CN1400107A - Ink jet printing method for preparing metal oxide functional film - Google Patents

Ink jet printing method for preparing metal oxide functional film Download PDF

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Publication number
CN1400107A
CN1400107A CN 01128005 CN01128005A CN1400107A CN 1400107 A CN1400107 A CN 1400107A CN 01128005 CN01128005 CN 01128005 CN 01128005 A CN01128005 A CN 01128005A CN 1400107 A CN1400107 A CN 1400107A
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metal
ink
organic solvent
prepare
water
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CN 01128005
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CN1199795C (en
Inventor
赵岩
郝传勇
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Institute of Metal Research of CAS
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Institute of Metal Research of CAS
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Abstract

The method for preparing metal oxide function film by using ink-jet printing process includes the following steps: 1). using soluble metal compound as raw material, dissolving it in water or organic solvent, the weight ratio of raw material and water or organic solvent is 1-30:100-200; or dispersing nano granules of metal oxide in water or organic solvent according to same weight ratio; 2) adding additive, added quantity is 0.01-5% of weight of water or organic solvent, the controlled ink viscosity is 20-60 mPa.s and its surface tension is 20-40 mNm(-1), and preparing metal oxide ink with stable property; 3). injecting said ink into ink box and adopting conventional ink-jet printing process to make the ink deposit on the substrate; and 4). heating film layer deposited on the substrate at 200-700 deg.C to form the metal oxide functional film.

