JP2608758B2 - Method for producing titanium oxide thin film forming material - Google Patents
Method for producing titanium oxide thin film forming materialInfo
- Publication number
- JP2608758B2 JP2608758B2 JP63122602A JP12260288A JP2608758B2 JP 2608758 B2 JP2608758 B2 JP 2608758B2 JP 63122602 A JP63122602 A JP 63122602A JP 12260288 A JP12260288 A JP 12260288A JP 2608758 B2 JP2608758 B2 JP 2608758B2
- Authority
- JP
- Japan
- Prior art keywords
- acid
- thin film
- titanium oxide
- oxide thin
- film forming
- 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
- 239000010409 thin film Substances 0.000 title claims description 19
- 239000000463 material Substances 0.000 title claims description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims description 17
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims description 15
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 150000007524 organic acids Chemical class 0.000 claims description 14
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims description 12
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 235000005985 organic acids Nutrition 0.000 claims description 4
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 3
- 235000015165 citric acid Nutrition 0.000 claims description 3
- 239000004310 lactic acid Substances 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 3
- 239000011976 maleic acid Substances 0.000 claims description 3
- 239000001630 malic acid Substances 0.000 claims description 3
- 235000011090 malic acid Nutrition 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 description 12
- 239000010408 film Substances 0.000 description 10
- 239000000499 gel Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 229910010413 TiO 2 Inorganic materials 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 238000003618 dip coating Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229920000298 Cellophane Polymers 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910001854 alkali hydroxide Inorganic materials 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/003—Compounds containing elements of Groups 4 or 14 of the Periodic Table without C-Metal linkages
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Coating Of Shaped Articles Made Of Macromolecular Substances (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Surface Treatment Of Glass (AREA)
- Chemically Coating (AREA)
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は光学的に透明で基板との付着性に優れた酸化
チタン薄膜を形成するゾル状材料の製造方法に関する。TECHNICAL FIELD The present invention relates to a method for producing a sol-like material for forming a titanium oxide thin film which is optically transparent and has excellent adhesion to a substrate.
（従来の技術） 酸化チタンの透明薄膜はガラス又はプラスチツクの表
面に、光の反射防止、特定波長の光の吸収、透過、反射
等の機能を有する光学薄膜を形成する際の高屈折膜とし
て用いられている。又、近年酸化チタン薄膜を用いた光
触媒、センサー等の開発も盛んに行われている。(Prior art) A transparent thin film of titanium oxide is used as a high-refractive-index film when forming an optical thin film having functions of preventing reflection of light, absorbing, transmitting, and reflecting light of a specific wavelength on the surface of glass or plastic. Has been. In recent years, photocatalysts, sensors, and the like using a titanium oxide thin film have been actively developed.
酸化チタン薄膜の形成方法として化学蒸着法、真空蒸
着法、スパツター法等が知られているが、いずれの方法
も装置が複雑で作業性も劣り、また大面積の薄膜を得る
には不適であり、コストも高い。これに対してデイツプ
法は基板を液状の薄膜形成材料に浸漬して引き上げて焼
成する方法であり、スプレー法は加熱した基板上に液を
スプレーする方法であり、簡単な装置で大面積の薄膜を
形成させることができる。Known methods for forming a titanium oxide thin film include a chemical vapor deposition method, a vacuum vapor deposition method, and a sputter method. However, any of these methods has a complicated apparatus, is inferior in workability, and is not suitable for obtaining a large-area thin film. , The cost is also high. On the other hand, the dipping method is a method of immersing the substrate in a liquid thin film forming material, pulling it up and baking it, and the spraying method is a method of spraying the liquid on a heated substrate. Can be formed.
酸化チタンの液状薄膜形成材料（以下デイツプコート
材と呼ぶ）としては一般にチタンのアルコキシドから調
製されたものが用いられるが、可燃性又は有害な有機溶
剤を多量に含有するので使用時に安全面及び衛生面で十
分な対応が必要である。有機溶剤を含まない材料として
チタニヤゾルが市販されているが、これは微粒子の酸化
チタン又はチタン酸の水性懸濁物であり、これを用いて
薄膜を形成させた場合、基板との付着性の良い膜が得ら
れないという問題がある。又、両者とも共通の問題点と
して、貯蔵中に粘度が高くなつたり、沈殿物を形成する
等の経時変化が生じる。As a material for forming a liquid thin film of titanium oxide (hereinafter referred to as a dip coating material), a material prepared from an alkoxide of titanium is generally used. However, since it contains a large amount of flammable or harmful organic solvents, safety and hygiene in use are considered. It is necessary to take sufficient measures. Although titania sol is commercially available as a material containing no organic solvent, this is an aqueous suspension of fine particles of titanium oxide or titanic acid, and when a thin film is formed using this, good adhesion to the substrate is obtained. There is a problem that a film cannot be obtained. Further, as a problem common to both of them, there is a change with time such as an increase in viscosity during storage and formation of a precipitate.
