JP2013115132A - Metal oxide semiconductor particle dispersion body composition and semiconductor - Google Patents
Metal oxide semiconductor particle dispersion body composition and semiconductor Download PDFInfo
- Publication number
- JP2013115132A JP2013115132A JP2011257954A JP2011257954A JP2013115132A JP 2013115132 A JP2013115132 A JP 2013115132A JP 2011257954 A JP2011257954 A JP 2011257954A JP 2011257954 A JP2011257954 A JP 2011257954A JP 2013115132 A JP2013115132 A JP 2013115132A
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- Prior art keywords
- metal oxide
- oxide semiconductor
- group
- dispersant
- particle dispersion
- Prior art date
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- 239000002245 particle Substances 0.000 title claims abstract description 66
- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 53
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 53
- 239000006185 dispersion Substances 0.000 title claims abstract description 49
- 239000000203 mixture Substances 0.000 title claims abstract description 32
- 239000002270 dispersing agent Substances 0.000 claims abstract description 57
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 23
- 239000002904 solvent Substances 0.000 claims abstract description 13
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- 125000005702 oxyalkylene group Chemical group 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 4
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- 125000000217 alkyl group Chemical group 0.000 claims description 10
- 125000005647 linker group Chemical group 0.000 claims description 7
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Abstract
Description
本発明は、金属酸化物半導体粒子分散体組成物および半導体に関し、より詳細には、金属酸化物半導体粒子の含有量が多く、しかも分散性に優れ、塗工後において緻密性、均一性、表面平滑性に優れた半導体膜を得ることができる金属酸化物半導体粒子分散体組成物、およびこれを用いた半導体に関する。 The present invention relates to a metal oxide semiconductor particle dispersion composition and a semiconductor, and more specifically, has a high content of metal oxide semiconductor particles, excellent dispersibility, denseness, uniformity and surface after coating. The present invention relates to a metal oxide semiconductor particle dispersion composition capable of obtaining a semiconductor film having excellent smoothness, and a semiconductor using the same.
酸化インジウム−酸化ガリウム−酸化亜鉛（ＩＧＺＯ）などの金属酸化物からなる半導体は、電極材料等として広く使用されている。従来、これらの金属酸化物からなる電極等を製造する方法として、真空蒸着やスパッタリングなどが用いられている。しかし、これらの方法は、製造に長時間を要し、また、特殊な装置を必要とするなど、生産性に関しての問題がある。 A semiconductor made of a metal oxide such as indium oxide-gallium oxide-zinc oxide (IGZO) is widely used as an electrode material. Conventionally, vacuum deposition, sputtering, or the like has been used as a method for producing an electrode made of these metal oxides. However, these methods have problems related to productivity, such as requiring a long time for production and requiring special equipment.
最近、生産性を向上させる方法として、金属酸化物半導体からなるナノ粒子を分散剤を用いて分散させ、得られる分散体を塗布・乾燥することにより半導体膜を形成する方法が提案されている。例えば、特許文献１では、ステアリン酸などのアルキルカルボン酸を分散剤として用いることが記載されている。 Recently, as a method for improving productivity, a method of forming a semiconductor film by dispersing nanoparticles made of a metal oxide semiconductor using a dispersant and applying and drying the obtained dispersion is proposed. For example, Patent Document 1 describes using an alkyl carboxylic acid such as stearic acid as a dispersant.
しかしながら、この従来技術により得られる半導体膜は、緻密性、均一性、表面平滑性等の点において十分ではなく、また、分散剤の添加量が多いため、相対的に金属酸化物半導体粒子の含有量が低くなり、半導体としての性能も低下してしまうという問題点がある。 However, the semiconductor film obtained by this conventional technique is not sufficient in terms of denseness, uniformity, surface smoothness, and the like, and since the amount of the dispersant added is large, the metal oxide semiconductor particles are relatively contained. There is a problem that the amount becomes low and the performance as a semiconductor also deteriorates.
本発明は従来技術の有するこのような問題点に鑑みてなされたものであって、本発明の課題は、分散剤の使用量が少なく、緻密性、均一性、表面平滑性に優れた半導体膜を簡便な方法で得ることができる金属酸化物半導体粒子分散体組成物を提供することであり、また、そのような半導体を提供することである。 The present invention has been made in view of such problems of the prior art, and the object of the present invention is to reduce the amount of dispersant used and to provide a semiconductor film excellent in denseness, uniformity, and surface smoothness. It is to provide a metal oxide semiconductor particle dispersion composition that can be obtained by a simple method, and to provide such a semiconductor.
本発明の金属酸化物半導体粒子分散体組成物は、平均粒子径が１〜１００ｎｍである金属酸化物半導体粒子と、下記式（１）で示される化合物からなる分散剤と、溶媒とを含有することを特徴とする。 The metal oxide semiconductor particle dispersion composition of the present invention contains metal oxide semiconductor particles having an average particle diameter of 1 to 100 nm, a dispersant composed of a compound represented by the following formula (1), and a solvent. It is characterized by that.
ここで、式（１）のＲは、分岐鎖を有し炭素数が３〜２４のアルキル基またはアルケニル基であり、ＡＯは炭素数が１ないし４のオキシアルキレン基であり、ｎはアルキレンオキシドの平均付加モル数を示す５〜３０の範囲の数値であり、Ｘは炭素原子、水素原子及び／又は酸素原子からなる連結基である。 Here, R in the formula (1) is a branched chain alkyl group or alkenyl group having 3 to 24 carbon atoms, AO is an oxyalkylene group having 1 to 4 carbon atoms, and n is an alkylene oxide. Is a numerical value in the range of 5 to 30 indicating the average number of moles added, and X is a linking group comprising a carbon atom, a hydrogen atom and / or an oxygen atom.
ここで、前記分散剤における前記式（１）のＸは、炭素数が１ないし１５のアルキレン基であることが好ましい。 Here, X in the formula (1) in the dispersant is preferably an alkylene group having 1 to 15 carbon atoms.
また、前記分散剤における前記式（１）のＸは、下記式（２）で示される連結基であることを特徴とする請求項１記載の金属酸化物半導体粒子分散体組成物。 2. The metal oxide semiconductor particle dispersion composition according to claim 1, wherein X in the formula (1) in the dispersant is a linking group represented by the following formula (2).
ただし、式（２）のＹは、炭素数が１ないし１５のアルキレン基、ビニレン基、フェニレン基およびカルボキシル基含有フェニレン基の中から選択されるいずれかである。 However, Y in the formula (2) is any selected from an alkylene group having 1 to 15 carbon atoms, a vinylene group, a phenylene group, and a carboxyl group-containing phenylene group.
また、上記において、前記金属酸化物半導体粒子を１００重量％とした場合に、前記分散剤の配合量が１〜３０重量％であることが好ましい。 Moreover, in the above, when the metal oxide semiconductor particles are 100% by weight, the blending amount of the dispersant is preferably 1 to 30% by weight.
