JPH02157121A - Screen printing ink for forming superconducting oxide thin film and formation of superconducting oxide thin film using this ink - Google Patents
Screen printing ink for forming superconducting oxide thin film and formation of superconducting oxide thin film using this inkInfo
- Publication number
- JPH02157121A JPH02157121A JP63311076A JP31107688A JPH02157121A JP H02157121 A JPH02157121 A JP H02157121A JP 63311076 A JP63311076 A JP 63311076A JP 31107688 A JP31107688 A JP 31107688A JP H02157121 A JPH02157121 A JP H02157121A
- Authority
- JP
- Japan
- Prior art keywords
- salt
- thin film
- ink
- oxide thin
- superconducting oxide
- 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.)
- Pending
Links
- 239000010409 thin film Substances 0.000 title claims abstract description 24
- 238000007650 screen-printing Methods 0.000 title claims description 12
- 230000015572 biosynthetic process Effects 0.000 title description 3
- -1 Terpenoid carboxylic acid Chemical class 0.000 claims abstract description 24
- 239000002562 thickening agent Substances 0.000 claims abstract description 21
- 150000001412 amines Chemical class 0.000 claims abstract description 20
- 239000000758 substrate Substances 0.000 claims abstract description 19
- 150000003839 salts Chemical class 0.000 claims abstract description 17
- 238000007639 printing Methods 0.000 claims abstract description 14
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 150000002148 esters Chemical class 0.000 claims abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 7
- 239000001301 oxygen Substances 0.000 claims abstract description 7
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 7
- 238000004898 kneading Methods 0.000 claims abstract 3
- 238000000034 method Methods 0.000 claims description 16
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 9
- BTXXTMOWISPQSJ-UHFFFAOYSA-N 4,4,4-trifluorobutan-2-one Chemical compound CC(=O)CC(F)(F)F BTXXTMOWISPQSJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000005749 Copper compound Substances 0.000 claims description 5
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 5
- 150000001553 barium compounds Chemical class 0.000 claims description 5
- 150000001880 copper compounds Chemical class 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 5
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 4
- BQACOLQNOUYJCE-FYZZASKESA-N Abietic acid Natural products CC(C)C1=CC2=CC[C@]3(C)[C@](C)(CCC[C@@]3(C)C(=O)O)[C@H]2CC1 BQACOLQNOUYJCE-FYZZASKESA-N 0.000 claims 6
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical class CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 claims 5
- 150000002739 metals Chemical class 0.000 claims 4
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical class CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 claims 2
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical class CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims 2
- 150000005332 diethylamines Chemical class 0.000 claims 2
- 238000001035 drying Methods 0.000 claims 2
- 238000010438 heat treatment Methods 0.000 claims 2
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical class CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 claims 2
- 150000001875 compounds Chemical class 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 22
- 239000000976 ink Substances 0.000 description 30
- 239000010408 film Substances 0.000 description 20
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- 239000002253 acid Substances 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 125000004432 carbon atom Chemical group C* 0.000 description 6
- 238000011156 evaluation Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 230000005587 bubbling Effects 0.000 description 4
- 230000007704 transition Effects 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 150000002736 metal compounds Chemical class 0.000 description 3
- 238000007665 sagging Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 150000003505 terpenes Chemical class 0.000 description 3
- AGOMHFKGCMKLDA-UHFFFAOYSA-K 2-ethylhexanoate;yttrium(3+) Chemical compound [Y+3].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O AGOMHFKGCMKLDA-UHFFFAOYSA-K 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229920002871 Dammar gum Polymers 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- QUKGYYKBILRGFE-UHFFFAOYSA-N benzyl acetate Chemical compound CC(=O)OCC1=CC=CC=C1 QUKGYYKBILRGFE-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000025 natural resin Substances 0.000 description 2
