JPH0214820A - Production of titanium oxide thin film-forming material - Google Patents
Production of titanium oxide thin film-forming materialInfo
- Publication number
- JPH0214820A JPH0214820A JP63122602A JP12260288A JPH0214820A JP H0214820 A JPH0214820 A JP H0214820A JP 63122602 A JP63122602 A JP 63122602A JP 12260288 A JP12260288 A JP 12260288A JP H0214820 A JPH0214820 A JP H0214820A
- Authority
- JP
- Japan
- Prior art keywords
- titanium oxide
- thin film
- oxide thin
- forming material
- organic acid
- 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.)
- Granted
Links
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000010409 thin film Substances 0.000 claims abstract description 21
- 150000007524 organic acids Chemical class 0.000 claims abstract description 19
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims abstract description 12
- 235000005985 organic acids Nutrition 0.000 claims abstract description 5
- 125000000896 monocarboxylic acid group Chemical group 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 15
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims 1
- 239000000758 substrate Substances 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 238000003860 storage Methods 0.000 abstract description 5
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical class CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 235000014655 lactic acid Nutrition 0.000 abstract description 2
- 239000002085 irritant Substances 0.000 abstract 1
- 231100000021 irritant Toxicity 0.000 abstract 1
- 239000010408 film Substances 0.000 description 13
- 239000007788 liquid Substances 0.000 description 7
- 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
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000011521 glass Substances 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
- 239000002002 slurry Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- 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
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-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
- 241000269821 Scombridae Species 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 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
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 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
- 235000015165 citric acid Nutrition 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000000499 gel 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
- 239000004310 lactic acid Substances 0.000 description 1
- 235000020640 mackerel Nutrition 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- -1 titanium alkoxides Chemical class 0.000 description 1
- 229910000348 titanium sulfate Inorganic materials 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
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 238000007738 vacuum evaporation 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)
Abstract
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液状拐料の％ｌ！造力法に関する。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention is directed to the use of a liquid additive that forms a titanium oxide thin film that is optically transparent and has excellent adhesion to a substrate. Concerning the force-building method.
（従来の技術）
酸化チタンの透明薄膜はプ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
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打ｔ）れている。(Prior art) A transparent thin film of titanium oxide is used as a high refractive film when forming an optical thin film with functions such as antireflection of light, absorption, transmission, and reflection of light of a specific wavelength on the surface of plastic or plastic. It is being Furthermore, in recent years, photocatalysts, sensors, etc. using titanium oxide thin films 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、スパッ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、Ｊ二げて
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。Chemical vapor deposition, vacuum evaporation, sputtering, and other methods are known as methods for forming titanium oxide thin films, but all of these methods require complicated equipment, have poor workability, and are unsuitable for obtaining thin films over a large area. , and the cost is high. On the other hand, the dip method is a method in which the substrate is immersed in a liquid thin film-forming material, drawn, and fired, and the spray method is a method in which a liquid is sprayed onto a heated substrate, using simple equipment. A thin film with a large area can be formed.
酸化チタンの液状薄膜形成材料（以下デイツプフート材
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１面で十
分な対応が必要である。Titanium oxide liquid thin film-forming materials (hereinafter referred to as dipfoot materials) are generally prepared from titanium alkoxides, but since they contain a large amount of flammable or harmful organic solvents, there are safety and hygiene concerns during use. It is necessary to take adequate measures in this area.
有機溶剤を含まない材料としてチタニャゾルが市販され
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、貯蔵中に粘度が商
くなったり、沈殿物を形成する等の経時変化が生じる。Titania sol is commercially available as a material that does not contain organic solvents, but it is an aqueous suspension of fine particles of titanium oxide or titanic acid, and when used to form a thin film,
There is a problem that a film with good adhesion to the substrate cannot be obtained. In addition, both have common problems such as changes over time such as loss of viscosity and formation of precipitates during storage.
（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、付着性に浸れた
酸化チタン薄膜を形成しうるデイツプフート材の製造方
法を提供することにある。(Problems to be Solved by the Invention) The object of the present invention is to form a titanium oxide thin film that does not contain flammable, toxic, or irritating volatile substances, does not change over time during storage, and is highly transparent and adhesive. An object of the present invention is to provide a method for manufacturing a wet dipfoot material.
（課題を解決するための手段）
本発明はチタン酸と一般式
％式％（）
（ＣＯＯｌ（）ＣＩ＋□−１■はＯ又は１〜３の整数を
示す。）で表わされる有機酸の１種以上を反応させるこ
とを特徴とす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 relates to titanic acid and 1 of an organic acid represented by the general formula % () (COOl()CI+□-1■ represents O or an integer from 1 to 3). The present invention relates to a method for producing a titanium oxide thin film forming material, which is characterized by reacting more than one species.
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、加熱しで加水分解
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
濾過ケーク状又はスラリー状で有機酸と反応させる。In the present invention, various known titanic acids can be used, but for example, gelled titanic acid obtained by reacting titanium sulfate or chloride with ammonia, alkali hydroxide, or 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 then reacted with the organic acid, preferably in the form of a filter cake or slurry.