本発明の半導体は、上記の何れかの金属酸化物半導体粒子分散体組成物を塗工してなることを特徴とする。 The semiconductor of the present invention is formed by coating any of the above metal oxide semiconductor particle dispersion compositions.
本発明の金属酸化物半導体粒子分散体組成物を使用すれば、分散剤の使用量が少ないにもかかわらず分散性に優れ、得られる塗工膜の緻密性、均一性、表面平滑性に優れた半導体膜を簡便な方法で得ることができる。 If the metal oxide semiconductor particle dispersion composition of the present invention is used, the dispersibility is excellent despite the small amount of the dispersant used, and the resulting coating film has excellent denseness, uniformity, and surface smoothness. The semiconductor film can be obtained by a simple method.
１．分散質粒子
本発明の金属酸化物半導体粒子分散体組成物における金属酸化物半導体として代表的なものは、酸化インジウム−酸化ガリウム−酸化亜鉛（ＩＧＺＯ）、酸化インジウム−酸化亜鉛（ＩＺＯ）、酸化亜鉛−酸化スズ（ＺＴＯ）等を挙げることができる。これらの金属酸化物半導体粒子は、媒体中から安定に取り出す為に、アルカン酸類や脂肪酸類、ヒドロキシカルボン酸類、脂環族、芳香族カルボン酸類、アルケニルコハク酸無水物類、チオール類、フェノール誘導体類、アミン類、両親媒性ポリマー、高分子界面活性剤、低分子界面活性剤などの保護剤で被覆されていてもよい。
1. Dispersoid particles Typical examples of the metal oxide semiconductor in the metal oxide semiconductor particle dispersion composition of the present invention include indium oxide-gallium oxide-zinc oxide (IGZO), indium oxide-zinc oxide (IZO), and zinc oxide. -Tin oxide (ZTO) etc. can be mentioned. These metal oxide semiconductor particles are used for alkanoic acids, fatty acids, hydroxycarboxylic acids, alicyclic, aromatic carboxylic acids, alkenyl succinic anhydrides, thiols, and phenol derivatives for stable removal from the medium. , Amines, amphiphilic polymers, polymeric surfactants, low molecular surfactants and other protective agents.
本発明において分散剤により分散される金属酸化物半導体粒子は、平均粒子径が１〜１００ｎｍのものであり、結晶状であってもアモルファス状であってもよい。また、本発明における分散剤により分散される金属酸化物半導体粒子は等方性粒子であっても異方性粒子であってもよく、繊維状であってもよい。 In the present invention, the metal oxide semiconductor particles dispersed by the dispersant have an average particle diameter of 1 to 100 nm and may be crystalline or amorphous. In addition, the metal oxide semiconductor particles dispersed by the dispersant in the present invention may be isotropic particles, anisotropic particles, or fibrous.
本発明で被分散質となる金属酸化物半導体粒子は、公知の方法で得たものが使用できる。微粒子の調製方法としては、粗大粒子を機械的に解砕、微細化していくトップダウン方式と、いくつかの単位粒子を生成させ、それが凝集したクラスター状態を経由して粒子が形成されるボトムアップ方式の２通りの方式があるが、いずれの方法で調製されたものであっても好適に使用できる。また、それらは湿式法、乾式法のいずれの方法によるものであってもよい。また、ボトムアップ方式には、物理的方法と化学的方法があるが、いずれの方法によるものであってもよい。本発明における分散剤は、粗大粒子を機械的に解砕、微細化していくトップダウン方式の工程中で使用してもよく、いくつかの単位粒子を生成させ、それが凝集したクラスター状態を経由して粒子が形成されるボトムアップ方式の工程中で使用してもよく、或いは、事前に前記方法で微粒子を調製後、該分散質粒子を媒体中から安定に取り出すために表面修飾剤や表面保護剤と称する公知の保護剤で被覆或いは含浸させて取り出された粒子を使用することもできる。保護剤としては前記の公知分散剤で代用することができる。 What was obtained by the well-known method can be used for the metal oxide semiconductor particle used as a to-be-dispersed material by this invention. As a method for preparing fine particles, a top-down method in which coarse particles are mechanically pulverized and refined, and a bottom in which particles are formed through a cluster state in which several unit particles are generated and aggregated. Although there are two types of up systems, any one prepared by any method can be suitably used. Further, they may be either a wet method or a dry method. The bottom-up method includes a physical method and a chemical method, and any method may be used. The dispersant in the present invention may be used in a top-down process in which coarse particles are mechanically pulverized and refined to form several unit particles, which pass through a cluster state in which they are aggregated. May be used in a bottom-up process in which particles are formed, or after preparing fine particles in advance by the above-described method, a surface modifier or surface may be used to stably remove the dispersoid particles from the medium. It is also possible to use particles taken out by being coated or impregnated with a known protective agent called a protective agent. As the protective agent, the above-mentioned known dispersants can be substituted.
ボトムアップ方式をより具体的に説明するために、前記分散質粒子の内、金属ナノ粒子の調製法を例示する。ボトムアップ方式の内、物理的方法の代表例としてはバルク金属を不活性ガス中で蒸発させ、ガスとの衝突により冷却凝縮させてナノ粒子を生成するガス中蒸発法がある。また、化学的方法には、液相中で保護剤の存在下で金属イオンを還元し、生成した０価の金属をナノサイズで安定化させる液相還元法や金属錯体の熱分解法などがある。液相還元法としては、化学的還元法、電気化学的還元法、光還元法、または化学的還元法と光照射法を組み合わせた方法などを利用することができる。 In order to more specifically explain the bottom-up method, a method for preparing metal nanoparticles among the dispersoid particles will be exemplified. Among the bottom-up methods, a representative example of a physical method is an in-gas evaporation method in which bulk metal is evaporated in an inert gas and cooled and condensed by collision with the gas to generate nanoparticles. Chemical methods include a liquid phase reduction method in which metal ions are reduced in the liquid phase in the presence of a protective agent, and the generated zero-valent metal is stabilized at the nanosize, and a metal complex thermal decomposition method. is there. As the liquid phase reduction method, a chemical reduction method, an electrochemical reduction method, a photoreduction method, a method combining a chemical reduction method and a light irradiation method, or the like can be used.
また、本発明で好適に使用できる分散質粒子は、前記の如く、トップダウン方式、ボトムアップ方式のいずれも手法で得たものであってもよく、それらは水系、非水系、気相中のいずれの環境下で調製されたものであってもよい。なお、これらの分散質粒子ReturningPointReturningPointを使用する際には、各種溶媒に分散質粒子をあらかじめ分散したものを使用してもよい。 Further, as described above, the dispersoid particles that can be suitably used in the present invention may be those obtained by any of the top-down method and the bottom-up method, and they are aqueous, non-aqueous, and in the gas phase. It may be prepared in any environment. In addition, when using these dispersoid particles ReturningPointReturningPoint, you may use what disperse | distributed particle | grains disperse | distributed previously in various solvents.
分散質粒子の平均粒径は、５〜１００ｎｍの範囲内であることが好ましい。 The average particle size of the dispersoid particles is preferably in the range of 5 to 100 nm.