- 150000003141 primary amines Chemical class 0.000 description 2
- 150000003335 secondary amines Chemical class 0.000 description 2
- WXENESFPQCWDHY-UHFFFAOYSA-M silver;2-ethylhexanoate Chemical compound [Ag+].CCCCC(CC)C([O-])=O WXENESFPQCWDHY-UHFFFAOYSA-M 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 239000002887 superconductor Substances 0.000 description 2
- 150000003512 tertiary amines Chemical class 0.000 description 2
- MHVJRKBZMUDEEV-APQLOABGSA-N (+)-Pimaric acid Chemical compound [C@H]1([C@](CCC2)(C)C(O)=O)[C@@]2(C)[C@H]2CC[C@](C=C)(C)C=C2CC1 MHVJRKBZMUDEEV-APQLOABGSA-N 0.000 description 1
- MHVJRKBZMUDEEV-UHFFFAOYSA-N (-)-ent-pimara-8(14),15-dien-19-oic acid Natural products C1CCC(C(O)=O)(C)C2C1(C)C1CCC(C=C)(C)C=C1CC2 MHVJRKBZMUDEEV-UHFFFAOYSA-N 0.000 description 1
- WUOACPNHFRMFPN-SECBINFHSA-N (S)-(-)-alpha-terpineol Chemical compound CC1=CC[C@@H](C(C)(C)O)CC1 WUOACPNHFRMFPN-SECBINFHSA-N 0.000 description 1
- OBETXYAYXDNJHR-UHFFFAOYSA-N 2-Ethylhexanoic acid Chemical compound CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 1
- QGJZLNKBHJESQX-UHFFFAOYSA-N 3-Epi-Betulin-Saeure Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CCC5(C(O)=O)CCC(C(=C)C)C5C4CCC3C21C QGJZLNKBHJESQX-UHFFFAOYSA-N 0.000 description 1
- CLOUCVRNYSHRCF-UHFFFAOYSA-N 3beta-Hydroxy-20(29)-Lupen-3,27-oic acid Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C(O)=O)CCC5(C)CCC(C(=C)C)C5C4CCC3C21C CLOUCVRNYSHRCF-UHFFFAOYSA-N 0.000 description 1
- MIJYXULNPSFWEK-GTOFXWBISA-N 3beta-hydroxyolean-12-en-28-oic acid Chemical compound C1C[C@H](O)C(C)(C)[C@@H]2CC[C@@]3(C)[C@]4(C)CC[C@@]5(C(O)=O)CCC(C)(C)C[C@H]5C4=CC[C@@H]3[C@]21C MIJYXULNPSFWEK-GTOFXWBISA-N 0.000 description 1
- OPAORDVBZRVVNQ-RNQWEJQRSA-N 4-[(z,2r)-4-(4-hydroxy-3-methoxyphenyl)-2,3-dimethylbut-3-enyl]-2-methoxyphenol Chemical compound C1=C(O)C(OC)=CC(C[C@@H](C)C(\C)=C/C=2C=C(OC)C(O)=CC=2)=C1 OPAORDVBZRVVNQ-RNQWEJQRSA-N 0.000 description 1
- 240000000972 Agathis dammara Species 0.000 description 1
- 241000208340 Araliaceae Species 0.000 description 1
- DIZWSDNSTNAYHK-XGWVBXMLSA-N Betulinic acid Natural products CC(=C)[C@@H]1C[C@H]([C@H]2CC[C@]3(C)[C@H](CC[C@@H]4[C@@]5(C)CC[C@H](O)C(C)(C)[C@@H]5CC[C@@]34C)[C@@H]12)C(=O)O DIZWSDNSTNAYHK-XGWVBXMLSA-N 0.000 description 1
- 239000004859 Copal Substances 0.000 description 1
- 239000004860 Dammar gum Substances 0.000 description 1
- JKLISIRFYWXLQG-UHFFFAOYSA-N Epioleonolsaeure Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CCC5(C(O)=O)CCC(C)(C)CC5C4CCC3C21C JKLISIRFYWXLQG-UHFFFAOYSA-N 0.000 description 1
- 241000147041 Guaiacum officinale Species 0.000 description 1
- 241000782205 Guibourtia conjugata Species 0.000 description 1
- RWWVEQKPFPXLGL-ONCXSQPRSA-N L-Pimaric acid Chemical compound [C@H]1([C@](CCC2)(C)C(O)=O)[C@@]2(C)[C@H]2CC=C(C(C)C)C=C2CC1 RWWVEQKPFPXLGL-ONCXSQPRSA-N 0.000 description 1
- RWWVEQKPFPXLGL-UHFFFAOYSA-N Levopimaric acid Natural products C1CCC(C(O)=O)(C)C2C1(C)C1CC=C(C(C)C)C=C1CC2 RWWVEQKPFPXLGL-UHFFFAOYSA-N 0.000 description 1
- KGMSWPSAVZAMKR-UHFFFAOYSA-N Me ester-3, 22-Dihydroxy-29-hopanoic acid Natural products C1CCC(C(O)=O)(C)C2C1(C)C1CCC(=C(C)C)C=C1CC2 KGMSWPSAVZAMKR-UHFFFAOYSA-N 0.000 description 1
- KGMSWPSAVZAMKR-ONCXSQPRSA-N Neoabietic acid Chemical compound [C@H]1([C@](CCC2)(C)C(O)=O)[C@@]2(C)[C@H]2CCC(=C(C)C)C=C2CC1 KGMSWPSAVZAMKR-ONCXSQPRSA-N 0.000 description 1
- YBRJHZPWOMJYKQ-UHFFFAOYSA-N Oleanolic acid Natural products CC1(C)CC2C3=CCC4C5(C)CCC(O)C(C)(C)C5CCC4(C)C3(C)CCC2(C1)C(=O)O YBRJHZPWOMJYKQ-UHFFFAOYSA-N 0.000 description 1
- MIJYXULNPSFWEK-UHFFFAOYSA-N Oleanolinsaeure Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CCC5(C(O)=O)CCC(C)(C)CC5C4=CCC3C21C MIJYXULNPSFWEK-UHFFFAOYSA-N 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- OVKDFILSBMEKLT-UHFFFAOYSA-N alpha-Terpineol Natural products CC(=C)C1(O)CCC(C)=CC1 OVKDFILSBMEKLT-UHFFFAOYSA-N 0.000 description 1
- 229940088601 alpha-terpineol Drugs 0.000 description 1
- JXSVIVRDWWRQRT-UYDOISQJSA-N asiatic acid Chemical compound C1[C@@H](O)[C@H](O)[C@@](C)(CO)[C@@H]2CC[C@@]3(C)[C@]4(C)CC[C@@]5(C(O)=O)CC[C@@H](C)[C@H](C)[C@H]5C4=CC[C@@H]3[C@]21C JXSVIVRDWWRQRT-UYDOISQJSA-N 0.000 description 1
