JPS6148589B2 - - Google Patents
Info
- Publication number
- JPS6148589B2 JPS6148589B2 JP19762881A JP19762881A JPS6148589B2 JP S6148589 B2 JPS6148589 B2 JP S6148589B2 JP 19762881 A JP19762881 A JP 19762881A JP 19762881 A JP19762881 A JP 19762881A JP S6148589 B2 JPS6148589 B2 JP S6148589B2
- Authority
- JP
- Japan
- Prior art keywords
- paste
- film
- cerium
- organic
- transparent
- 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
- 239000003960 organic solvent Substances 0.000 claims description 6
- 150000001785 cerium compounds Chemical class 0.000 claims description 5
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims 2
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 6
- CUJRVFIICFDLGR-UHFFFAOYSA-N acetylacetonate Chemical compound CC(=O)[CH-]C(C)=O CUJRVFIICFDLGR-UHFFFAOYSA-N 0.000 description 5
- QUKGYYKBILRGFE-UHFFFAOYSA-N benzyl acetate Chemical compound CC(=O)OCC1=CC=CC=C1 QUKGYYKBILRGFE-UHFFFAOYSA-N 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 2
- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical compound CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 description 2
- NIQCNGHVCWTJSM-UHFFFAOYSA-N Dimethyl phthalate Chemical compound COC(=O)C1=CC=CC=C1C(=O)OC NIQCNGHVCWTJSM-UHFFFAOYSA-N 0.000 description 2
- 239000001856 Ethyl cellulose Substances 0.000 description 2
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 2
- 239000000020 Nitrocellulose Substances 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- -1 alcohol ethers Chemical class 0.000 description 2
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 2
- 229940007550 benzyl acetate Drugs 0.000 description 2
- 235000019445 benzyl alcohol Nutrition 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 229920001249 ethyl cellulose Polymers 0.000 description 2
- 235000019325 ethyl cellulose Nutrition 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 229920001220 nitrocellulos Polymers 0.000 description 2
- 238000000059 patterning Methods 0.000 description 2
- 238000007650 screen-printing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229940116411 terpineol Drugs 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 1
- ZQWJZVCRQDBHBQ-UHFFFAOYSA-N 1-butyl-9h-carbazole Chemical compound C12=CC=CC=C2NC2=C1C=CC=C2CCCC ZQWJZVCRQDBHBQ-UHFFFAOYSA-N 0.000 description 1
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- FBSAITBEAPNWJG-UHFFFAOYSA-N dimethyl phthalate Natural products CC(=O)OC1=CC=CC=C1OC(C)=O FBSAITBEAPNWJG-UHFFFAOYSA-N 0.000 description 1
- 229960001826 dimethylphthalate Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
- C03C17/27—Oxides by oxidation of a coating previously applied
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)
- Inorganic Insulating Materials (AREA)
- Surface Treatment Of Glass (AREA)
- Paints Or Removers (AREA)
- Chemically Coating (AREA)
Description
本発明はガラス、セラミツクス等の基板上に形
成する透明金属酸化物被膜に係り、更に詳しくは
該透明被膜が酸化セリウムCe2O3である透明金属
酸化物被膜に関する。
一般にCe2O3透明被膜の形成方法は、真空蒸着
法、化学スプレー法、浸漬法が主である。真空蒸
着法は形成される被膜特性は優れているが、量産
性に問題があり、又、パターン化に対応する為に
は更にエツチング等の処理に施す必要があつた。
一方、化学スプレー法、浸漬法では量産性に問題
はないが、パターン化については前者と同様の問
題がある。この様に、従来方法では一長一短があ
り、必ずしも優れた方法とは言い難い。
本発明は、スクリーン印刷が可能で、焼成によ
つてCe2O3被膜が形成できる印刷ペーストを提供
する為になされたもので、焼成によつてCe2O3被
膜を形成する化合物で、有機溶媒に可溶な有機鉛
化物をペースト中に含有することを特徴とする。
すなわち、前記有機セリウム化合物と有機溶剤と
粘性剤とでペーストを構成する。前記有機セリウ
ム化合物としては化学的に安定な例えばトリスア
セチルアセトナートセリウム()〔Ce
(acac)3〕が好適である。また、有機セリウム化合
物を溶解させる有機溶剤としては、ターピネオー
ル、2−エチルヘキサノール、ベンジルアルコー
ル等の高沸点アルコール類、ベンジルアセテー
ト、ジメチルフタレート等の高沸点エステル類、
カルビトール、ブチルカルビトール、ブチルセロ
ソルブ等の高沸点アルコールエーテル類等の高沸
点有機溶剤が用いられ、粘性剤としてニトロセル
ローズ、エチルセルローズ等のセルローズ化合物
が使用される。
このようにして作られたペーストを使用し、所