２．分散剤の疎水基（Ｒ）について
本発明における分散剤の疎水基（Ｒ）は、分岐鎖を有し炭素数が３〜２４のアルキル基またはアルケニル基を含んでいる。分岐鎖を有し炭素数が３〜２４のアルキル基またはアルケニル基の含有量は、Ｒの全体に対して７０重量％以上であることが好ましい。
2. About the hydrophobic group (R) of the dispersant
The hydrophobic group (R) of the dispersant in the present invention contains a branched chain alkyl group or alkenyl group having 3 to 24 carbon atoms. The content of the branched chain alkyl group or alkenyl group having 3 to 24 carbon atoms is preferably 70% by weight or more based on the total of R.
Ｒの生成に使用し得る原料アルコールの炭素数は、単一であっても異なる炭素数のアルコールの混合物であってもよい。また、その原料アルコールは合成由来であっても天然由来であってもよく、また、その化学構造は単一組成であっても複数の異性体からなる混合物であってもよい。使用できる原料アルコールは公知のものが選択できるが、具体例としては、合成由来のブタノール、イソブタノール、ペンタノール及び／又はその異性体、ヘキサノール及び／又はその異性体、ヘプタノール及び／又はその異性体、オクタノール及び／又はその異性体、３，５，５−トリメチル−１−ヘキサノールの他、プロピレン或いはブテン、又はその混合物から誘導される高級オレフィンを経てオキソ法によって製造されるイソノナノール、イソデカノール、イソウンデカノール、イソドデカノール、イソトリデカノール、シェルケミカルズ社製のネオドール２３、２５、４５、サソール社製のＳＡＦＯＬ２３、エクソン・モービル社製のＥＸＸＡＬ７、ＥＸＸＡＬ８Ｎ、ＥＸＸＡＬ９、ＥＸＸＡＬ１０、ＥＸＸＡＬ１１及びＥＸＸＡＬ１３も好適に使用できる高級アルコールの一例である。更に天然由来のオクチルアルコール、デシルアルコール、ラウリルアルコール（１−ドデカノール）、ミリスチルアルコール（１−テトラデカノール）、セチルアルコール（１−ヘキサデカノール）、ステアリルアルコール（１−オクタデカノール）、オレイルアルコール（ｃｉｓ−９−オクタデセン−１−オール）なども使用できる高級アルコールの一例である。また、２−アルキル−１−アルカノール型の化学構造をもつゲルベアルコール（Ｇｕｅｒｂｅｔ Ａｌｃｏｈｏｌ）類の単一組成、或いはその混合物なども好適に使用できる高級アルコールの一例であり、２−エチル−１−ヘキサノール、２−プロピル−１−ヘキサノール、２−ブチル−１−ヘキサノール、２−エチル−１−ヘプタノール、２−プロピル−１−ヘプタノール、２−エチル−１−オクタノール、２−ヘキシル−１−デカノール、２−ヘプチル−１−ウンデカノール、２−オクチル−１−ドデカノール、２−デシル−1−テトラデカノールの他、分岐アルコールから誘導されるイソステアリルアルコールなどがある。また、上記各種アルコールを２種以上配合して使用することも可能である。但し、本発明における分散剤では、前記の如く疎水基（Ｒ）は、炭素数３〜２４の分岐型のアルキル基及び／又はアルケニル基を含むものである。 The raw material alcohol that can be used to generate R may have a single carbon number or a mixture of alcohols having different carbon numbers. The raw material alcohol may be synthetically or naturally derived, and the chemical structure may be a single composition or a mixture of a plurality of isomers. As the raw material alcohol that can be used, known alcohols can be selected. Specific examples include butanol, isobutanol, pentanol and / or its isomer, hexanol and / or its isomer, heptanol and / or its isomer derived from synthesis. , Octanol and / or its isomer, 3,5,5-trimethyl-1-hexanol, isononanol, isodecanol, isounol produced by the oxo process via higher olefins derived from propylene or butene, or mixtures thereof Decanol, isododecanol, isotridecanol, Neodol 23, 25, 45 manufactured by Shell Chemicals, SAFOL23 manufactured by Sasol, EXXAL7, EXXAL8N, EXXAL9, EXXAL10, EXXXAL11 and EXXXA manufactured by Exxon Mobil 13 illustrates another example of a higher alcohol which can be suitably used. Furthermore, natural octyl alcohol, decyl alcohol, lauryl alcohol (1-dodecanol), myristyl alcohol (1-tetradecanol), cetyl alcohol (1-hexadecanol), stearyl alcohol (1-octadecanol), oleyl alcohol (Cis-9-octadecen-1-ol) and the like are also examples of higher alcohols that can be used. In addition, a single composition of Guerbet Alcohol having a 2-alkyl-1-alkanol type chemical structure, or a mixture thereof is an example of a higher alcohol that can be suitably used. 2-ethyl-1-hexanol 2-propyl-1-hexanol, 2-butyl-1-hexanol, 2-ethyl-1-heptanol, 2-propyl-1-heptanol, 2-ethyl-1-octanol, 2-hexyl-1-decanol, 2 In addition to heptyl-1-undecanol, 2-octyl-1-dodecanol, 2-decyl-1-tetradecanol, there are isostearyl alcohols derived from branched alcohols. Moreover, it is also possible to mix | blend and use 2 or more types of said various alcohol. However, in the dispersant of the present invention, as described above, the hydrophobic group (R) contains a branched alkyl group and / or alkenyl group having 3 to 24 carbon atoms.
なお、疎水基（Ｒ）が水素或いは炭素数が１〜２の炭化水素基である場合、炭素数が２５を超える場合、および疎水基（Ｒ）の炭素数が３〜２４の範囲にある場合でも直鎖型のアルキル基及び／又はアルケニル基の含有量が３０重量％を超える場合には、分散媒中で分散質を安定に分散させることができないか、又は使用できる分散媒の選択範囲が限定されたり、分散体の調製工程において異種の分散媒への置換や混合が生じることがある。その結果、分散体の安定性が著しく低下して直ちに沈降物を生じたり、経時安定性が著しく低下して最終製品の付加価値低下、生産性低下、加工特性低下および品質劣化などの問題を生じる。これらの問題を回避し、更に本発明において分散剤の作用を特に効果的なものにするためには、疎水基（Ｒ）は炭素数８〜１８の分岐型のアルキル基であることがより好ましい。 In addition, when the hydrophobic group (R) is hydrogen or a hydrocarbon group having 1 to 2 carbon atoms, when the carbon number exceeds 25, and when the hydrophobic group (R) has a carbon number in the range of 3 to 24 However, when the content of the linear alkyl group and / or alkenyl group exceeds 30% by weight, the dispersoid cannot be stably dispersed in the dispersion medium, or the selection range of the dispersion medium that can be used is It may be limited, or substitution or mixing with a different type of dispersion medium may occur in the dispersion preparation process. As a result, the stability of the dispersion is significantly reduced, resulting in immediate sedimentation, and the stability over time is significantly reduced, resulting in problems such as a decrease in added value, productivity, processing characteristics, and quality deterioration of the final product. . In order to avoid these problems and make the action of the dispersant particularly effective in the present invention, the hydrophobic group (R) is more preferably a branched alkyl group having 8 to 18 carbon atoms. .