チタン酸と反応させる有機酸は一般式
％式％（１）
（ＣＯＯＨ）ＣＨ２−１１１はＯ又は１〜３の整数を示
す。）で表わされ、具体的には例えばシュウ酸、クエン
酸、酒石酸、乳酸、マレイン酸、マロン酸、グリコール
酸、リンゴ酸等の水溶性有機酸であり、これらの１１１
１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ＴｉＯ□換Ｗ、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、濾過して実用に供する。The organic acid to be reacted with titanic acid has the general formula % (1) (COOH)CH2-111 represents O or an integer from 1 to 3. ), specifically water-soluble organic acids such as oxalic acid, citric acid, tartaric acid, lactic acid, maleic acid, malonic acid, glycolic acid, malic acid, etc.
One or more types can be used. This reaction is preferably carried out at room temperature, but it can also be heated to about 70°C. The amount of organic acid is 1 mole of TiO□W,
A range of about 0.1 to 2 moles is preferred. When a film is formed using a dip coat material prepared by adding less than 0.1 mol or more than 2 mol of an organic acid, the adhesion and hardness of the film are low, causing practical problems. The reaction between titanic acid and organic acid is usually carried out under stirring, and the reaction solution is maintained until its appearance and viscosity are constant. After that, it is filtered and used for 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、即もゾ
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 exhibits a state in which colloidal particles of titanic acid are dispersed, that is, it exhibits the appearance of a sol. If the amount of organic acid is small, a precipitate will be formed, and if the amount of organic acid is large, the appearance will be more like a solution than a sol, and both are undesirable as dip coat materials.
本発明の方法によっ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、デイツプフ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ｆＩ４ＮＮ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
。As a means of forming a thin film on a substrate using the dip coat material obtained by the method of the present invention, commonly used dip methods, spray methods, spinner methods, etc. can be applied, and deterioration of the dip foot material It is also possible to add a solvent such as alcohol to an extent that does not cause the problem. Furthermore, water-soluble organic polymer compounds such as methyl cellulose, gelatin, and polyvinyl alcohol may be added for the purpose of increasing the viscosity fI4NN and stability of the liquid.
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〃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
。In the present invention, the thin film formed on the substrate is then dried, if necessary, and then fired. Drying at room temperature to 200℃
Preferably, the firing is carried out at a temperature of about 400 to 900°C or higher. During this firing process, the organic acid changes into carbonic acid and water and evaporates, 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がラス又はプラ
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 can be used as a high refractive film when forming an optical thin film with functions such as anti-reflection of light, absorption, transmission, and reflection of light of a specific wavelength on the surface of glass or plastic. Alternatively, it is useful as a photocatalyst, sensor, etc.
（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 coating material that does not contain flammable or irritating volatile substances, does not change over time during storage, and can form a titanium oxide thin film with excellent transparency and adhesion. can be provided.
（実 施 例）
以下、実施例により本発明の詳細な説明するが、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 explained 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Ｋｔ（Ｔ ｉ （’） ２５０８／
Ｉ ）に撹拌下でアンモニア水（２５％）を徐々に加
えてＩ）１（を５．５にｉ＄ｉ！９Ｌ、チタン酸デルを
沈殿させた。このスラリーを枦別した後、デル中に塩素
が認められなくなるまで水を注加して濾過洗浄を行−〕
た。得られたゲルのＴｉＯ□含有量は１０．３％であっ
た。Examples 1 to 11 and Comparative Example 1 Water-soluble Kt of titanium tetrachloride (T i (') 2508/
Aqueous ammonia (25%) was gradually added to I) with stirring to make I) 1 (5.5 i$i!9L), and the titanate del was precipitated. After separating this slurry, it was poured into the del. Filter and wash by adding water until no chlorine is detected.
Ta. The TiO□ content of the resulting gel was 10.3%.
上述のチタン酸デル７７７８（′「ｉ ０２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目間攪
１′トシた。その後濾過し、デイツプコート材を得た。Dell 7778 titanate ('i02 as 1.
0 mol) and repulped by adding 500 g of water to
Various organic acids as shown in the table were added and the mixture was stirred for 3 minutes at room temperature. Thereafter, it was filtered to obtain a dip coat material.
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った。In all cases, the liquid was not transparent but had the appearance of a sol, and no precipitate was formed even after standing.
（＋）安定性試験
得られたデイツプフート材を室温で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っ
て、貯蔵による経時変化を調べｔこ。(+) Stability test The obtained dipfoot material was left at room temperature for 3 months, and the changes in appearance and viscosity were examined, and furthermore, a film formation test was conducted to examine changes over time due to storage.
（２）成膜試験
Ａ面を洗浄したマイクロスライドガラスを、Ｔ ＋ ０
２濃度を３％に調整したデイツプコート故に侵潰し、ｌ
ｏｃｍ／分の速度で引き上げ、１００°Ｃ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
て一定の力で押しイ４けながらスライドさセたと鰺に傷
がつかないらのを良とし、つくものを不良とした。(2) Film formation test Microslide glass with surface A cleaned was heated to T + 0
2 concentration was adjusted to 3%, it eroded and l
It was pulled up at a speed of ocm/min, dried at 100°C for 30 minutes, and then fired at 500°C for 30 minutes. For evaluation of adhesion of the film, when cellophane tape was brought into close contact with the film surface and then peeled off, the film was evaluated as good if the film did not peel off, and the film was evaluated as poor if even a portion of the film peeled off. In addition, for hardness evaluation, if the razor blade was applied diagonally to the membrane surface and pressed with a constant force four times while sliding, it was evaluated as good if the mackerel did not get scratched, and if it did, it was evaluated as poor.