Description

Inkjet printing prepares the method for metal oxide functional film
Technical field
The present invention relates to the metal-oxide film technology, specifically a kind of inkjet printing prepares the method for metal oxide functional film.
Background technology
Metal oxide has many special physicochemical performances, and the metal-oxide film material that preparation has a fixed structure, composition and pattern is the basis of many modern functions devices.Preparation has the functional material film of specific pattern and mainly takes technology such as lithographic printing and thick film screen printing at present.Lithographic printing at first adopts thin film preparation processes such as vacuum coating to prepare film, adopts the method for photoetching and chemical attack to prepare specific pattern then.The thick film screen printing technology at first prepares template and material paste, is printed onto then on the substrate, obtains rete through oversintering again.These technology all need to prepare template, apparatus expensive, and the preparation cost height, the cycle is long.
Inkjet technology is one of major technique that generally adopts in the modern handle official bussiness printing, is divided into continous way and random mode two classes according to ink-jetting style.The continous inkjet technology utilizes Piexoelectric actuator that the shower nozzle ink inside is applied fixation pressure, makes its continuous injection, utilizes the heading of deflecting electrode change ink droplet and forms pattern.The only ink-jet when needed of random mode ink-jet technology, it mainly contains two kinds of bubble type and piezoelectric types.Bubble type is provided with heater on the tube wall of shower nozzle, under the electric pulse effect, form very little bubble on the heater, and the bubble expanded by heating produces pressure-driven ink droplet jetting nozzle.Piezoelectric type utilizes the minute-pressure electric device to make transducer, produces pressure wave and drive the ink droplet jetting nozzle under the pulse voltage effect.The a plurality of ink-jet systems of configuration in the general printer, each ink-jet system connects with the print cartridge that the different colours ink is housed, and can print colourful pattern.In recent years, the researcher begins to attempt it is used for the preparation of plane function material, and obtain some preliminary results, as prepare conducting polymer film (D.Pede, G.erra, and De Rossi, Mater.Sci.Eng.C.5 (1998) 289), preparation color organic light emitting diode (Adv.Mater.11 (1999) 734 for S.-C.Chang, et al), prepare function nano structure graph (H.Y.Fan by the self organizing function ink that has that contains surfactant, et al, Nature, 405 (2000) 56).Inkjet technology is as the functional material preparation means of plane function material particularly, because it has and is easy to prepare complex figure, but and the characteristics of pointwise control composition, be expected under a stable condition, to be used to replace the technologies such as plated film, offset printing of existing complexity.Utilize inkjet technology to prepare metal oxide functional film and yet there are no report.
Summary of the invention
It is low to the purpose of this invention is to provide a kind of preparation cost, and the cycle is short, does not need template, and the inkjet printing that directly prepares figure prepares the method for metal oxide functional film.
To achieve these goals, technical scheme of the present invention is: operation as follows: be raw material with the soluble metal compound 1), it is dissolved in water or the organic solvent that the weight ratio of described raw material and water or organic solvent is 1-30: 100-200; 2) add additive, addition is the 0.01-5% of water or organic solvent weight, is that 20-60mPas, surface tension are 20-40mNm with the viscosity of controlling ink -1, be made into the metal oxide ink of stable performance; 3) described ink is injected in the print cartridge, adopts conventional inkjet technology to deposit on the substrate; 4) deposit to on-chip rete through 200-700 ℃ heat treatment with described, reaction forms the metal oxide functional film with special pattern;
In addition, raw material described in the step 1) of the present invention is a metal oxide nanoparticles, and it is dispersed in water or the organic solvent;
Water of the present invention can be deionized water; Described organic solvent can be absolute ethyl alcohol; Described additive adopts surfactant or high molecular polymer; Described surfactant is anion surfactant, cationic surfactant or nonionic surface active agent; Described anion surfactant is odium stearate, lauryl sodium sulfate or neopelex etc.; Described cationic surfactant is a softex kw etc.; Described nonionic surface active agent is dodecyl diethanol amine, polyvinyl alcohol etc.
The principle of the invention is: the raw material that employing can add thermal response generation metal oxide is dissolved in deionized water or the organic solvent, or adopt the nanoparticulate dispersed of metal oxide in deionized water or organic solvent, to make ink-jet ink, regulate various performances such as the stability of ink, surface tension, viscosity by adding surfactant or high molecular polymer and other reagent, with conventional ink-jet printer ink is coated on the substrate, obtains having the metal-oxide film of certain figure through the heat treatment of uniform temperature.
The present invention has following advantage:
Adopt the present invention can prepare multiple metal-oxide film material, as Fe 2O 3, SnO 2, TiO 2, SiO 2, ZnO, NiO, BaTiO 3, monobasic and polynary, multiple layer metal oxide material such as PZT; The figure and the composition of the control of pointwise simply and easily rete, the figure of output has the precision height, sharpness of border, characteristics such as be evenly distributed realize having according to given composition and graphics request preparation the monobasic or the polynary metal oxide film material with function of specific (special) requirements; Applied range in addition, the present invention is particularly suitable for preparing the responsive rete of the function element of composition and figure complexity.
The specific embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1
The preparation sull:
Operation as follows: 1) get 10g metallic compound FeCl 3Be raw material, it is dissolved in the 200ml deionized water, place reactor hydrolysis at a certain temperature to form the ferric oxide nanometer particle precipitation; The present embodiment temperature of reactor is 80 ℃, and the weight ratio of described raw material and deionized water is 10: 200; 2) add deionized water 100ml with the centrifuge eccentric cleaning for several times, add polyethylene of dispersing agent alcohol 1g under brute force stirs, addition is 1% of a deionized water weight, is 30mNm with the viscosity of controlling ink less than 50mPas (room temperature), surface tension -1Be made into the iron oxide ink-jet ink; 3) described ink is injected in the print cartridge, adopts conventional inkjet technology to deposit on the alumina ceramic substrate; 4) deposit to on-chip film through 400 ℃ heat treatment with described, form sull; Described raw material can also be Fe (NO) 3
Embodiment 2
The preparation SnO 2 thin film:
Operation as follows: 1) get 10g metallic compound SnCl 2Be raw material, it be dissolved in the 100ml organic solvent absolute ethyl alcohol, insert in the return channel that the present embodiment reflux temperature is that 80 ℃, return time are 36 hours; In reflux course, can see producing a large amount of smog, be HCl; Adding absolute ethyl alcohol in the tin alcoholates that reaction forms, to make volume be 100ml; The weight ratio of described raw material and organic solvent is 10: 100; 2) add surfactant softex kw 0.5g, addition is 0.5% of an organic solvent weight, is that 40mPas (room temperature), surface tension are 40mNm with the viscosity of controlling ink -1, be made into burning tin ink-jet ink; 3) described ink is injected in the print cartridge, adopts conventional inkjet technology to deposit on the alumina ceramic substrate; 4) deposit to on-chip film through 600 ℃ heat treatment with described, reaction forms SnO 2 thin film.
Embodiment 3
The preparation zinc-oxide film:
Operation as follows: 1) getting 15g metallic compound zinc acetate is raw material, and it is dissolved in the 100ml deionized water, and the weight ratio of described raw material and water is 15: 100; 2) add the dispersant lauryl sodium sulfate O.3g, addition is 0.3% of a water weight, is that 30mPas (room temperature), surface tension are 30mNm with the viscosity of controlling ink -1, be made into the zinc oxide ink; 3) described ink is injected in the print cartridge, adopts conventional inkjet technology spray deposited to alumina ceramic substrate by predetermined pattern; 4) deposit to on-chip rete through 550 ℃ heat treatment with described, reaction forms zinc-oxide film.
The present invention also can adopt anion surfactant such as odium stearate, neopelex, and nonionic surface active agent such as dodecyl diethanol amine etc. is made dispersant or high molecular polymer.
Adopt the present invention can prepare multiple metal-oxide film or multiple layer metal sull.