３．分散剤のオキシアルキレン基（ＡＯ）n
本発明において分散剤に好適に選択されるアルキレンオキシド種について、式（１）におけるＡＯは炭素数１ないし４のオキシアルキレン基を示すものであり、具体的には炭素数２のアルキレンオキシドはエチレンオキシドである。炭素数３のアルキレンオキシドはプロピレンオキシドである。炭素数４のアルキレンオキシドは、テトラヒドロフラン或いはブチレンオキシドであるが、好ましくは、１，２−ブチレンオキシドまたは２，３−ブチレンオキシドである。分散剤におけるオキシアルキレン鎖（−（ＡＯ）n−）は分散剤の分散媒親和性を調整する目的を果たし、アルキレンオキシドは単独重合鎖であっても、２種以上のアルキレンオキサイドのランダム重合鎖でもブロック重合鎖でもよく、また、その組み合わせであってもよい。式（１）のアルキレンオキシドの平均付加モル数を示すｎは１ないし３０の範囲であるが、３ないし２０の範囲にあることが好ましい。
3. Dispersant oxyalkylene group (AO) n
In the alkylene oxide species preferably selected as the dispersant in the present invention, AO in the formula (1) represents an oxyalkylene group having 1 to 4 carbon atoms, specifically, an alkylene oxide having 2 carbon atoms is ethylene oxide. It is. The alkylene oxide having 3 carbon atoms is propylene oxide. The alkylene oxide having 4 carbon atoms is tetrahydrofuran or butylene oxide, preferably 1,2-butylene oxide or 2,3-butylene oxide. The oxyalkylene chain (-(AO) n-) in the dispersant serves the purpose of adjusting the dispersion medium affinity of the dispersant. Even if the alkylene oxide is a homopolymer chain, it is a random polymer chain of two or more alkylene oxides. However, it may be a block polymer chain or a combination thereof. N which shows the average added mole number of the alkylene oxide of Formula (1) is in the range of 1 to 30, but is preferably in the range of 3 to 20.
４．分散剤の連結基（Ｘ）
連結基（Ｘ）は炭素原子、水素原子、酸素原子からなる公知の構造から選択可能であるが、好ましくは飽和炭化水素基、不飽和炭化水素基、エーテル基、カルボニル基、エステル基からなり、脂環構造、芳香環構造を有していてもよく、また、繰り返し単位を有していてもよい。連結基Ｘに窒素原子及び／又は硫黄原子及び／又はリン原子などを含む場合は、カルボキシル基の分散質への親和効果を弱める作用があるために本発明における分散剤の構造因子としては適さない。
4). Dispersing agent linking group (X)
The linking group (X) can be selected from a known structure consisting of a carbon atom, a hydrogen atom, and an oxygen atom, preferably a saturated hydrocarbon group, an unsaturated hydrocarbon group, an ether group, a carbonyl group, or an ester group. It may have an alicyclic structure or an aromatic ring structure, and may have a repeating unit. When the linking group X contains a nitrogen atom and / or a sulfur atom and / or a phosphorus atom, it has an action of weakening the affinity effect of the carboxyl group on the dispersoid, and thus is not suitable as a structural factor of the dispersant in the present invention. .
また、式（１）のＸは炭素数が１ないし１５のアルキレン基であることが好ましく、炭素数が１ないし８のアルキレン基であることがより好ましい。 X in the formula (1) is preferably an alkylene group having 1 to 15 carbon atoms, and more preferably an alkylene group having 1 to 8 carbon atoms.
また、式（１）のＸは、前述の式（２）で示される物質であることが好ましい。ただし、式（２）におけるＹは、炭素数が１ないし１５のアルキレン基、ビニレン基、フェニレン基およびカルボキシル基含有フェニレン基の中から選択されるいずれかである。 Further, X in the formula (1) is preferably a substance represented by the above formula (2). However, Y in Formula (2) is any selected from an alkylene group having 1 to 15 carbon atoms, a vinylene group, a phenylene group, and a carboxyl group-containing phenylene group.
５．一層好ましい分散剤
本発明においては、下記式（３）に記載の分散剤を使用することが一層好ましい。
5. More preferable dispersant In the present invention, it is more preferable to use a dispersant described in the following formula (3).
但し、式（３）においてＲは炭素数が８ないし１８であって分岐鎖を有するアルキル基が好適であり、ｎはエチレンオキシドの平均付加モル数を示し、３ないし２０の範囲が好適である。分散剤の組成をこの範囲に限定することで、分散体の調製に使用できる分散媒の選択範囲の拡大、異種の分散媒の混合、置換に対する適用性が向上する。このように、分散剤の組成範囲を限定することで、分散体の経時安定性に対して更に好適に作用し、その結果、最終製品の付加価値向上、生産性向上、加工特性向上および品質安定化などを達成できる。 However, in formula (3), R is preferably an alkyl group having 8 to 18 carbon atoms and having a branched chain, and n represents the average number of moles of ethylene oxide added, preferably in the range of 3 to 20. By limiting the composition of the dispersant to this range, the applicability to expansion of the selection range of the dispersion medium that can be used for preparation of the dispersion, mixing of different types of dispersion medium, and substitution is improved. In this way, by limiting the composition range of the dispersant, it works more favorably with respect to the stability of the dispersion over time. As a result, the added value of the final product is improved, the productivity is improved, the processing characteristics are improved, and the quality is stable. Can be achieved.
６．分散剤の配合量
本発明における分散剤の配合量は特に限定されるものではないが、分散質粒子である金属酸化物半導体粒子１００重量％に対して、１〜３０重量％であり、３〜２０重量％が好ましく、３〜１５重量％がより好ましく、５〜１０重量％がさらに好ましい。
6). The compounding amount of the dispersant is not particularly limited, but is 1 to 30% by weight with respect to 100% by weight of the metal oxide semiconductor particles as the dispersoid particles, and 3 to 3%. 20 weight% is preferable, 3-15 weight% is more preferable, and 5-10 weight% is further more preferable.
７．分散剤の製造方法
本発明における分散剤は公知の方法で製造することができる。例えば、アルコール、アミン、チオールに公知の方法でアルキレンオキシドを付加した一般的な非イオン界面活性剤化合物を原料として、モノハロゲン化低級カルボン酸またはその塩を用い、塩基存在下でアルキレンオキシド末端の水酸基と反応させる方法、または、酸無水物を用いてアルキレンオキシド末端の水酸基との開環反応による方法により製造することができるが、これらの方法に限定されるものではない。
7). Dispersant Production Method The dispersant in the present invention can be produced by a known method. For example, using a general nonionic surfactant compound obtained by adding an alkylene oxide to an alcohol, amine, or thiol by a known method as a raw material, a monohalogenated lower carboxylic acid or a salt thereof is used. Although it can manufacture by the method of making it react with a hydroxyl group, or the method of ring-opening reaction with the hydroxyl group of the alkylene oxide terminal using an acid anhydride, it is not limited to these methods.