（発明が解決しようとする課題） 本発明の目的は可燃性、有毒、刺激性の揮発物質を含
まず、貯蔵時の経時変化もなく、透明性、付着性に優れ
た酸化チタン薄膜を形成しうるデイツプコート材の製造
方法を提供することにある。(Problems to be Solved by the Invention) An object of the present invention is to form a titanium oxide thin film which does not contain flammable, toxic and irritating volatile substances, does not change with time during storage, and is excellent in transparency and adhesion. An object of the present invention is to provide a method for producing a dip coat material.
（課題を解決するための手段） 本発明はチタン酸ゲルとシュウ酸、クエン酸、酒石
酸、乳酸、マレイン酸、マロン酸、グリコール酸、リン
ゴ酸から選ばれる有機酸の１種以上を反応させることを
特徴とするゾル状のチタン酸からなる酸化チタン薄膜形
成材料の製造方法に係る。(Means for Solving the Problems) The present invention is to react a titanate gel with one or more organic acids selected from oxalic acid, citric acid, tartaric acid, lactic acid, maleic acid, malonic acid, glycolic acid, and malic acid. The present invention relates to a method for producing a titanium oxide thin film-forming material comprising sol-form titanic acid.
本発明においてチタン酸としては公知の各種のものが
使用できるが、例えばチタンの硫酸塩又は塩化物とアン
モニア、水酸化アルカリ、炭酸アルカリと反応させて得
られるゲル状のチタン酸が適しており、加熱して加水分
解させたチタン酸は反応性に乏しいので好ましくない。
チタン酸は水で洗浄して不純物を十分に除き、好ましく
は過ケーク状又はスラリー状で有機酸と反応させる。As the titanic acid in the present invention, various known ones can be used.For example, a gel-form titanic acid obtained by reacting a sulfate or chloride of titanium with ammonia, an alkali hydroxide, or an alkali carbonate is suitable. Titanic acid hydrolyzed by heating is not preferred because it has poor reactivity.
The titanic acid is washed with water to sufficiently remove impurities, and is preferably reacted with the organic acid in the form of a cake or slurry.
チタン酸と反応させる有機酸はシユウ酸、クエン酸、
酒石酸、乳酸、マレイン酸、マロン酸、グリコール酸、
リンゴ酸の水溶性有機酸であり、これらの１種又は２種
以上を使用することができる。本反応は常温で行うのが
望ましいが、70℃程度まで加温することもできる。有機
酸の量はTiO2換算１モルに対して、約0.1〜２モルの範
囲が好ましい。0.1モル未満及び２モルを越えて有機酸
を加えて調製したデイツプコート材を用いて成膜すると
膜の付着性及び硬度が低く、実用面で問題を生じる。チ
タン酸と有機酸との反応は通常、攪拌下で行い、反応液
の外観及び粘度が一定するまで保持する。その後、過
して実用に供する。Organic acids to react with titanic acid are oxalic acid, citric acid,
Tartaric acid, lactic acid, maleic acid, malonic acid, glycolic acid,
It is a water-soluble organic acid of malic acid, and one or more of these can be used. This reaction is desirably performed at room temperature, but can be heated to about 70 ° C. The amount of the organic acid is preferably in the range of about 0.1 to 2 mol based on 1 mol of TiO 2 . When a film is formed using a dip coating material prepared by adding an organic acid in an amount of less than 0.1 mol or more than 2 mol, adhesion and hardness of the film are low, which causes a problem in practical use. The reaction between the titanic acid and the organic acid is usually carried out with stirring, and the reaction solution is maintained until the appearance and viscosity become constant. After that, pass it and put it to practical use.
チタン酸と有機酸の反応において重要なのは、反応さ
せた液がチタン酸のコロイド粒子が分散した状態、即ち
ゾルの外観を示すことである。有機酸量が少ないと沈殿
物を生じ、又有機酸量が多くなるとゾルというよりはむ
しろ溶液に近い外観を呈し、いずれもデイツプコート材
としては好ましくない。What is important in the reaction between titanic acid and an organic acid is that the reacted liquid shows a state in which colloidal particles of titanic acid are dispersed, that is, the appearance of a sol. When the amount of the organic acid is small, a precipitate is formed, and when the amount of the organic acid is large, the appearance is more like a solution rather than a sol, and both are not preferable as the depth coat material.