望の形状にパターン化されたスクリーン版を用い
てスクリーン印刷し、予備乾燥後400℃以上の温
度で焼成するとCe2O3透明被膜が所望の形状に形
成される。この被膜は透明であることは勿論、膜
強度が大で、比較的高い絶縁性を有する。又、ペ
ースト中に含有するCe(acac)3量を適当にコン
トロールすることで任意の厚さの被膜を自由に形
成することができる。
本発明のCe2O3透明被膜及びCe2O3透明被膜形
成用ペーストは従来のものと若干性質が異なり、
多方面への応用が可能である。以下、実施例に基
づいて詳しく説明する。
実施例 1
アセチルアセトンの配位したトリスアセチルア
セトナートセリウム〔Ce(acac)3〕に、ベンジル
アセテート:ブチルカルバゾール:ブチルセロソ
ルブ=5:3:2の割合に混合した混合有機溶
媒、粘性剤としてニトロセルローズを15wt%添
加してペースト粘度80000cpとし、最終的にCe
(acac)3の含有量をペーストを全量に対し、1〜
30wt%となる様に調製し、夫々ペーストを作成
した。このペーストを用いてステンレスネツト
250メツシユのスクリーン版で、ソーダガラス基
板上にスクリーン印刷し、150℃で20分間予備乾
燥後、500℃で30分間焼成して、それぞれの被膜
の膜厚及びその他の特性を調べ、その結果を次の
表に示す。なお表中の×印は悪いと判断されたも
の、△印はやや悪いと判断されたもの、○印は良
いと判断されたもの、−印は測定不可能なものを
それぞれ示す。また、光透過率(可視部min.)
は、波長が380〜800nmのうち、最低の透過率の
ものを示している。
The present invention relates to a transparent metal oxide film formed on a substrate such as glass or ceramics, and more particularly to a transparent metal oxide film in which the transparent film is cerium oxide Ce 2 O 3 . Generally, the main methods for forming Ce 2 O 3 transparent films are vacuum evaporation, chemical spraying, and dipping. Although the vacuum evaporation method has excellent film characteristics, it has problems in mass production, and in order to support patterning, it is necessary to perform further processing such as etching.
On the other hand, the chemical spray method and the dipping method have no problems in mass production, but have the same problems with patterning. As described above, the conventional methods have advantages and disadvantages, and cannot necessarily be called superior methods. The present invention was made in order to provide a printing paste that can be screen printed and form a Ce 2 O 3 film upon firing. The paste is characterized by containing a solvent-soluble organic leadide.
That is, the organic cerium compound, organic solvent, and viscosity agent constitute a paste. The organic cerium compound is chemically stable, such as trisacetylacetonatocerium () [Ce
(acac) 3 ] is suitable. In addition, examples of organic solvents for dissolving organic cerium compounds include high-boiling alcohols such as terpineol, 2-ethylhexanol, and benzyl alcohol; high-boiling esters such as benzyl acetate and dimethyl phthalate;
High boiling point organic solvents such as high boiling point alcohol ethers such as carbitol, butyl carbitol and butyl cellosolve are used, and cellulose compounds such as nitrocellulose and ethyl cellulose are used as viscosity agents. Using the paste made in this way, screen printing is performed using a screen plate patterned into the desired shape, and after pre-drying, the Ce 2 O 3 transparent film is baked at a temperature of 400℃ or higher to form the desired shape. is formed. This film is not only transparent, but also has high film strength and relatively high insulation properties. Furthermore, by appropriately controlling the amount of Ce(acac) 3 contained in the paste, a film of any desired thickness can be freely formed. The Ce 2 O 3 transparent coating and Ce 2 O 3 transparent coating forming paste of the present invention have slightly different properties from conventional ones,
It can be applied in many fields. Hereinafter, a detailed explanation will be given based on examples. Example 1 Tris acetylacetonate cerium [Ce(acac) 3 ] coordinated with acetylacetone was mixed with a mixed organic solvent in a ratio of benzyl acetate: butyl carbazole: butyl cellosolve = 5:3:2, and nitrocellulose as a viscosity agent. 15wt% was added to make the paste viscosity 80000cp, and finally Ce
(acac) The content of 3 is 1 to 1 to the total amount of paste.
