CN108231277A - A kind of method for reducing MOD type silver ink water film defects by adjusting ink droplet spacing - Google Patents

A kind of method for reducing MOD type silver ink water film defects by adjusting ink droplet spacing Download PDF

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Publication number
CN108231277A
CN108231277A CN201711323607.3A CN201711323607A CN108231277A CN 108231277 A CN108231277 A CN 108231277A CN 201711323607 A CN201711323607 A CN 201711323607A CN 108231277 A CN108231277 A CN 108231277A
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China
Prior art keywords
type silver
ink droplet
droplet spacing
water film
mod type
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CN201711323607.3A
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Chinese (zh)
Inventor
宁洪龙
周艺聪
姚日晖
陶瑞强
陈建秋
杨财桂
蔡炜
朱镇南
魏靖林
彭俊彪
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South China University of Technology SCUT
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South China University of Technology SCUT
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Priority to CN201711323607.3A priority Critical patent/CN108231277A/en
Publication of CN108231277A publication Critical patent/CN108231277A/en
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
    • H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Manufacturing Of Printed Wiring (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)

Abstract

The invention belongs to optoelectronic materials technologies, disclose a kind of method for reducing MOD type silver ink water film defects by adjusting ink droplet spacing.Substrate is cleaned by ultrasonic and dried, then by 35~45 μm of ink droplet spacing ranges of the method choice of inkjet printing by MOD type silver ink waters print preset figure in substrate, then formation liquid Ag films cure in thermal station, obtain silver-colored conductive film.The present invention by adjust ink droplet spacing reduce MOD type silver inks it is hydrothermal hardening after surface filming defect, to obtain the Ag films of surface uniform ground, can be applied to prepare metal conducting electrodes.