- VJFFDDQGMMQGTQ-UHFFFAOYSA-L barium(2+);2-ethylhexanoate Chemical compound [Ba+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O VJFFDDQGMMQGTQ-UHFFFAOYSA-L 0.000 description 1
- YIXUBKJRRPSDRB-UHFFFAOYSA-L barium(2+);hexanoate Chemical compound [Ba+2].CCCCCC([O-])=O.CCCCCC([O-])=O YIXUBKJRRPSDRB-UHFFFAOYSA-L 0.000 description 1
- 229940007550 benzyl acetate Drugs 0.000 description 1
- QGJZLNKBHJESQX-FZFNOLFKSA-N betulinic acid Chemical compound C1C[C@H](O)C(C)(C)[C@@H]2CC[C@@]3(C)[C@]4(C)CC[C@@]5(C(O)=O)CC[C@@H](C(=C)C)[C@@H]5[C@H]4CC[C@@H]3[C@]21C QGJZLNKBHJESQX-FZFNOLFKSA-N 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- SHZIWNPUGXLXDT-UHFFFAOYSA-N caproic acid ethyl ester Natural products CCCCCC(=O)OCC SHZIWNPUGXLXDT-UHFFFAOYSA-N 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- PZXJOHSZQAEJFE-UHFFFAOYSA-N dihydrobetulinic acid Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CCC5(C(O)=O)CCC(C(C)C)C5C4CCC3C21C PZXJOHSZQAEJFE-UHFFFAOYSA-N 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 150000004141 diterpene derivatives Chemical class 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229940091561 guaiac Drugs 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- 150000002391 heterocyclic compounds Chemical class 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229930003658 monoterpene Natural products 0.000 description 1
- MQYXUWHLBZFQQO-UHFFFAOYSA-N nepehinol Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CCC5(C)CCC(C(=C)C)C5C4CCC3C21C MQYXUWHLBZFQQO-UHFFFAOYSA-N 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229940100243 oleanolic acid Drugs 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- HZLWUYJLOIAQFC-UHFFFAOYSA-N prosapogenin PS-A Natural products C12CC(C)(C)CCC2(C(O)=O)CCC(C2(CCC3C4(C)C)C)(C)C1=CCC2C3(C)CCC4OC1OCC(O)C(O)C1O HZLWUYJLOIAQFC-UHFFFAOYSA-N 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は、エレクトロニクス産業において使用される超
伝導酸化物薄膜をスクリーン印刷工法によって製造する
だめのインキおよびこのインキを使用した薄膜抵抗体形
成方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to an ink used in the electronics industry for producing superconducting oxide thin films by a screen printing method, and a method for forming a thin film resistor using this ink. It is.
従来の技術
一般式ｙＢａ２ ＣｕＫ ０７−Ｘで示される酸化物超
伝導体は、その超伝導転移温度が液体窒素温度以上であ
るという点で工業的にも非常に有用な材料である。この
超電導体は、電力用としてはその焼結体を線状に加工し
たものが使われ、能動的な電子デバイスとしては薄膜状
で利用されることの多いものである。この物質の薄１摸
形成は、現在主としてスパッタリングを用いて行なわれ
ている。この也に薄膜形成法として金属有機物の熱分解
による方法が提案され、スピンコードやデイ、プといっ
た方法で基板上に形成した膜についての研究が現在性な
われている。BACKGROUND OF THE INVENTION Oxide superconductors represented by the general formula yBa2 CuK 07-X are industrially very useful materials in that their superconducting transition temperature is higher than the liquid nitrogen temperature. This superconductor is used as a sintered body processed into a linear shape for power purposes, and is often used in the form of a thin film for active electronic devices. Formation of a thin film of this material is currently performed primarily using sputtering. A method based on thermal decomposition of metal-organic substances has been proposed as a thin film formation method for this purpose, and research is currently underway on films formed on substrates using methods such as spin-coating and dip-coating.
発明が解決しようとする課題
しかしながら、スパッタリングでは高コストで製造設備
も高価となり、スピンコートエ法やディノプ工法では、
−度基板全面に形成した膜をそのちとなんらかの方法で
パターン精度グするという、繁雑でコストアップの原因
となる工程を取らざるを得ないものであった。丑たスク
リーン印刷法を導入するには平滑性、パターン精度に問
題を有するものとならざるを得なかった。Problems to be Solved by the Invention However, sputtering requires high costs and expensive manufacturing equipment, and the spin coat method and Dinop method
- The pattern precision of the film formed on the entire surface of the substrate must be checked by some method, a process that is complicated and causes an increase in costs. In order to introduce the screen printing method, problems with smoothness and pattern accuracy were inevitable.
課題を解決するだめの手段
本発明は超伝導酸化物薄膜形成用インキ（以下、インキ
と言う）に添加する。増粘剤としてテルペノイドのカル
ボン酸あるいはそれらのエステルと、これにテルペノイ
ドのカルボン酸のアンモニウム塩かアミン類との塩を添
加したものを用いたものである。Means for Solving the Problems The present invention is added to an ink for forming a superconducting oxide thin film (hereinafter referred to as ink). As a thickener, a terpenoid carboxylic acid or an ester thereof is used, and an ammonium salt of the terpenoid carboxylic acid or a salt of amines is added thereto.