また、前述の範囲で疎水基の種類、アルキレンオキシド種とその付加形態、付加モル量、連結基などを特に限定して組成を最適選定することにより、公知の分散剤よりも、より広範な種類の分散質を分散でき、より広範な種類の分散媒に分散質を分散安定化できる点で産業上の利用価値は大きい。 In addition, the types of hydrophobic groups, alkylene oxide types and addition forms thereof, addition molar amounts, linking groups, etc. are particularly limited within the above-mentioned range, so that a wider range of types than known dispersants can be selected. The industrial utility value is great in that it can disperse various dispersoids and can disperse and stabilize the dispersoids in a wider variety of dispersion media.
また、本発明に使用される分散剤は、公知の精製法により含有するイオン種、特にアルカリ金属イオン、アルカリ土類金属イオン、重金属イオン、ハロゲンイオンの各イオンの含有量を低減して用いることができる。分散剤中のイオン種は分散体の分散安定性、耐触性、耐酸化性、分散塗膜の電気特性（導電特性、絶縁特性）、経時安定性、耐熱性、低湿性、耐候性に大きく影響するため、上記イオンの含有量は適宜決定することができるが、分散剤中で１０ｐｐｍ未満であることが望ましい。 In addition, the dispersant used in the present invention should be used by reducing the content of ionic species, particularly alkali metal ions, alkaline earth metal ions, heavy metal ions, and halogen ions, contained by a known purification method. Can do. The ionic species in the dispersant is greatly affected by the dispersion stability, touch resistance, oxidation resistance, electrical properties (conductive properties, insulation properties), aging stability, heat resistance, low humidity, and weather resistance of the dispersion. However, it is desirable that the content of the ions is less than 10 ppm in the dispersant.
また、本発明の金属酸化物半導体粒子分散体組成物は公知の撹拌手段、均一化手段、分散化手段を用いて調製することができる。採用することができる分散機の一例としては、２本ロール、３本ロールなどのロールミル、ボールミル、振動ボールミルなどのボールミル、ペイントシェーカー、連続ディスク型ビーズミル、連続アニュラー型ビーズミルなどのビーズミル、サンドミル、ジェットミルなどが挙げられる。また、超音波発生浴中において分散処理を行うことも出来る。 In addition, the metal oxide semiconductor particle dispersion composition of the present invention can be prepared using known stirring means, homogenizing means, and dispersing means. Examples of dispersers that can be adopted include roll mills such as two rolls and three rolls, ball mills such as ball mills and vibration ball mills, paint shakers, continuous disk type bead mills, bead mills such as continuous annular type bead mills, sand mills, and jets. Mill etc. are mentioned. Further, the dispersion treatment can be performed in an ultrasonic wave generation bath.
８．溶媒
本発明で使用できる分散媒としては、トルエン、キシレン、芳香族炭化水素系溶剤、ｎ−ヘキサン、シクロヘキサン、ｎ−ヘプタンなどの炭化水素系溶剤、塩化メチレン、クロロホルム、ジクロロエタンなどのハロゲン化炭化水素系溶剤、エチルエーテル、イソプロピルエーテル、ジオキサン、テトラヒドロフラン、ジブチルエーテル、ブチルエチルエーテル、メチル−ｔ−ブチルエーテル、ターピニルメチルエーテル、ジヒドロターピニルメチルエーテル、ジグライム １，３−ジオキソランなどのエーテル系溶媒、アセトン、アセトフェノン、メチルエチルケトン、メチルプロピルケトン、ジエチルケトン、メチルｎ−ブチルケトン、メチルイソブチルケトン、ジプロピルケトン、ジイソブチルケトン、メチルアミルケトン、アセトニルアセトン、イソホロン、シクロヘキサノン、メチルシクロヘキサノン、２−（１−シクロヘキセニル）シクロヘキサノンメチルイソブチルケトン、シクロヘキサノン、イソホロンなどのケトン系溶媒、ギ酸エチル、ギ酸プロピル、ギ酸ブチル、ギ酸イソブチル、ギ酸ペンチル、酢酸メチル、酢酸エチル、酢酸ｎ−プロピル、酢酸イソプロピル、酢酸ｎ−ブチル、酢酸イソブチル、酢酸ｓｅｃ−ブチル、酢酸（イソ）アミル、酢酸シクロヘキシル、乳酸エチル、酢酸３−メトキシブチル、酢酸ｓｅｃ−ヘキシル、酢酸２−エチルブチル、酢酸２−エチルヘキシル、酢酸ベンジル、プロピオン酸メチル、プロピオン酸エチル、モノクロロ酢酸メチル、モノクロロ酢酸エチル、モノクロロ酢酸ブチル、アセト酢酸メチル、アセト酢酸エチル、プロピオン酸ブチル、プロピオン酸イソアミル、γ−ブチロラクトンなどのエステル系溶剤、エチレングリコールモノエチルエーテル、エチレングリコールモノイソプロピルエーテル、エチレングリコールモノブチルエーテル、ジエチレングリコールモノエチルエーテル、ジエチレングリコールモノｎ−ブチルエーテル、プロピレングリコールモノメチルエーテル、プロピレングリコールモノエチルエーテル、プロピレングリコールモノｎ−プロピルエーテル、プロピレングリコールモノｎ−ブチルエーテル、ジプロピレングリコールモノメチルエーテル、ジプロピレングリコールモノエチルエーテル、ジプロピレングリコールモノｎ−プロピルエーテル、ジプロピレングリコールモノｎ−ブチルエーテル、トリエチレングリコールモノメチルエーテル、トリエチレングリコールモノエチルエーテル、トリエチレングリコールモノｎ−プロピルエーテル、トリエチレングリコールモノｎ−ブチルエーテル、トリプロピレングリコールモノエチルエーテル、トリプロピレングリコールモノｎ−プロピルエーテル、トリプロピレングリコールモノｎ−ブチルエーテルなどのグリコールエーテル系溶剤、及び、それらモノエーテル類の酢酸エステル系溶剤、ジエチレングリコールジメチルエーテル、ジエチレングリコールジエチルエーテル、ジエチレングリコールメチルイソブチルエーテル、ジプロピレングリコールジメチルエーテル、ジプロピレングリコールジエチルエーテルなどのジアルキルエーテル系溶剤が挙げられる。メタノール、エタノール、ｎ−プロピルアルコール、イソプロピルアルコール、ｎ−ブチルアルコール、イソブチルアルコール、ｓｅｃ−ブチルアルコール、ｔ−ブチルアルコール、ヘプタノール、ｎ−アミルアルコール、ｓｅｃ−アミルアルコール、ｎ−ヘキシルアルコール、テトラヒドロフルフリルアルコール、フルフリルアルコール、アリルアルコール、エチレンクロロヒドリン、オクチルドデカノール、１−エチル−１−プロパノール、２−メチル−１−ブタノール、イソアミルアルコール、ｔ−アミルアルコール、ｓｅｃ−イソアミルアルコール、ネオアミルアルコール、ヘキシルアルコール、２−メチル−１−ペンタノール、４−メチル−２−ペンタノール、ヘプチルアルコール、ｎ−オクチルアルコール、２−エチルヘキシルアルコール、ノニルアルコール、デシルアルコール、ウンデシルアルコール、ラウリルアルコール、シクロペンタノール、シクロヘキサノール、ベンジルアルコール、α−テルピネオール、ターピネオールＣ、Ｌ−α−ターピネオール、ジヒドロターピネオール、ターピニルオキシエタノール、ジヒドロターピニルオキシエタノール、日本テルペン化学株式会社製のテルソルブＭＴＰＨ、テルソルブＤＴＯ−２１０、テルソルブＴＨＡ−９０、テルソルブＴＨＡ−７０や、シクロヘキサノール、３−メトキシブタノール、ジアセトンアルコール、１，４−ブタンジオール、オクタンジオール等や、日産化学工業株式会社製のファインオキソコール１４０Ｎ、ファインオキソコール１６００、ファインオキソコール１８０、ファインオキソコール１８０Ｎ、ファインオキソコール２０００などのアルコール系溶媒、エチレングリコール、ジエチレングリコール、トリエチレングリコール、プロピレングリコール、ジプロピレングリコール、１，３−ブチレングリコール、へキシレングリコール、ポリエチレングリコール、ポリプロピレングリコールなどのグリコール系溶剤が挙げられる。その他、ジメチルアセトアミド、ジメチルホルムアミドなどのアミド系溶媒などが挙げられる。また、分散媒として反応性基を有する（メタ）アクリル酸、（メタ）アクリル酸エステル類、酢酸ビニルなどのビニル系単量体、ビニルエーテル誘導体類、ポリアリル誘導体などのエチレン系不飽和単量体類も使用することができる。なお、前記分散媒は単独または２種以上を混合して適宜使用することができる。