Claims (9)

1. an inkjet printing prepares the method for metal oxide functional film, it is characterized in that operating as follows: be raw material 1) with the soluble metal compound, it is dissolved in water or the organic solvent, and the weight ratio of described raw material and water or organic solvent is 1-30: 100-200; 2) add additive, addition is the 0.01-5% of water or organic solvent weight, is that 20-60mPas, surface tension are 20-40mNm with the viscosity of controlling ink -1, be made into the metal oxide ink of stable performance; 3) described ink is injected in the print cartridge, adopts conventional inkjet technology to deposit on the substrate; 4) deposit to on-chip rete through 200-700 ℃ heat treatment with described, reaction forms the metal oxide functional film with special pattern.
2. prepare the method for metal-oxide film according to the described inkjet printing of claim 1, it is characterized in that: raw material described in the step 1) is a metal oxide nanoparticles, and it is dispersed in water or the organic solvent.
3. prepare the method for metal-oxide film according to claim 1 or 2 described inkjet printings, it is characterized in that: described water can be deionized water.
4. prepare the method for metal-oxide film according to claim 1 or 2 described inkjet printings, it is characterized in that: described organic solvent is an absolute ethyl alcohol.
5. prepare the method for metal-oxide film according to claim 1 or 2 described inkjet printings, it is characterized in that: described additive adopts surfactant or high molecular polymer.
6. prepare the method for metal-oxide film according to the described inkjet printing of claim 5, it is characterized in that: described surfactant is anion surfactant, cationic surfactant or nonionic surface active agent.
7. prepare the method for metal-oxide film according to the described inkjet printing of claim 6, it is characterized in that: described anion surfactant is odium stearate, lauryl sodium sulfate or neopelex.
8. prepare the method for metal-oxide film according to the described inkjet printing of claim 6, it is characterized in that: described cationic surfactant is a softex kw.
9. prepare the method for metal-oxide film according to the described inkjet printing of claim 6, it is characterized in that: described nonionic surface active agent is dodecyl diethanol amine, polyvinyl alcohol.
CN 01128005 2001-08-03 2001-08-03 Ink jet printing method for preparing metal oxide functional film Expired - Fee Related CN1199795C (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101161377B (en) * 2006-10-11 2010-06-02 三星电机株式会社 Methods for surface modification of non-dispersible metal nanoparticles and modified metal nanoparticles for inkjet by the same method
CN102002275A (en) * 2010-12-13 2011-04-06 尚越光电科技有限公司 Preparation method of zinc oxide ink
CN102775847A (en) * 2012-07-16 2012-11-14 中国科学院宁波材料技术与工程研究所 Ink used for preparing zinc oxide-based film and preparation method thereof
WO2013097729A1 (en) * 2011-12-27 2013-07-04 Shenzhen Byd Auto R&D Company Limited Ink composition, method of metalizing surface and article obtainable
CN104099586A (en) * 2013-04-15 2014-10-15 中国科学院理化技术研究所 Preparation method for film
EP2798097A4 (en) * 2011-12-27 2015-11-18 Shenzhen Byd Auto R & D Co Ltd Method of metalizing surface and article obtainable
CN107903712A (en) * 2017-11-17 2018-04-13 福州大学 Metal oxide semiconductor ink and application method in a kind of inkjet printing technology
CN108145165A (en) * 2017-12-13 2018-06-12 天齐锂业股份有限公司 The method that 3D printing prepares metal lithium bands
CN110423516A (en) * 2018-09-04 2019-11-08 广东聚华印刷显示技术有限公司 Ink and preparation method thereof and gas sensor film
CN111239203A (en) * 2018-11-29 2020-06-05 中国科学院大连化学物理研究所 Preparation method of copper oxide film