作用
本発明は以上のように増粘剤としてテルペノイドのカル
ボン酸あるいはそれらのエステルと、テルペノイドのカ
ルボン酸のアンモニウム塩するいはアミン類との塩を添
加したものを使用したので、インキは印刷時のメツシュ
通過によっても泡が発生することなく被印刷物上に移さ
れるようになり、非常に平滑でムラのない印刷膜面が得
られ、しかもテルペノイドのカルボン酸のアンモニウム
塩又はアミン類との塩は、高温で分解して灰分を残さな
いため、焼成により品質良好な超伝導酸化物薄膜が得ら
れるものである。Function As described above, the present invention uses a terpenoid carboxylic acid or its ester as a thickener, and an ammonium salt of a terpenoid carboxylic acid or a salt with amines. Even when it passes through the mesh, it is transferred onto the printing substrate without generating bubbles, and a very smooth and even printing surface is obtained. Since it decomposes at high temperatures and leaves no ash, a high-quality superconducting oxide thin film can be obtained by firing.
実施例 まず、本発明の概要について説明する。Example First, an overview of the present invention will be explained.
本発明で用いることのできるイツトリウム化合物、バリ
ウム化合物、銅化合物には特に制限はなく、適当な溶媒
によって増粘剤と相溶するようなものであればよい。The yttrium compound, barium compound, and copper compound that can be used in the present invention are not particularly limited, as long as they are compatible with the thickener in an appropriate solvent.
次に本発明で増粘剤を構成するテルペノイドのカ
ルボン
ビエチン酸とその誘導体であるピマル酸，ネオアビエチ
ン酸，レボピマル酸など、また、グアヤコン酸とその誘
導体、グアヤク酸，／１／ベニン酸などである。さらに
は、ダンマルゴムに含有されるダンマロール酸とその誘
導体、ウルンル酸，オレアノール酸，ベツリン酸なども
用いることができる。Next, in the present invention, the terpenoids constituting the thickener include carbobietic acid and its derivatives such as pimaric acid, neoabietic acid, and levopimaric acid, as well as guaiaconic acid and its derivatives, guaiacic acid, /1/bennic acid, etc. It is. Furthermore, dammarolic acid and its derivatives, urunuric acid, oleanolic acid, betulinic acid, etc. contained in dammar gum can also be used.
モノテルペノイドのカルボン酸は、常温で液体のものが
多いため、単独では使用できないが、前述のようなジテ
ルペノイドやトリテルペノイドのカルボン酸と混合すれ
ば使用してもよい。これらは、精製分離されたものが一
般には入手しがたく高価でもあるので、それらを含む天
然樹脂である日ジンやグアヤク脂，ダンマル，コーパル
などを利用することができる。これらのような天然樹脂
は、産地やメーカーによ゛って成分が大幅に異なり、カ
ルボン酸以外の成分も含まれていることがあるが、本発
明の目的にはいっこうに差支えなく使用できる。これ等
のエステルとしては、主にアビエチン酸のエステル類が
使用でき、一般に市販されてい７・＼−７
るロジンエステルであれば、その種類は何でもよい。Most monoterpenoid carboxylic acids are liquid at room temperature, so they cannot be used alone, but they may be used if mixed with the aforementioned diterpenoid or triterpenoid carboxylic acids. Since refined and separated products of these are generally difficult to obtain and expensive, natural resins containing them such as ginseng, guaiac, dammar, and copal can be used. Natural resins such as these can be used without any problem for the purpose of the present invention, although their components vary widely depending on the region of production and manufacturer, and they may contain components other than carboxylic acids. As these esters, abietic acid esters can mainly be used, and any type of rosin ester that is generally commercially available may be used.
テルペノイドのカルボン酸のアンモニウム塩、あるいは
アミン類との塩は、前述のような酸とアンモニアやアミ
ン類との中和反応によって合成されたものが使用できる
。アミン類については、第級、第二級、第三級のすべて
の種類及び脂肪族芳香族、複素環化合物の種類を問わず
使えるが、そのアルキル基に含まれる炭素数は、あ−１
シ多くないほうが好ましい。これは、炭素数が増加する
につれ、塩の無機塩的な性質が消失していくため本明細
書の作用で述べたような効果が期待できなくなるためで
ある。実際には、一つのアルキル基の炭素数は６以下、
全体でも１５以下程度のものが望ましいと思われる。な
お、増粘剤の好適な組成範囲は用いた酸やアミン類の種
類によって異なるが、これについては後述する。As ammonium salts of terpenoid carboxylic acids or salts with amines, those synthesized by the neutralization reaction of the acid with ammonia or amines as described above can be used. Regarding amines, all types of primary, secondary, and tertiary, as well as aliphatic aromatic and heterocyclic compounds can be used, but the number of carbon atoms contained in the alkyl group is -1
It is preferable not to have too many. This is because as the number of carbon atoms increases, the inorganic salt properties of the salt disappear, making it impossible to expect the effects described in the section of this specification. In reality, the number of carbon atoms in one alkyl group is 6 or less,
It seems desirable that the total value be about 15 or less. Note that the preferred composition range of the thickener varies depending on the type of acid or amine used, and this will be described later.