Description

A kind of method for reducing MOD type silver ink water film defects by adjusting ink droplet spacing
Technical field
The invention belongs to optoelectronic materials technologies, and in particular to a kind of to reduce MOD type silver inks by adjusting ink droplet spacing The method of water film defects.
Background technology
Metal-organic decomposition type silver ink water (Metal-Organic decomposition silver ink, abbreviation MOD Silver ink), it is a kind of silver ink water for being widely used in preparing conductive film, mainly passes through the decomposition of silver compound Reaction generates silver nano-grain, so as to form conductive Ag films.
Since MOD types silver ink water is mainly made of silver compound and organic solvent, decomposition reaction need longer time and Higher temperature can be just fully finished.And a large amount of bubbles caused by the violent volatilization of organic solvent are discharged from bottom during heat cure During surface, the part easily led in liquid film certain time is uneven or thinned, simultaneously because solvent is quick Removal, it is difficult to these defects are eliminated using the flowing of solution, so as to which film regional area be made slight crack or hole occur.
And such issues that solve common method is to change the ingredient or proportioning of silver-colored solution, improves the boiling point of solvent, is reduced The evaporation rate of solvent or viscosity, the surface tension for adjusting solution improve liquid fluidity etc..And the implementation of these methods Process is relatively complicated, and theoretical and principle is sufficiently complex, increases technique required time and cost.
Invention content
In place of above shortcoming and defect of the existing technology, the purpose of the present invention is to provide one kind to pass through adjusting The method that ink droplet spacing reduces MOD type silver ink water film defects.
The object of the invention is achieved through the following technical solutions：
A kind of method for reducing MOD type silver ink water film defects by adjusting ink droplet spacing, includes the following steps：
(1) substrate is cleaned by ultrasonic and dried；
(2) pass through 35~45 μm of ink droplet spacing ranges of method choice of inkjet printing (inkjet printing) at room temperature By MOD type silver ink waters print preset figure in substrate, liquid Ag films are formed；
(3) the liquid Ag films of step (2) in thermal station are cured, obtains silver-colored conductive film.
Preferably, the substrate described in step (1) is the sheet glass of length and width 1cm × 1cm, thickness 0.7mm.
Preferably, cleaning described in step (1) refers to successively using isopropanol, tetrahydrofuran, alkaline cleaning fluid, deionization Water and isopropanol are cleaned by ultrasonic.
Preferably, drying temperature described in step (1) is 80~85 DEG C.
Preferably, MOD type silver ink waters solid content described in step (2) are 15%, and viscosity is 9~15cps, and surface tension is 30~32dynes/cm, the solvent used are 130~150 DEG C with reference to sintering temperature for ethyl alcohol, and corresponding resistivity is 4.2 μ Ω·cm。
Preferably, the parameter of inkjet printing described in step (2) is：1000 μm of nozzle and substrate spacing, base reservoir temperature 50 ~55 DEG C, 50~55 DEG C of nozzle temperature.
Preferably, cured temperature described in step (3) is 160~165 DEG C.
Preferably, the cured time described in step (3) is 1min.
The principle of the present invention is：Select best ink droplet spacing range and by silver ink water inkjet printing to glass substrate, The thickness for controlling liquid film is smaller, reaction is enable quickly to carry out, bubble can be discharged rapidly, so as to give liquid film one The part that the fixed time carries out flowing reparation liquid film is uneven or thinned, the higher solidification temperature of use and shorter curing Curing makes Ag films shape rapidly in time.
The method of the present invention has the following advantages that and advantageous effect：
(1) it does not need to change formula again and adjusts silver inks aqueous nature, it is simple and practicable, reduce time and materials cost.
(2) the silver-colored conductive film surface uniform ground obtained by this method, no significant defect.
(3) application of the MOD types silver ink water in metal conducting electrodes preparation is realized.
Description of the drawings
Fig. 1 is the patterned Ag films that embodiment 1 obtains.
Fig. 2 is the patterned Ag films that embodiment 2 obtains.
Fig. 3 is the patterned Ag films that embodiment 3 obtains.
Fig. 4 is the patterned Ag films that embodiment 4 obtains.
Fig. 5 is the patterned Ag films that embodiment 5 obtains.
Fig. 6 is the patterned Ag films that embodiment 6 obtains.
Fig. 7 is the patterned Ag films that embodiment 7 obtains.
Specific embodiment
With reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited In this.
Embodiment 1
(1) the glass chip bottom of length and width 1cm × 1cm, thickness about 0.7mm are cleaned successively through isopropanol, tetrahydrofuran, alkalinity Liquid, deionized water first pass, deionized water second time, isopropanol cleaning, often walk and all shake 5~10min with ultrasonic cleaner. Then the substrate cleaned is put into baking oven, is dried at 80~85 DEG C.