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101161377B (en) * 2006-10-11 2010-06-02 三星电机株式会社 Methods for surface modification of non-dispersible metal nanoparticles and modified metal nanoparticles for inkjet by the same method
CN102002275A (en) * 2010-12-13 2011-04-06 尚越光电科技有限公司 Preparation method of zinc oxide ink
CN102002275B (en) * 2010-12-13 2012-12-05 尚越光电科技有限公司 Preparation method of zinc oxide ink
WO2013097729A1 (en) * 2011-12-27 2013-07-04 Shenzhen Byd Auto R&D Company Limited Ink composition, method of metalizing surface and article obtainable
US9758682B2 (en) 2011-12-27 2017-09-12 Shenzhen Byd Auto R&D Company Limited Ink composition, method of metalizing surface and article obtainable
EP2798097A4 (en) * 2011-12-27 2015-11-18 Shenzhen Byd Auto R & D Co Ltd Method of metalizing surface and article obtainable
CN102775847A (en) * 2012-07-16 2012-11-14 中国科学院宁波材料技术与工程研究所 Ink used for preparing zinc oxide-based film and preparation method thereof
CN102775847B (en) * 2012-07-16 2014-10-08 中国科学院宁波材料技术与工程研究所 Ink used for preparing zinc oxide-based film and preparation method thereof
CN104099586B (en) * 2013-04-15 2017-04-19 中国科学院理化技术研究所 Preparation method for film
CN104099586A (en) * 2013-04-15 2014-10-15 中国科学院理化技术研究所 Preparation method for film
CN107903712A (en) * 2017-11-17 2018-04-13 福州大学 Metal oxide semiconductor ink and application method in a kind of inkjet printing technology
CN108145165A (en) * 2017-12-13 2018-06-12 天齐锂业股份有限公司 The method that 3D printing prepares metal lithium bands
CN108145165B (en) * 2017-12-13 2019-11-08 天齐锂业股份有限公司 The method that 3D printing prepares metal lithium bands
CN110423516A (en) * 2018-09-04 2019-11-08 广东聚华印刷显示技术有限公司 Ink and preparation method thereof and gas sensor film
CN110423516B (en) * 2018-09-04 2022-04-19 广东聚华印刷显示技术有限公司 Ink, preparation method thereof and gas sensor film
CN111239203A (en) * 2018-11-29 2020-06-05 中国科学院大连化学物理研究所 Preparation method of copper oxide film

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