基体としては、超伝導酸化物薄膜が結晶化する温度に耐
えるような耐熱性の物質を用いることができ、例えば、
アルミナ、ジルコニアをはじメトするセラミックスや、
ステンレスやチタンなどの金属２石英ガラスやホウケイ
酸ガラスなど、サラに表面にグレーズをかけたセラミッ
クスなどが使用できる。しかしながら、超伝導特性のよ
しあしという観点から、焼成を酸素雰囲気中で行うこと
が必要であるため、金属の基体は耐酸化性の良いものを
使うのが好捷しい。As the substrate, a heat-resistant material that can withstand the temperature at which the superconducting oxide thin film crystallizes can be used, for example,
Ceramics including alumina and zirconia,
Metallic materials such as stainless steel and titanium can be used, such as silica glass, borosilicate glass, and ceramics with a smooth surface glaze. However, from the viewpoint of good superconducting properties, it is necessary to perform the firing in an oxygen atmosphere, so it is preferable to use a metal substrate with good oxidation resistance.
次に具体的な実施例について述べる。Next, a specific example will be described.
（実施例１）
第１表に示した組成で増粘剤を１００ｇ調製し、これら
に２−エチルヘキサン酸イツトリウム、２−工ｆ ｚｌ
ｚヘキサン酸バリウム、２−エチルヘキサン酸銀をモル
比で１ ：２：３に混合したものを２０Ｉ添加し、溶剤
としてアセトフェノンヲ３０ｇ加えて混練し、各組成の
スクリーン印刷インキを製造した。これらのインキを乳
剤厚み１６７ｚｍ、２００メツシユのスクリーン版を用
いてガラス基板上に１ｏｍｍＸ３０ｍｍの矩形状パター
ンに印刷を行った。この被印刷物を１５０℃で３０分間
乾燥し、印刷膜面の評価を行った。評価は、膜面のムラ
の有無とパターンエツジのダレの二点と、印刷時の泡立
ちの有無で行った。(Example 1) 100g of thickener was prepared with the composition shown in Table 1, and yttrium 2-ethylhexanoate and 2-ethylhexanoate were added to the thickener.
20 I of a mixture of barium hexanoate and silver 2-ethylhexanoate in a molar ratio of 1:2:3 was added, and 30 g of acetophenone as a solvent was added and kneaded to produce screen printing inks of each composition. These inks were printed in a rectangular pattern of 1 om x 30 mm on a glass substrate using a screen plate with an emulsion thickness of 167 zm and 200 meshes. This printed material was dried at 150° C. for 30 minutes, and the surface of the printed film was evaluated. The evaluation was based on two points: the presence or absence of unevenness on the film surface, the sagging of the pattern edges, and the presence or absence of bubbling during printing.
（以下余 白）
第１表
１１へ一／
表中、評価欄の記号は、Ｏ−＋々し、ム→若干あり、×
→あり、をそれぞれ示す。また、−は、インキを製造で
きないことを意味する。以下の表についても同様。(The following is a margin) Go to Table 1 11/ In the table, the symbols in the evaluation column are O-+, M → Slightly, ×
→Indicates “Yes” and “Yes” respectively. Moreover, - means that ink cannot be manufactured. The same applies to the table below.
これら評価結果も、第１表中に示した。これから分るよ
うに、テルペノイドのカルボン酸のアンモニウム塩かア
ミン類との塩を含有させたインキについては、印刷時の
泡立ちがなくなって印刷膜面が良好となる。その効果が
現れる組成については、用いたテルペノイドのカルボン
酸の種類と組成によって異なるが、第１表の結果から、
良好なインキを得るために必要なこれら塩類の添加すべ
き最小量は、アンモニア、第一級アミン、第二級アミン
、第三級アミンの順に増加していき、アミンの炭素数増
加と共に増加する傾向にあることが分る。寸だ、アミン
によっては全く酸類を含有させなくても、良好なインキ
（印刷時の泡立ち、膜面のムラ、パターンのダレについ
て全て△評価以上のもの、以下同じ）を製造できる塩の
あることが分る。These evaluation results are also shown in Table 1. As can be seen, the ink containing the ammonium salt of terpenoid carboxylic acid or the salt with amines eliminates bubbling during printing and provides a good printed film surface. The composition in which this effect appears varies depending on the type and composition of the terpenoid carboxylic acid used, but from the results in Table 1,
The minimum amount of these salts required to obtain a good ink increases in the order of ammonia, primary amine, secondary amine, and tertiary amine, and increases as the number of carbon atoms in the amine increases. It can be seen that there is a trend. In fact, some amines have salts that can produce good ink (bubbling during printing, unevenness on the film surface, and sagging of patterns all rated △ or above, the same applies hereinafter) without containing any acids. I understand.
これらの印刷物で、膜面の良好なものを酸素雰囲気中、
７００℃で１時間加熱すると、膜厚２０００Ａ程度の黒
色の酸化物薄膜が得られた。Among these printed materials, those with good film surfaces were placed in an oxygen atmosphere.
When heated at 700° C. for 1 hour, a black oxide thin film with a thickness of about 2000 Å was obtained.
これらの結晶形をＸ線回折で調べたところ、超広１３１
、−７
導酸化物焼結体の結晶形と同様であることが分った。When these crystal forms were examined by X-ray diffraction, it was found that ultra-wide 131
, -7 It was found that the crystal form is similar to that of the conductive oxide sintered body.