(2) with printer (Dimatix DMP-2800 printers) using TEC-IJ-010MOD solution-types silver ink water (from Korea Spro InkTec companies of state buy；Solid content is 15%, and viscosity is 9~15cps, and surface tension is 30~32dynes/cm, use Solvent is ethyl alcohol, and it is 130 DEG C~150 DEG C to recommend sintering temperature, and reference resistance rate is 4.2 μ Ω cm), it cleans and dries in step (1) Print preset figure in substrate after dry, wherein print parameters are set as：1000 μm of nozzle and substrate spacing, ink droplet spacing 15 μm, 50~55 DEG C of base reservoir temperature, 50~55 DEG C of nozzle temperature.
(3) substrate after step (2) inkjet printing preset pattern is placed in thermal station with 160~165 DEG C of curing 1min, obtained To Ag films.
Patterned Ag films that the present embodiment obtains are as shown in Figure 1, it is found that when 15 μm of ink droplet spacing, after curing There is a large amount of fine cracks and a small amount of larger crackle in Ag films, it is seen that when ink droplet spacing is nearer, liquid film thickness compared with Greatly, decomposition reaction is slower, and bubble is also discharged relatively slowly, leads to a large amount of crackles occur.
Embodiment 2
(1) the glass chip bottom of length and width 1cm × 1cm, thickness about 0.7mm are cleaned successively through isopropanol, tetrahydrofuran, alkalinity Liquid, deionized water first pass, deionized water second time, isopropanol cleaning, often walk and all shake 5~10min with ultrasonic cleaner. Then the substrate cleaned is put into baking oven, is dried at 80~85 DEG C.
(2) with printer (Dimatix DMP-2800 printers) using TEC-IJ-010MOD solution-types silver ink water (from Korea Spro InkTec companies of state buy；Solid content is 15%, and viscosity is 9~15cps, and surface tension is 30~32dynes/cm, use Solvent is ethyl alcohol, and it is 130 DEG C~150 DEG C to recommend sintering temperature, and reference resistance rate is 4.2 μ Ω cm), it cleans and dries in step (1) Print preset figure in substrate after dry, wherein print parameters are set as：1000 μm of nozzle and substrate spacing, ink droplet spacing 20 μm, 50~55 DEG C of base reservoir temperature, 50~55 DEG C of nozzle temperature.
(3) substrate after step (2) inkjet printing preset pattern is placed in thermal station with 160~165 DEG C of curing 1min, obtained To Ag films.
Patterned Ag films that the present embodiment obtains are tiny to split as shown in Fig. 2, it is found that when ink droplet spacing gradually increases Line quantity significantly reduces, but still has a small amount of larger crackle, and coffee toroidal effect is apparent.
Embodiment 3
(1) the glass chip bottom of length and width 1cm × 1cm, thickness about 0.7mm are cleaned successively through isopropanol, tetrahydrofuran, alkalinity Liquid, deionized water first pass, deionized water second time, isopropanol cleaning, often walk and all shake 5~10min with ultrasonic cleaner. Then the substrate cleaned is put into baking oven, is dried at 80~85 DEG C.
(2) with printer (Dimatix DMP-2800 printers) using TEC-IJ-010MOD solution-types silver ink water (from Korea Spro InkTec companies of state buy；Solid content is 15%, and viscosity is 9~15cps, and surface tension is 30~32dynes/cm, use Solvent is ethyl alcohol, and it is 130 DEG C~150 DEG C to recommend sintering temperature, and reference resistance rate is 4.2 μ Ω cm), it cleans and dries in step (1) Print preset figure in substrate after dry, wherein print parameters are set as：1000 μm of nozzle and substrate spacing, ink droplet spacing 25 μm, 50~55 DEG C of base reservoir temperature, 50~55 DEG C of nozzle temperature.
(3) substrate after step (2) inkjet printing preset pattern is placed in thermal station with 160~165 DEG C of curing 1min, obtained To Ag films.
Patterned Ag films that the present embodiment obtains are tiny to split as shown in figure 3, it is found that when ink droplet spacing gradually increases Line quantity significantly reduces, but still has a small amount of larger crackle, and coffee toroidal effect is apparent.
Embodiment 4
(1) the glass chip bottom of length and width 1cm × 1cm, thickness about 0.7mm are cleaned successively through isopropanol, tetrahydrofuran, alkalinity Liquid, deionized water first pass, deionized water second time, isopropanol cleaning, often walk and all shake 5~10min with ultrasonic cleaner. Then the substrate cleaned is put into baking oven, is dried at 80~85 DEG C.
(2) with printer (Dimatix DMP-2800 printers) using TEC-IJ-010MOD solution-types silver ink water (from Korea Spro InkTec companies of state buy；Solid content is 15%, and viscosity is 9~15cps, and surface tension is 30~32dynes/cm, use Solvent is ethyl alcohol, and it is 130 DEG C~150 DEG C to recommend sintering temperature, and reference resistance rate is 4.2 μ Ω cm), it cleans and dries in step (1) Print preset figure in substrate after dry, wherein print parameters are set as：1000 μm of nozzle and substrate spacing, ink droplet spacing 30 μm, 50~55 DEG C of base reservoir temperature, 50~55 DEG C of nozzle temperature.