8). Solvent The dispersion medium that can be used in the present invention includes toluene, xylene, aromatic hydrocarbon solvents, hydrocarbon solvents such as n-hexane, cyclohexane and n-heptane, and halogenated hydrocarbons such as methylene chloride, chloroform and dichloroethane. Solvents such as ethyl ether, isopropyl ether, dioxane, tetrahydrofuran, dibutyl ether, butyl ethyl ether, methyl-t-butyl ether, terpinyl methyl ether, dihydroterpinyl methyl ether, diglyme 1,3-dioxolane , Acetone, acetophenone, methyl ethyl ketone, methyl propyl ketone, diethyl ketone, methyl n-butyl ketone, methyl isobutyl ketone, dipropyl ketone, diisobutyl ketone, methyl amyl ketone, aceto Ketone solvents such as luacetone, isophorone, cyclohexanone, methylcyclohexanone, 2- (1-cyclohexenyl) cyclohexanone methyl isobutyl ketone, cyclohexanone, isophorone, ethyl formate, propyl formate, butyl formate, isobutyl formate, pentyl formate, methyl acetate, acetic acid Ethyl acetate, n-propyl acetate, isopropyl acetate, n-butyl acetate, isobutyl acetate, sec-butyl acetate, (iso) amyl acetate, cyclohexyl acetate, ethyl lactate, 3-methoxybutyl acetate, sec-hexyl acetate, 2-ethylbutyl acetate 2-ethylhexyl acetate, benzyl acetate, methyl propionate, ethyl propionate, methyl monochloroacetate, ethyl monochloroacetate, butyl monochloroacetate, methyl acetoacetate, ethyl acetoacetate, pro Ester solvents such as butyl pionate, isoamyl propionate, γ-butyrolactone, ethylene glycol monoethyl ether, ethylene glycol monoisopropyl ether, ethylene glycol monobutyl ether, diethylene glycol monoethyl ether, diethylene glycol mono n-butyl ether, propylene glycol monomethyl ether, Propylene glycol monoethyl ether, propylene glycol mono n-propyl ether, propylene glycol mono n-butyl ether, dipropylene glycol monomethyl ether, dipropylene glycol monoethyl ether, dipropylene glycol mono n-propyl ether, dipropylene glycol mono n-butyl ether , Triethylene glycol monomethyl ester Tellurium, triethylene glycol monoethyl ether, triethylene glycol mono n-propyl ether, triethylene glycol mono n-butyl ether, tripropylene glycol monoethyl ether, tripropylene glycol mono n-propyl ether, tripropylene glycol mono n-butyl ether, etc. And glycol ether solvents of these monoethers, and dialkyl ether solvents such as acetate solvents of diethers, diethylene glycol dimethyl ether, diethylene glycol diethyl ether, diethylene glycol methyl isobutyl ether, dipropylene glycol dimethyl ether, and dipropylene glycol diethyl ether. Methanol, ethanol, n-propyl alcohol, isopropyl alcohol, n-butyl alcohol, isobutyl alcohol, sec-butyl alcohol, t-butyl alcohol, heptanol, n-amyl alcohol, sec-amyl alcohol, n-hexyl alcohol, tetrahydrofurfuryl Alcohol, furfuryl alcohol, allyl alcohol, ethylene chlorohydrin, octyldodecanol, 1-ethyl-1-propanol, 2-methyl-1-butanol, isoamyl alcohol, t-amyl alcohol, sec-isoamyl alcohol, neoamyl alcohol Hexyl alcohol, 2-methyl-1-pentanol, 4-methyl-2-pentanol, heptyl alcohol, n-octyl alcohol, 2-ethylhexyl Lucol, nonyl alcohol, decyl alcohol, undecyl alcohol, lauryl alcohol, cyclopentanol, cyclohexanol, benzyl alcohol, α-terpineol, terpineol C, L-α-terpineol, dihydroterpineol, terpinyloxyethanol, dihydroterpi Nyloxyethanol, Tersolve MTPH, Tersolve DTO-210, Tersolve THA-90, Tersolve THA-70, cyclohexanol, 3-methoxybutanol, diacetone alcohol, 1,4-butanediol, octane manufactured by Nippon Terpene Chemical Co., Ltd. Diol, etc., Fine Oxocol 140N, Fine Oxocol 1600, Fine Oxocol 180, Fine Oxocol manufactured by Nissan Chemical Industries, Ltd. Alcohol solvents such as 80N, fine oxocol 2000, glycol solvents such as ethylene glycol, diethylene glycol, triethylene glycol, propylene glycol, dipropylene glycol, 1,3-butylene glycol, hexylene glycol, polyethylene glycol, and polypropylene glycol Can be mentioned. Other examples include amide solvents such as dimethylacetamide and dimethylformamide. In addition, (meth) acrylic acid having a reactive group as a dispersion medium, (meth) acrylic acid esters, vinyl monomers such as vinyl acetate, vinyl ether derivatives, and ethylenically unsaturated monomers such as polyallyl derivatives Can also be used. In addition, the said dispersion medium can be used suitably individually or in mixture of 2 or more types.