本発明の方法によつて得られたデイツプコート材を用
いて基板上に薄膜を形成する手段として、通常行われて
いるデイツプ法、スプレー法、スピンナー法等を適用す
ることができ、又、デイツプコート材の変質を起こさな
い程度にアルコール等の溶剤を添加して用いることもで
きる。更に、液の粘度調整及び安定性増大を目的として
メチルセルロース、ゼラチン、ポリビニルアルコール等
の水溶性有機高分子化合物を添加することもできる。本
発明において基板上に形成された薄膜は次いで必要に応
じ乾燥された後、焼成される。乾燥は室温〜200℃程
度、又焼成は約400〜900℃程度又はそれ以上で行うのが
好ましい。この焼成過程で有機酸は炭酸ガスと水に変化
して揮発し、酸化チタン薄膜中には残存しない。As a means for forming a thin film on a substrate using the deep coat material obtained by the method of the present invention, a usual dip method, a spray method, a spinner method, or the like can be applied. A solvent such as an alcohol can be added to such an extent that no deterioration occurs. Further, for the purpose of adjusting the viscosity of the liquid and increasing the stability, a water-soluble organic high molecular compound such as methylcellulose, gelatin, or polyvinyl alcohol can be added. In the present invention, the thin film formed on the substrate is then dried, if necessary, and then fired. Drying is preferably performed at room temperature to about 200 ° C., and firing is preferably performed at about 400 to 900 ° C. or higher. During this firing process, the organic acid changes to carbon dioxide gas and water and volatilizes, and does not remain in the titanium oxide thin film.
上記で得られた酸化チタンの透明薄膜はガラス又はプ
ラスチックの表面に、光の反射防止、特定波長の光の吸
収、透過、反射等の機能を有する光学薄膜を形成する際
の高屈折膜として、或いは光触媒、センサー等として有
用である。The transparent thin film of titanium oxide obtained above is on the surface of glass or plastic, as a high-refractive-index film when forming an optical thin film having functions such as antireflection of light, absorption of light of a specific wavelength, transmission, and reflection. Alternatively, it is useful as a photocatalyst, a sensor, or the like.
（発明の効果） 本発明は可燃性、刺激性の揮発物質を含まず、貯蔵時
の経時変化もなくて、透明性、付着性の優れた酸化チタ
ン薄膜を形成しうるデイツプコート材の製造方法を提供
することができる。(Effects of the Invention) The present invention provides a method for producing a dip coat material which does not contain flammable and irritating volatile substances, does not change over time during storage, and can form a titanium oxide thin film having excellent transparency and adhesion. Can be provided.
（実 施 例） 以下、実施例により本発明を詳細に説明するが、本発
明はこれら実施例に限定されるものではない。(Examples) Hereinafter, the present invention will be described in detail with reference to examples, but the present invention is not limited to these examples.
実施例１〜11及び比較例１ 四塩化チタンの水溶液（TiO250g/）に攪拌下でアン
モニア水（25％）を徐々に加えてpHを5.5に調整し、チ
タン酸ゲルを沈殿させた。このスラリーを別した後、
ゲル中に塩素が認められなくなるまで水を注加して過
洗浄を行つた。得られたゲルのTiO2含有量は10.3％であ
つた。Examples 1 to 11 and Comparative Example 1 Aqueous ammonia (25%) was gradually added to an aqueous solution of titanium tetrachloride (TiO 2 50 g /) with stirring to adjust the pH to 5.5, thereby precipitating a titanate gel. After separating this slurry,
The gel was overwashed by pouring water until no chlorine was found in the gel. The obtained gel had a TiO 2 content of 10.3%.
上述のチタン酸ゲル777g（TiO2として1.0モルを含
む）に水500gを加えてリパルプし、第１表に示したよう
な各種の有機酸を加えて室温で３日間攪拌した。その後
過し、デイツプコート材を得た。いずれの場合も液は
透明ではなくゾルの外観を示し、放置しても沈殿物を生
成しなかつた。500 g of water was added to 777 g of the titanic acid gel (containing 1.0 mol of TiO 2 ) for repulping, various organic acids shown in Table 1 were added, and the mixture was stirred at room temperature for 3 days. After that, a deep coat material was obtained. In all cases, the liquid was not transparent and showed the appearance of a sol, and no precipitate was formed even when left standing.