（実施例２）
第２表に示した組成でビヒクｌし１００ｇを調製し、こ
れに実施例１と同様の金属化合物を同量添加し、溶剤と
してα−ターピネオールを３０９加えて混練し、インキ
を製造した。これらのインキを実施例１と同様な方法で
評価した結果も第２表中に示した。(Example 2) 100 g of a vehicle was prepared with the composition shown in Table 2, the same amount of the same metal compound as in Example 1 was added thereto, 309 g of α-terpineol was added as a solvent and kneaded, and an ink was prepared. was manufactured. The results of evaluating these inks in the same manner as in Example 1 are also shown in Table 2.
第２表
（以下余白）
これから、実施例１と同様に、テルペノイドのカルボン
酸のアンモニウム塩かアミン類との塩全含有するビヒク
ルのインキが良好な膜面を与えることが分る。捷だ、第
２表から、良好な印刷インキを得るために増粘剤中に含
有させるべきこれら塩類の最小量は、アミンの炭素数が
増加するに伴って増大するということが分る。Table 2 (blank below) shows that, as in Example 1, ink with a vehicle containing all ammonium salts of terpenoid carboxylic acids or salts with amines gives a good film surface. It can be seen from Table 2 that the minimum amount of these salts that must be included in the thickener to obtain a good printing ink increases as the number of carbon atoms in the amine increases.
なお、この実施例からも明らかなように、テルペノイド
のカルボン酸が何種かの混合物であっても差支えないの
と同様に、そのアンモニウム塩かアミン類との塩も何種
類かの混合物であってもかまわない。As is clear from this example, just as terpenoid carboxylic acids can be a mixture of several types, their ammonium salts or salts with amines can also be a mixture of several types. It doesn't matter.
これら印刷物で、膜面の良好なものを実施例１と同様に
焼成して得られた薄膜は、実施例１と同様な性質を示し
た。Thin films obtained by firing these printed materials with good film surfaces in the same manner as in Example 1 exhibited properties similar to those in Example 1.
（実施例３）
第３表に示した組成で増粘剤１０ｏｇを調製し、これに
実施例１と同様な金属化合物を同量添加し、溶剤として
酢酸ベンジルを３Ｑｇ加えて混練し、インキを製造した
。これらのインキを実施例１と同じ方法で評価した結果
も第３表中に示した。(Example 3) 10 og of thickener was prepared with the composition shown in Table 3, the same amount of the same metal compound as in Example 1 was added thereto, and 3 Qg of benzyl acetate was added as a solvent and kneaded to form an ink. Manufactured. The results of evaluating these inks using the same method as in Example 1 are also shown in Table 3.
第６表
１９Ａ−７
これからも、前述の実施例と同様、テルペノイドのカル
ボン酸のアンモニウム塩かアミン類との塩を含有させた
増粘剤のインキが良好な印刷膜面を与えることが分る。Table 6 19A-7 As in the above-mentioned examples, it can be seen that ink with a thickener containing an ammonium salt of terpenoid carboxylic acid or a salt with amines gives a good printed film surface. .
（実施例４）
第４表に示した組成で増粘剤を１００ｇ調製し、これら
に２−エチルヘキサン酸イツトリウム、２エチルヘキサ
ン酸バリウム、２−エチルヘキサン酸銀をモル比で１
二２：３に混合したものを２０ｇ添加し、溶剤としてア
セトフェノンを３゜ｇ加えて混練し、各組成のスクリー
ン印刷インキを製造した。これらのインキを乳剤厚み１
ｓ７ｚｍ、２５０メツシユのスクリーン版を用いて石英
ガラス基板上に１０１０ｍｍＸ３０の矩形状パターンに
印刷を行った。この被印刷物を１５０’Ｃで３０分間乾
燥し、印刷膜面の評価を行った。評価は、膜面のムラの
有無とパターンエツジのダレの二点と、印刷時の泡立ち
の有無で行った。(Example 4) 100g of thickener was prepared with the composition shown in Table 4, and yttrium 2-ethylhexanoate, barium 2-ethylhexanoate, and silver 2-ethylhexanoate were added in a molar ratio of 1
20g of a 2:3 mixture was added, and 3g of acetophenone was added as a solvent and kneaded to produce screen printing inks of each composition. These inks have an emulsion thickness of 1
A rectangular pattern of 1010 mm x 30 mm was printed on a quartz glass substrate using a s7zm, 250 mesh screen plate. This printing material was dried at 150'C for 30 minutes, and the surface of the printed film was evaluated. The evaluation was based on two points: the presence or absence of unevenness on the film surface, the sagging of the pattern edges, and the presence or absence of bubbling during printing.
表中、評価欄の記号は、○→なし、△→若干あり、×→
あり、をそれぞれ示す。また、−は、インキを製造でき
ないことを意味する。以下の表についても同様。In the table, the symbols in the evaluation column are ○→none, △→slightly present, ×→
Yes and Yes, respectively. Moreover, - means that ink cannot be manufactured. The same applies to the table below.