９．任意成分
本発明の金属酸化物半導体粒子分散体組成物は、酢酸セルロース、エチルセルロース、プロピルセルロース、ヒドロキシプロピルセルロース等の粘度調整剤を添加することができる。
9. Optional ingredients
Viscosity adjusting agents such as cellulose acetate, ethyl cellulose, propyl cellulose, and hydroxypropyl cellulose can be added to the metal oxide semiconductor particle dispersion composition of the present invention.
１０．使用方法
本発明の金属酸化物半導体粒子分散体組成物を基材上に塗布し、溶剤を蒸発させた後、塗工することにより、本発明の半導体からなる薄膜が形成される。塗工の対象となる基材としては、ステンレス箔、銅箔等の金属基板やガラス基板、シリコン基板その他PETフィルム、ポリイミド樹脂等のプラスチック基板などを挙げることができるが、これらに限定されない。塗工方法も、上記に限らず、通常用いられる装置、器具等を用いて行うことが出来る。
10. Method of Use The metal oxide semiconductor particle dispersion composition of the present invention is applied onto a substrate, the solvent is evaporated, and then the coating is applied to form a thin film made of the semiconductor of the present invention. Examples of the base material to be applied include, but are not limited to, a metal substrate such as stainless steel foil and copper foil, a glass substrate, a silicon substrate, a PET film, a plastic substrate such as polyimide resin, and the like. The coating method is not limited to the above, and can be performed using a commonly used apparatus, instrument, or the like.
以下に本発明の実施例および比較例について説明する。なお、以下において、配合量を示す「部」は「重量部」を示し、「％」は「重量％」を示す。言うまでもないが、本発明は下記実施例に限定されるものではなく、本発明の技術的範囲を逸脱しない範囲において適宜変更や修正が可能である。 Examples of the present invention and comparative examples will be described below. In the following, “part” indicating the blending amount indicates “part by weight” and “%” indicates “% by weight”. Needless to say, the present invention is not limited to the following examples, and appropriate changes and modifications can be made without departing from the technical scope of the present invention.
＜金属酸化物半導体粒子（ＩＧＺＯ）の調製＞
硝酸インジウム（アルドリッチ社製試薬）、硝酸亜鉛（アルドリッチ社製試薬）、硝酸ガリウム（アルドリッチ社製試薬）をモル比率で１：１：１となるよう水に溶解した後、アンモニア水により中和を行って水和物を得、これを水洗した。水洗した水和物を耐圧容器に封入し、１８０℃で３時間反応させることにより、金属酸化物半導体粒子（ＩＧＺＯ）を得た。この金属酸化物半導体粒子の比表面積を、日本ベル製ＢＥＬ−ＳＯＲＰｍｉｎｉにより測定し、一次粒子径を算出したところ、１７ｎｍであった。
<Preparation of metal oxide semiconductor particles (IGZO)>
Indium nitrate (Aldrich reagent), zinc nitrate (Aldrich reagent) and gallium nitrate (Aldrich reagent) are dissolved in water at a molar ratio of 1: 1: 1, and then neutralized with ammonia water. To obtain a hydrate which was washed with water. The water-washed hydrate was sealed in a pressure vessel and reacted at 180 ° C. for 3 hours to obtain metal oxide semiconductor particles (IGZO). It was 17 nm when the specific surface area of this metal oxide semiconductor particle was measured by Nippon Bell BEL-SORPmini, and the primary particle diameter was computed.
＜分散剤Ａの合成＞
［製造例１（分散剤Ａの合成）］
トルエン溶媒中に、分岐Ｃ１１〜１４アルキルアルコール（製品名：ＥＸＸＡＬ１３、エクソン・モービル社製）エチレンオキシド１０モル付加物６４０ｇ（１モル）およびモノクロロ酢酸ナトリウム１５２ｇ（１．３モル）を反応器にとり、均一になるよう撹拌した。その後、反応系の温度を６０℃の条件で水酸化ナトリウム５２ｇを添加した。次いで、反応系の温度を８０℃に昇温させ、３時間熟成させた。熟成後、反応系が５０℃の条件で９８％硫酸１１７ｇ（１．２モル）を滴下することにより、白色懸濁溶液を得た。次いで、この白色懸濁溶液を蒸留水で洗浄し、溶媒を減圧留去することにより、分散剤Ａ（Ｒ：分岐Ｃ１１〜１４アルキル、ＡＯ：エチレンオキシド、ｎ：１０、Ｘ：ＣＨ２）を得た。
［製造例２（分散剤Ｂの合成）］
製造例１において、分岐Ｃ１１〜１４アルキルアルコールエチレンオキシド１０モル付加物に代えて、イソデシルアルコールエチレンオキシド１０モル付加物５９８ｇ（１モル）とした以外は製造例１と同様の方法で行い、分散剤Ｂ（Ｒ：イソデシル、ＡＯ：エチレンオキシド、ｎ：１０、Ｘ：ＣＨ２）を得た。
［製造例３（分散剤Ｃの合成）］
製造例１において、分岐C11〜14アルキルアルコールエチレンオキシド１０モル付加物に代えて、分岐Ｃ１１〜１４アルキルアルコールエチレンオキシド５モル付加物４２０ｇ（１モル）とした以外は製造例１と同様の方法で行い、分散剤Ｃ（Ｒ：分岐Ｃ１１〜１４アルキル、ＡＯ：エチレンオキシド、ｎ：５、Ｘ：ＣＨ２）を得た。
<Synthesis of Dispersant A>
[Production Example 1 (Synthesis of Dispersant A)]
In a toluene solvent, 640 g (1 mol) of ethylene oxide 10 mol adduct and 152 g (1.3 mol) of sodium monochloroacetate, branched C11-14 alkyl alcohol (product name: EXXAL13, manufactured by Exxon Mobil Co.) are uniformly added It stirred until it became. Thereafter, 52 g of sodium hydroxide was added at a reaction system temperature of 60 ° C. Subsequently, the temperature of the reaction system was raised to 80 ° C. and aged for 3 hours. After aging, 117 g (1.2 mol) of 98% sulfuric acid was added dropwise with the reaction system at 50 ° C. to obtain a white suspension. Subsequently, this white suspension solution is washed with distilled water, and the solvent is distilled off under reduced pressure to obtain a dispersant A (R: branched C11-14 alkyl, AO: ethylene oxide, n: 10, X: CH 2 ). It was.
[Production Example 2 (Synthesis of Dispersant B)]
Dispersant B was produced in the same manner as in Production Example 1 except that 598 g (1 mol) of isodecyl alcohol ethylene oxide 10 mol adduct was used instead of the branched C11-14 alkyl alcohol ethylene oxide 10 mol adduct in Production Example 1. (R: isodecyl, AO: ethylene oxide, n: 10, X: CH 2 ) was obtained.
[Production Example 3 (Synthesis of Dispersant C)]
In Production Example 1, in place of the branched C11-14 alkyl alcohol ethylene oxide 10 mol adduct, 420 g (1 mol) of the branched C11-14 alkyl alcohol ethylene oxide 5 mol adduct was used. dispersant C (R: branched C11~14 alkyl, AO: ethylene oxide, n: 5, X: CH 2) was obtained.