Claims (2)
−、−ＣＨ＝ＣＨ−、−ＣＨ（ＯＨ）ＣＨ＿２−、−Ｃ
Ｈ（ＯＨ）ＣＨ（ＯＨ）−又は−ＣＨ＿２Ｃ（ＯＨ）（
ＣＯＯＨ）ＣＨ＿２−、ｎは０又は１〜３の整数を示す
。）で表わされる有機酸の１種以上を反応させることを
特徴とする酸化チタン薄膜形成材料の製造方法。(1) Titanic acid and general formula X-A-COOH (1) (X is H, OH or COOH, A is -(CH_2)_n
-, -CH=CH-, -CH(OH)CH_2-, -C
H(OH)CH(OH)- or -CH_2C(OH)(
COOH)CH_2-, n represents 0 or an integer of 1-3. 1. A method for producing a titanium oxide thin film forming material, the method comprising reacting one or more organic acids represented by the following.
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) Approximately 0.1 to 2 organic acids per mole of titanium oxide
2. The method for producing a titanium oxide thin film forming material according to claim 1, wherein the titanium oxide thin film forming material is used in molar amounts.
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 |
|---|---|---|---|
| JP7036688 | 1988-03-23 | ||
| JP63-70366 | 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 true JPH0214820A (en) | 1990-01-18 |
| JP2608758B2 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) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05155726A (en) * | 1991-12-06 | 1993-06-22 | Agency Of Ind Science & Technol | Material for preventing proliferation of saprophytic bacteria |
| JPH1053438A (en) * | 1996-08-06 | 1998-02-24 | Showa Denko Kk | Fluorescent lamp |
| WO1999058451A1 (en) * | 1998-05-14 | 1999-11-18 | Showa Denko Kabushiki Kaisha | Titanium oxide sol, thin film, and processes for producing these |
| WO2000010921A1 (en) | 1998-08-19 | 2000-03-02 | Showa Denko Kabushiki Kaisha | Finely particulate titanium-containing substance, coating fluid containing the same, processes for producing these, and molded article having thin film comprising the substance |
| WO2002006159A1 (en) * | 2000-07-17 | 2002-01-24 | Industrial Research Limited | Titanium-containing materials |
Citations (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 |
| JPS6325205A (en) * | 1986-07-14 | 1988-02-02 | コ−ニング グラス ワ−クス | Manufacture of metallic oxide particle |
-
1988
- 1988-05-19 JP JP63122602A patent/JP2608758B2/en not_active Expired - Fee Related
Patent Citations (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 |
| JPS6325205A (en) * | 1986-07-14 | 1988-02-02 | コ−ニング グラス ワ−クス | Manufacture of metallic oxide particle |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05155726A (en) * | 1991-12-06 | 1993-06-22 | Agency Of Ind Science & Technol | Material for preventing proliferation of saprophytic bacteria |
| JPH1053438A (en) * | 1996-08-06 | 1998-02-24 | Showa Denko Kk | Fluorescent lamp |
| WO1999058451A1 (en) * | 1998-05-14 | 1999-11-18 | Showa Denko Kabushiki Kaisha | Titanium oxide sol, thin film, and processes for producing these |
| US6627336B1 (en) | 1998-05-14 | 2003-09-30 | Showa Denko Kabushiki Kaisha | Titanium oxide sol, thin film, and processes for producing these |
| US7084179B2 (en) | 1998-05-14 | 2006-08-01 | Showa Denko Kabushiki Kaisha | Titanium oxide dispersion, thin film and process for producing these |
| WO2000010921A1 (en) | 1998-08-19 | 2000-03-02 | Showa Denko Kabushiki Kaisha | Finely particulate titanium-containing substance, coating fluid containing the same, processes for producing these, and molded article having thin film comprising the substance |
| EP1127844A1 (en) * | 1998-08-19 | 2001-08-29 | Showa Denko Kabushiki Kaisha | Finely particulate titanium-containing substance, coating fluid containing the same, processes for producing these, and molded article having thin film comprising the substance |
| US6610135B1 (en) | 1998-08-19 | 2003-08-26 | Showa Denko K.K. | Titanium-containing finely divided particulate material, aqueous sol composition and coating liquid containing same, process for producing same, and shaped article having film thereof |
| EP1127844A4 (en) * | 1998-08-19 | 2008-04-09 | Showa Denko Kk | Finely particulate titanium-containing substance, coating fluid containing the same, processes for producing these, and molded article having thin film comprising the substance |
| WO2002006159A1 (en) * | 2000-07-17 | 2002-01-24 | Industrial Research Limited | Titanium-containing materials |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2608758B2 (en) | 1997-05-14 |
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