１／６ ）
（２／ｌ ）
第
表
（３／ｌ ’Ｉ
これら評価結果も、表中に示した。これから分るように
、テルペノイドのカルボン酸のアンモニウム塩かアミン
類との塩を含有させたインキについては、印刷時の泡立
ちがなくなって印刷膜面が良好となる。その効果が現れ
る組成については、用いたテルペノイドのカルボン酸の
種類と組成によって異なるが、Ｄ１〜Ｄ６０の結果から
、良好なインキを得るために必要なこれら塩類の添加す
ベキ最小量は、アンモニア、第一級アミン、第二級アミ
ン、第三級アミンの順に増加していき、アミンの炭素数
増加と共に増加する傾向にあることが分る。寸だ、アミ
ンによっては全く酸類を含有させなくても、良好なイン
キを製造できる塩のあることが分る。1/6) (2/l) Table (3/l'I) These evaluation results are also shown in the table.As can be seen, the terpenoid contains an ammonium salt of carboxylic acid or a salt with amines. Regarding the ink, bubbles during printing are eliminated and the printed film surface becomes good.The composition in which this effect appears depends on the type and composition of the carboxylic acid of the terpenoid used, but from the results of D1 to D60, it is found that the printed film surface is good. The minimum power addition amount of these salts necessary to obtain a good ink increases in the order of ammonia, primary amine, secondary amine, and tertiary amine, and tends to increase as the number of carbon atoms in the amine increases. It turns out that some amines can produce good ink without containing any acids at all.
なお、この実施例からも明らかなように、テルペノイド
のカルボン酸が何種かの混合物であっても差支えないの
と同様に、そのアンモニウム塩かアミン類との塩も何種
類かの混合物であってもか寸わない。As is clear from this example, just as terpenoid carboxylic acids can be a mixture of several types, their ammonium salts or salts with amines can also be a mixture of several types. It's not even close.
これらの印刷物で、膜面の良好なものを酸素雰２了７、
−７
囲気中、了００′Ｃで１時間加熱すると、膜厚２００Ｏ
Ａ程度の黒色の酸化物薄膜が得られた。Among these printed materials, those with good film surfaces are placed in an oxygen atmosphere.
-7 When heated for 1 hour at 00'C in an ambient atmosphere, a film thickness of 200O
A black oxide thin film of grade A was obtained.
これらの結晶形をＸ線回折で調べたところ、超伝導酸化
物焼結体の結晶形と同様であることが分った。四探針法
で測定したこれら薄膜の超伝導転移温度（転移の終了す
る温度）は、４０〜８０にの範囲でばらつき、組成によ
る系統的な依存性は特に昆られなかった。When these crystal forms were examined by X-ray diffraction, it was found that they were similar to the crystal form of the superconducting oxide sintered body. The superconducting transition temperatures (temperatures at which the transition ends) of these thin films measured by the four-probe method varied in the range of 40 to 80, and there was no particular systematic dependence on composition.
（実施例５）
実施例４で調製したインキのうち、良好な膜を製造でき
るものを用いて、アルミナ基板、ジルコニア基板及びス
テンレス基板上に、実施例４と同じ条件でスクリーン印
刷を行った。これらの基板上でも外観品質の良好な膜が
形成された。これらを実施例４と同様に乾燥し、酸素雰
囲気中で８００℃、１時間の加熱焼成を行って、酸化物
薄膜を得た。これらの結晶形は実施例４と同様であシ、
その超伝導転移温度は、アルミナ基板では４０〜８０Ｋ
、ジルコニア基板では６６〜８０Ｋ、ステンレス基板で
は５Ｑ〜７５にであった。(Example 5) Among the inks prepared in Example 4, screen printing was performed on an alumina substrate, a zirconia substrate, and a stainless steel substrate under the same conditions as in Example 4 using an ink that could produce a good film. Films with good appearance quality were also formed on these substrates. These were dried in the same manner as in Example 4, and fired at 800° C. for 1 hour in an oxygen atmosphere to obtain an oxide thin film. These crystal forms are the same as in Example 4,
The superconducting transition temperature is 40-80K for an alumina substrate.
, 66 to 80K for the zirconia substrate, and 5Q to 75 for the stainless steel substrate.
（実施例６）
実施例４で調製したインキ組成のうち、良好な膜を与え
る増粘剤組成のものについて、金属化合物含有量を２倍
にしてインキを調製した。これらのインキをアルミナ基
板及びジルコニア基板上に実施例４と同じ条件でスクリ
ーン印刷し、実施例６と同じ条件で乾燥、焼成して酸化
物薄膜を製造した。これらにおいては、電気的な導通の
とれないものはなく、超伝導特性は実施例６とほぼ同じ
であった。(Example 6) Of the ink compositions prepared in Example 4, the thickener composition that gave a good film was doubled in content of the metal compound to prepare an ink. These inks were screen printed on an alumina substrate and a zirconia substrate under the same conditions as in Example 4, and dried and fired under the same conditions as in Example 6 to produce an oxide thin film. None of these had electrical conductivity, and the superconducting properties were almost the same as in Example 6.
発明の効果
以上の実施例から明らかなように、本発明の超伝導酸化
物薄膜形成用スクリーン印刷インキおよびこのインキを
使用した超伝導酸化物薄膜の形成方法によれば、非常に
品質の良い超伝導酸化物薄膜をスクリーン印刷という簡
便な工法でパターン状に製造できるのでその工業上の効
果は大きいものである。Effects of the Invention As is clear from the above examples, the screen printing ink for forming a superconducting oxide thin film of the present invention and the method for forming a superconducting oxide thin film using this ink produce very high quality superconducting oxide films. The conductive oxide thin film can be manufactured in a pattern by the simple method of screen printing, which has great industrial effects.