（１）安定性試験 得られたデイツプコート材を室温で３ケ月間放置した
場合の外観の変化及び粘度を調べ、さらに成膜試験を行
つて、貯蔵による経時変化を調べた。(1) Stability test The obtained deep-coat material was examined for changes in appearance and viscosity when left at room temperature for 3 months, and a film-forming test was further conducted to examine changes over time due to storage.
（２）成膜試験 表面を洗浄したマイクロスライドガラスを、TiO2濃度
を３％に調整したデイツプコート液に浸漬し、10cm/分
の速度で引き上げ、100℃で30分間乾燥後、500℃で30分
間焼成した。膜の付着性評価はセロテープを膜面に密着
させた後、引き剥したときに膜が剥離しないものを良と
し、一部でも剥離した場合を不良とした。又硬度評価は
カミソリの刃を膜面に斜めに当て一定の力で押し付けな
がらスライドさせたときに傷がつかないものを良とし、
つくものを不良とした。(2) Film-forming test The surface-washed microslide glass was immersed in a dip coating solution whose TiO 2 concentration was adjusted to 3%, pulled up at a speed of 10 cm / min, dried at 100 ° C for 30 minutes, and then at 500 ° C for 30 minutes. Bake for minutes. The adhesiveness of the film was evaluated as good when the cellophane tape was adhered to the film surface and then the film was not peeled when peeled off, and poor when the film was partially peeled off. Also, for hardness evaluation, those that do not get scratched when sliding while pressing the razor blade diagonally against the film surface with a constant force are good,
The one that got rid of was considered defective.
Claims (2)
酸、乳酸、マレイン酸、マロン酸、グリコール酸、リン
ゴ酸から選ばれる有機酸の１種以上を反応させることを
特徴とするゾル状のチタン酸からなる酸化チタン薄膜形
成材料の製造方法。1. A sol-like composition comprising reacting a titanate gel with one or more organic acids selected from oxalic acid, citric acid, tartaric acid, lactic acid, maleic acid, malonic acid, glycolic acid and malic acid. A method for producing a titanium oxide thin film forming material comprising titanic acid.
0.1〜２モル使用する請求項１記載の酸化チタン薄膜形
成材料の製造方法。2. An organic acid is added to about 1 mol of titanium oxide.
2. The method for producing a titanium oxide thin film forming material according to claim 1, wherein the material is used in an amount of 0.1 to 2 mol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63122602A JP2608758B2 (en) | 1988-03-23 | 1988-05-19 | Method for producing titanium oxide thin film forming material |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63-70366 | 1988-03-23 | ||
| JP7036688 | 1988-03-23 | ||
| JP63122602A JP2608758B2 (en) | 1988-03-23 | 1988-05-19 | Method for producing titanium oxide thin film forming material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0214820A JPH0214820A (en) | 1990-01-18 |
| JP2608758B2 true JP2608758B2 (en) | 1997-05-14 |
Family
ID=26411527
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63122602A Expired - Fee Related JP2608758B2 (en) | 1988-03-23 | 1988-05-19 | Method for producing titanium oxide thin film forming material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2608758B2 (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2883761B2 (en) * | 1991-12-06 | 1999-04-19 | 工業技術院長 | Antibacterial growth inhibitor |
| JP3726366B2 (en) * | 1996-08-06 | 2005-12-14 | 昭和電工株式会社 | Fluorescent lamp |
| EP1083152B1 (en) | 1998-05-14 | 2006-01-25 | Showa Denko Kabushiki Kaisha | Titanium oxide sol, thin film, and processes for producing these |
| KR100630285B1 (en) | 1998-08-19 | 2006-09-29 | 쇼와 덴코 가부시키가이샤 | Finely particulate titanium-containing substance, coating fluid containing the same, processes for producing these, and molded article having thin film comprising the substance |
| NZ505774A (en) * | 2000-07-17 | 2002-12-20 | Ind Res Ltd | Oxalate stabilised titania solutions and coating compositions and catalysts formed therefrom |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61283629A (en) * | 1985-06-10 | 1986-12-13 | Nippon Shokubai Kagaku Kogyo Co Ltd | Plastic composite material |
| US4778671A (en) * | 1986-07-14 | 1988-10-18 | Corning Glass Works | Preparation of unagglomerated metal oxide particles with uniform particle size |
-
1988
- 1988-05-19 JP JP63122602A patent/JP2608758B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0214820A (en) | 1990-01-18 |
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