびその製造方法であり、可視線の短
波長域を効率よく透過し、近赤外線のシヤープカ
ツト特性を向上させ、かつすぐれた化学的耐久性
を有するガラスが得られるものである。
As described above, in the process of melting glass having a predetermined composition, the present invention involves introducing a dry gas containing 15 mol% or more of oxygen and a H 2 O content of 100 ppm or more into the molten glass. Limit the content of H 2 O in glass to 100 ppm or less and
Phosphate-based near-infrared absorbing glass with stabilized Cu 2+ ions and its manufacturing method.It efficiently transmits visible light in the short wavelength range, improves near-infrared sharp cut characteristics, and has excellent chemical durability. A glass having properties can be obtained.
図面は本発明に係るガラス溶融装置の例を示す
断面図である。
３……溶融ガラス、４……石英るつぼ、６……
導管。
The drawing is a sectional view showing an example of a glass melting apparatus according to the present invention. 3... Molten glass, 4... Quartz crucible, 6...
conduit.
Claims (1)
％、CaO，MgO，BaO，ZnOの１種または２種
以上の合量２〜15％、Li2O，Na2O，K2Oの合量
0.1〜８％、CuO0.2〜10％を含み、かつH2Oの含
有率が100ppm以下なる近赤外線吸収ガラス。 ２ 前記組成からなるガラスを溶融する工程にお
いて、15モル％以上の酸素を含み、かつH2Oの
含有率100ppm以下なる乾燥気体を溶融ガラス中
に導入することを特徴とする近赤外線吸収ガラス
の製造方法。 ３ 前記乾燥気体が不活性の気体である特許請求
の範囲第２項記載の近赤外線吸収ガラスの製造方
法。[Claims] 1. In weight percentage, P 2 O 5 55-85%, Al 2 O 3 5-15
%, total amount of one or more of CaO, MgO, BaO, ZnO 2-15%, total amount of Li 2 O, Na 2 O, K 2 O
A near-infrared absorbing glass containing 0.1 to 8% CuO, 0.2 to 10% CuO, and a H 2 O content of 100 ppm or less. 2. A near-infrared absorbing glass characterized in that, in the step of melting the glass having the above composition, a dry gas containing 15 mol% or more of oxygen and having a H 2 O content of 100 ppm or less is introduced into the molten glass. Production method. 3. The method for producing near-infrared absorbing glass according to claim 2, wherein the drying gas is an inert gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17732586A JPS6335434A (en) | 1986-07-28 | 1986-07-28 | Near infrared absorption glass and production thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17732586A JPS6335434A (en) | 1986-07-28 | 1986-07-28 | Near infrared absorption glass and production thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6335434A JPS6335434A (en) | 1988-02-16 |
| JPH0432018B2 true JPH0432018B2 (en) | 1992-05-28 |
Family
ID=16029001
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17732586A Granted JPS6335434A (en) | 1986-07-28 | 1986-07-28 | Near infrared absorption glass and production thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6335434A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007051055A (en) * | 2005-07-19 | 2007-03-01 | Ohara Inc | Optical glass |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03109234A (en) * | 1989-09-19 | 1991-05-09 | Hoya Corp | Near infrared ray and infrared ray absorbing glass |
| DE4031469C1 (en) * | 1990-10-05 | 1992-02-06 | Schott Glaswerke, 6500 Mainz, De | |
| JPH04193740A (en) * | 1990-11-22 | 1992-07-13 | Agency Of Ind Science & Technol | Porous glass carrier for fixing enzyme |
| TWI276611B (en) | 2000-08-17 | 2007-03-21 | Hoya Corp | Process for producing glass and glass-melting apparatus thereof |
| KR20170139010A (en) * | 2015-04-24 | 2017-12-18 | 아사히 가라스 가부시키가이샤 | Near infrared cut-off filter glass |
| DE102017207253B3 (en) | 2017-04-28 | 2018-06-14 | Schott Ag | filter glass |
-
1986
- 1986-07-28 JP JP17732586A patent/JPS6335434A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007051055A (en) * | 2005-07-19 | 2007-03-01 | Ohara Inc | Optical glass |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6335434A (en) | 1988-02-16 |
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