＜分散体、塗工膜、半導体膜の調製＞
〔実施例１〕
上記で調製した金属酸化物半導体粒子にソルフィット（クラレ製、３−メトキシ−３−メチルブタノール）を金属酸化物半導体粒子の濃度が０．３Ｍとなるよう加え、さらに、上記で調製した分散剤Ａを金属酸化物半導体粒子に対して１０ｗｔ％添加し、ペイントシェーカーにて分散処理を行い、実施例としての金属酸化物半導体粒子分散体を得た。
<Preparation of dispersion, coating film, semiconductor film>
[Example 1]
Solfit (manufactured by Kuraray, 3-methoxy-3-methylbutanol) was added to the metal oxide semiconductor particles prepared above so that the concentration of the metal oxide semiconductor particles was 0.3 M, and the dispersant prepared above was further added. 10 wt% of A was added to the metal oxide semiconductor particles, and dispersion treatment was performed with a paint shaker to obtain a metal oxide semiconductor particle dispersion as an example.
次に、このスピンコーター等を用い、この分散体を塗布し、８０℃で３０分乾燥することにより塗工膜を得た。 Next, using this spin coater or the like, this dispersion was applied and dried at 80 ° C. for 30 minutes to obtain a coating film.
更に、この塗工膜を２５０℃で３０分間熱処理することにより、半導体膜を得た。 Furthermore, this coating film was heat-treated at 250 ° C. for 30 minutes to obtain a semiconductor film.
〔実施例２、３〕
分散剤Ａに代えて、分散剤Ｂおよび分散剤Ｃをそれぞれ用い、その他については実施例１と同様の手順・条件で、実施例２および３の金属酸化物半導体粒子分散体および半導体膜を得た。
[Examples 2 and 3]
In place of Dispersant A, Dispersant B and Dispersant C were used, respectively, and the other procedures and conditions similar to Example 1 were used to obtain the metal oxide semiconductor particle dispersions and semiconductor films of Examples 2 and 3. It was.
〔実施例４、５〕
分散剤Ａの添加量を金属酸化物半導体粒子に対して、それぞれ５ｗｔ％および１５ｗｔ％添加し、その他については実施例１と同様の手順・条件で、実施例４および実施例５の金属酸化物分散体および半導体膜を得た。
[Examples 4 and 5]
Dispersant A was added in an amount of 5 wt% and 15 wt%, respectively, with respect to the metal oxide semiconductor particles, and the other procedures and conditions were the same as in Example 1, and the metal oxides of Examples 4 and 5 were used. A dispersion and a semiconductor film were obtained.
〔比較例１、２〕
分散剤Ａに代えて、ステアリン酸および分岐Ｃ１１〜１４アルキルアルコール（製品名：ＥＸＸＡＬ１３、エクソン・モービル社製）エチレンオキシド１０モル付加物をそれぞれ用い、その他については実施例と同様の手順・条件で、比較例１および２の金属酸化物半導体粒子分散体および半導体膜を得た。
[Comparative Examples 1 and 2]
Instead of Dispersant A, stearic acid and branched C11-14 alkyl alcohol (product name: EXXAL13, manufactured by Exxon Mobil Co.) ethylene oxide 10 mol adduct were used, respectively, and the other procedures and conditions were the same as in the examples. Metal oxide semiconductor particle dispersions and semiconductor films of Comparative Examples 1 and 2 were obtained.
＜分散体（分散液）の評価＞
上記実施例および比較例の金属酸化物半導体粒子分散体を１日静置し、金属酸化物半導体粒子の沈降の有無について評価を行い、その結果を表１に示した。
<Evaluation of dispersion (dispersion)>
The metal oxide semiconductor particle dispersions of the above examples and comparative examples were allowed to stand for 1 day, and the presence or absence of sedimentation of the metal oxide semiconductor particles was evaluated. The results are shown in Table 1.
＜塗工膜の評価＞
実施例１および比較例１および２で作製した塗工膜についてＳＥＭ画像の撮影を倍率１００倍および３０００倍で行い、その結果を図１〜６に示した。また、これらの塗工膜についてヘイズの測定をスガ試験機株式会社製ヘイズコンピューターにより行った。
<Evaluation of coating film>
SEM images of the coating films produced in Example 1 and Comparative Examples 1 and 2 were taken at magnifications of 100 and 3000, and the results are shown in FIGS. Moreover, the haze of these coating films was measured with a haze computer manufactured by Suga Test Instruments Co., Ltd.
＜半導体膜＞
実施例および比較例で作製した半導体膜について、体積抵抗を３回測定し、その平均値を表１に示した。体積抵抗の測定は、（ＡＤＶＡＮＴＥＣ製デジタル超高抵抗計Ｒ８３４０）により行った。
<Semiconductor film>
About the semiconductor film produced by the Example and the comparative example, volume resistance was measured 3 times and the average value was shown in Table 1. The volume resistance was measured by (ADVANTEC digital super high resistance meter R8340).
＜結果＞
表１から明らかなように、各実施例の分散体は、比較例の分散体に比較して、分散安定性に優れていることが分かる。また、実施例１の分散体から得られる塗工膜のＳＥＭ画像は、比較例１および２の分散体から得られる塗工膜に比較して、均一でムラが無く、ヘイズの値も良好な値を示している。従って、実施例の分散体から得られる塗工膜の方が、金属酸化物半導体としての特性が損なわれないことが予想される。更に、実施例の分散体から得られる半導体膜の体積抵抗値は、比較例の分散体から得られる半導体膜の体積抵抗値に比較して小さく、このことからも、各実施例の分散体から得られる半導体膜では、金属酸化物半導体としての特性が損なわれないことが予想される。
<Result>
As is clear from Table 1, it can be seen that the dispersion of each example is superior in dispersion stability compared to the dispersion of the comparative example. Further, the SEM image of the coating film obtained from the dispersion of Example 1 is uniform and non-uniform and has a good haze value as compared with the coating film obtained from the dispersions of Comparative Examples 1 and 2. The value is shown. Therefore, it is expected that the coating film obtained from the dispersion of the example does not impair the characteristics as a metal oxide semiconductor. Furthermore, the volume resistance value of the semiconductor film obtained from the dispersion of the example is smaller than the volume resistance value of the semiconductor film obtained from the dispersion of the comparative example, and also from this, from the dispersion of each example In the obtained semiconductor film, it is expected that characteristics as a metal oxide semiconductor are not impaired.
本発明の金属酸化物半導体粒子分散体組成物から得られる塗工膜および半導体膜は、電子回路、電子部品等の分野で利用可能である。 The coating film and semiconductor film obtained from the metal oxide semiconductor particle dispersion composition of the present invention can be used in the fields of electronic circuits, electronic components and the like.
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| CN108987597A (en) * | 2018-07-17 | 2018-12-11 | 嘉兴纳鼎光电科技有限公司 | The composition of ambient stable storage and the preparation method of light emitting diode with quantum dots device |
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