Claims (4)
をそれぞれに含まれる金属の原子比で１：２：３の割合
で混合し、増粘剤としてテルペノイドのカルボン酸又は
それらのエステルと、これにテルペノイドのカルボン酸
のアンモニウム塩又はアミン類との塩を添加するととも
に、溶剤を添加混練したことを特徴とする超伝導酸化物
薄膜形成用スクリーン印刷インキ。(1) Mix a yttrium compound, a barium compound, and a copper compound at an atomic ratio of 1:2:3 of the metals contained in each compound, add terpenoid carboxylic acid or their ester as a thickener, and add terpenoid carboxylic acid or ester thereof as a thickener. A screen printing ink for forming a superconducting oxide thin film, characterized in that an ammonium salt of carboxylic acid or a salt with amines is added, and a solvent is added and kneaded.
をそれぞれに含まれる金属の原子比で１：２：３の割合
で混合し、増粘剤としてアビエチン酸のジエチルアミン
塩、アビエチン酸のトリエチルアミン塩、アビエチン酸
のイソプロピルアミン塩、ロジンのイソプロピルアミン
塩、ロジンのｎ−ヘキシルアミン塩、ｎ−オクチルアミ
ン塩の少なくともいずれかを添加するとともに、溶剤を
添加混練したことを特徴とする超伝導酸化物薄膜形成用
スクリーン印刷インキ。(2) Mix a yttrium compound, a barium compound, and a copper compound at an atomic ratio of 1:2:3 of the metals contained in each, and use diethylamine salt of abietic acid, triethylamine salt of abietic acid, and abietic acid as thickeners. for forming a superconducting oxide thin film, characterized in that at least one of isopropylamine salt of , isopropylamine salt of rosin, n-hexylamine salt of rosin, and n-octylamine salt is added, and a solvent is added and kneaded. screen printing ink.
をそれぞれに含まれる金属の原子比で１：２：３の割合
で混合し、増粘剤としてテルペノイドのカルボン酸又は
それらのエステルと、これにテルペノイドのカルボン酸
のアンモニウム塩又はアミン類との塩を添加するととも
に、溶剤を添加混練したインキを基体上にスクリーン印
刷する工程と、この被印刷物を乾燥し、酸素雰囲気中で
加熱焼成する工程とからなることを特徴とする超伝導酸
化物薄膜の形成方法。(3) Mix a yttrium compound, a barium compound, and a copper compound at an atomic ratio of 1:2:3 of the metals contained in each, add terpenoid carboxylic acid or their ester as a thickener, and add terpenoid carboxylic acid or ester thereof as a thickener. It consists of a step of screen printing an ink prepared by adding an ammonium salt of carboxylic acid or a salt with amines and a solvent and kneading it onto a substrate, and a step of drying this printing material and heating and baking it in an oxygen atmosphere. A method for forming a superconducting oxide thin film, characterized by:
をそれぞれに含まれる金属の原子比で１：２：３の割合
で混合し、増粘剤としてアビエチン酸のジエチルアミン
塩、アビエチン酸のトリエチルアミン塩、アビエチン酸
のイソプロピルアミン塩、ロジンのイソプロピルアミン
塩、ロジンのｎ−ヘキシルアミン塩、ｎ−オクチルアミ
ン塩の少なくともいずれかを添加するとともに、溶剤を
添加混練したインキを基体上にスクリーン印刷する工程
と、この被印刷物を乾燥し、酸素雰囲気中で加熱焼成す
る工程とからなることを特徴とする超伝導酸化物薄膜の
形成方法。(4) Mix a yttrium compound, a barium compound, and a copper compound at an atomic ratio of 1:2:3 of the metals contained in each, and use diethylamine salt of abietic acid, triethylamine salt of abietic acid, and abietic acid as thickeners. a step of adding at least one of isopropylamine salt of isopropylamine salt, isopropylamine salt of rosin, n-hexylamine salt of rosin, and n-octylamine salt, as well as adding and kneading a solvent, and screen-printing the ink on the substrate; A method for forming a superconducting oxide thin film, comprising the steps of drying a printing material and heating and baking it in an oxygen atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63311076A JPH02157121A (en) | 1988-12-08 | 1988-12-08 | Screen printing ink for forming superconducting oxide thin film and formation of superconducting oxide thin film using this ink |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63311076A JPH02157121A (en) | 1988-12-08 | 1988-12-08 | Screen printing ink for forming superconducting oxide thin film and formation of superconducting oxide thin film using this ink |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02157121A true JPH02157121A (en) | 1990-06-15 |
Family
ID=18012828
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63311076A Pending JPH02157121A (en) | 1988-12-08 | 1988-12-08 | Screen printing ink for forming superconducting oxide thin film and formation of superconducting oxide thin film using this ink |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02157121A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0743284A1 (en) * | 1995-05-15 | 1996-11-20 | Matsushita Electric Industrial Co., Ltd | Paste for manufacturing ferrite and ferrite |
-
1988
- 1988-12-08 JP JP63311076A patent/JPH02157121A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0743284A1 (en) * | 1995-05-15 | 1996-11-20 | Matsushita Electric Industrial Co., Ltd | Paste for manufacturing ferrite and ferrite |
| US5698131A (en) * | 1995-05-15 | 1997-12-16 | Matsushita Electric Industrial Co., Ltd. | Paste for manufacturing ferrite and ferrite |
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