Each paste was prepared so as to have a concentration of 30 wt%. Use this paste to make stainless steel net
Screen printing was performed on a soda glass substrate using a 250-mesh screen plate, pre-dried at 150℃ for 20 minutes, and then baked at 500℃ for 30 minutes to examine the film thickness and other characteristics of each film. Shown in the table below. Note that in the table, an x mark indicates something that was judged to be bad, a △ mark something that was judged to be slightly bad, an ○ mark something that was judged to be good, and a - mark something that could not be measured. Also, light transmittance (visible area min.)
indicates the lowest transmittance among the wavelengths of 380 to 800 nm.
【表】
以上の結果より、Ce(acac)3含有率を10〜
15wt%とすると、透明度良好で、膜強度ならび
に電気絶縁性が大なる被膜を自由に形成できるこ
とがわかる。
実施例 2
有機溶媒に、ベンジルアルコール:ターピネオ
ール=2:1の混合溶剤、粘性剤にエチルセルロ
ーズ(12wt%)を用い、ペースト粘度80000cpに
調製し、実施例1と同様の実験を行なつたが、被
膜強度が若干劣つたことを除いて実施例1とほぼ
同様の結果が得られた。
本発明は前述のような構成になつており、スク
リーン印刷が可能なペーストを提供することがで
き、それによつて量産に適し、パターン化が容易
な透明被膜が得られる。[Table] From the above results, Ce (acac) 3 content is 10~
It can be seen that when the content is 15 wt%, a film with good transparency, film strength, and electrical insulation properties can be freely formed. Example 2 An experiment similar to Example 1 was conducted using a mixed solvent of benzyl alcohol: terpineol = 2:1 as an organic solvent and ethyl cellulose (12 wt%) as a viscosity agent to prepare a paste with a viscosity of 80,000 cp. Almost the same results as in Example 1 were obtained, except that the film strength was slightly inferior. The present invention has the above-described configuration, and can provide a paste that can be screen printed, thereby obtaining a transparent film that is suitable for mass production and easy to pattern.
Claims (1)
化合物で、有機溶媒に可溶な有機セリウム化合物
を含有することを特徴とする透明被膜形成用ペー
スト。 2 特許請求の範囲第1項記載において、前記有
機セリウム化合物がトリスアセチルアセトナート
セリウムであることを特徴とする透明被膜形成用
ペースト。 3 特許請求の範囲第2項記載において、前記ト
リスアセチルアセトナートセリウムがペースト全
量中に約10〜15重量%含有されていることを特徴
とする透明被膜形成用ペースト。[Scope of Claims] 1. A paste for forming a transparent film, which is a compound that forms a cerium oxide film upon firing, and contains an organic cerium compound that is soluble in an organic solvent. 2. A paste for forming a transparent film according to claim 1, wherein the organic cerium compound is cerium trisacetylacetonate. 3. The paste for forming a transparent film according to claim 2, wherein the cerium trisacetylacetonate is contained in an amount of about 10 to 15% by weight in the total amount of the paste.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP19762881A JPS5899143A (en) | 1981-12-10 | 1981-12-10 | Paste for forming transparent film |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP19762881A JPS5899143A (en) | 1981-12-10 | 1981-12-10 | Paste for forming transparent film |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS5899143A JPS5899143A (en) | 1983-06-13 |
JPS6148589B2 true JPS6148589B2 (en) | 1986-10-24 |
Family
ID=16377640
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP19762881A Granted JPS5899143A (en) | 1981-12-10 | 1981-12-10 | Paste for forming transparent film |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS5899143A (en) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE10342905B4 (en) * | 2003-09-17 | 2007-06-14 | Forschungszentrum Karlsruhe Gmbh | Use of a suspension for the production of a corrosion-resistant coating on a ceramic article and method of making the coating |
JP6182398B2 (en) * | 2013-04-10 | 2017-08-16 | 東京応化工業株式会社 | Composition for forming transparent insulating film |
CN105951178B (en) * | 2016-04-29 | 2019-01-18 | 中国工程物理研究院材料研究所 | A method of preparing cubic phase cerium sesquioxide monocrystal thin films |
-
1981
- 1981-12-10 JP JP19762881A patent/JPS5899143A/en active Granted
Also Published As
Publication number | Publication date |
---|---|
JPS5899143A (en) | 1983-06-13 |
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