(3) substrate after step (2) inkjet printing preset pattern is placed in thermal station with 160~165 DEG C of curing 1min, obtained To Ag films.
The patterned Ag films that the present embodiment obtains are split as shown in figure 4, it is found that when ink droplet spacing increases to 30 μm Line disappears, but coffee toroidal effect is still apparent.
Embodiment 5
(1) the glass chip bottom of length and width 1cm × 1cm, thickness about 0.7mm are cleaned successively through isopropanol, tetrahydrofuran, alkalinity Liquid, deionized water first pass, deionized water second time, isopropanol cleaning, often walk and all shake 5~10min with ultrasonic cleaner. Then the substrate cleaned is put into baking oven, is dried at 80~85 DEG C.
(2) with printer (Dimatix DMP-2800 printers) using TEC-IJ-010MOD solution-types silver ink water (from Korea Spro InkTec companies of state buy；Solid content is 15%, and viscosity is 9~15cps, and surface tension is 30~32dynes/cm, use Solvent is ethyl alcohol, and it is 130 DEG C~150 DEG C to recommend sintering temperature, and reference resistance rate is 4.2 μ Ω cm), it cleans and dries in step (1) Print preset figure in substrate after dry, wherein print parameters are set as：1000 μm of nozzle and substrate spacing, ink droplet spacing 35 μm, 50~55 DEG C of base reservoir temperature, 50~55 DEG C of nozzle temperature.
(3) substrate after step (2) inkjet printing preset pattern is placed in thermal station with 160~165 DEG C of curing 1min, obtained To Ag films.
For the patterned Ag films that the present embodiment obtains as shown in figure 5, it is found that when ink droplet spacing is 35 μm, nothing is apparent Coffee toroidal effect, without apparent crackle and hole, Ag films surface is uniform.
Embodiment 6
(1) the glass chip bottom of length and width 1cm × 1cm, thickness about 0.7mm are cleaned successively through isopropanol, tetrahydrofuran, alkalinity Liquid, deionized water first pass, deionized water second time, isopropanol cleaning, often walk and all shake 5~10min with ultrasonic cleaner. Then the substrate cleaned is put into baking oven, is dried at 80~85 DEG C.
(2) with printer (Dimatix DMP-2800 printers) using TEC-IJ-010MOD solution-types silver ink water (from Korea Spro InkTec companies of state buy；Solid content is 15%, and viscosity is 9~15cps, and surface tension is 30~32dynes/cm, use Solvent is ethyl alcohol, and it is 130 DEG C~150 DEG C to recommend sintering temperature, and reference resistance rate is 4.2 μ Ω cm), it cleans and dries in step (1) Print preset figure in substrate after dry, wherein print parameters are set as：1000 μm of nozzle and substrate spacing, ink droplet spacing 45 μm, 50~55 DEG C of base reservoir temperature, 50~55 DEG C of nozzle temperature.
(3) substrate after step (2) inkjet printing preset pattern is placed in thermal station with 160~165 DEG C of curing 1min, obtained To Ag films.
For the patterned Ag films that the present embodiment obtains as shown in fig. 6, it is found that when ink droplet spacing is 45 μm, nothing is apparent Coffee toroidal effect, without apparent crackle and hole, Ag films surface is uniform.
Embodiment 7
(1) the glass chip bottom of length and width 1cm × 1cm, thickness about 0.7mm are cleaned successively through isopropanol, tetrahydrofuran, alkalinity Liquid, deionized water first pass, deionized water second time, isopropanol cleaning, often walk and all shake 5~10min with ultrasonic cleaner. Then the substrate cleaned is put into baking oven, is dried at 80~85 DEG C.
(2) with printer (Dimatix DMP-2800 printers) using TEC-IJ-010MOD solution-types silver ink water (from Korea Spro InkTec companies of state buy；Solid content is 15%, and viscosity is 9~15cps, and surface tension is 30~32dynes/cm, use Solvent is ethyl alcohol, and it is 130 DEG C~150 DEG C to recommend sintering temperature, and reference resistance rate is 4.2 μ Ω cm), it cleans and dries in step (1) Print preset figure in substrate after dry, wherein print parameters are set as：1000 μm of nozzle and substrate spacing, ink droplet spacing 50 μm, 50~55 DEG C of base reservoir temperature, 50~55 DEG C of nozzle temperature.
(3) substrate after step (2) inkjet printing preset pattern is placed in thermal station with 160~165 DEG C of curing 1min, obtained To Ag films.
Patterned Ag films that the present embodiment obtains as shown in fig. 7, it is found that when ink droplet spacing continues to increase to 50 μm, Due between ink droplet too far, it is difficult to form continuous film.
In conclusion 35 μm~45 μm are comparatively ideal ink droplet spacing range, the MOD type silver inks of inkjet printing in the range of this Hydrothermal hardening rear surface film forming defect significantly reduces, and has ideal surface.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification, Equivalent substitute mode is should be, is included within protection scope of the present invention.

Claims (8)

  1. A kind of 1. method for reducing MOD type silver ink water film defects by adjusting ink droplet spacing, it is characterised in that including following step Suddenly：
    (1) substrate is cleaned by ultrasonic and dried；
    (2) at room temperature by 35~45 μm of ink droplet spacing ranges of the method choice of inkjet printing by MOD type silver ink waters in substrate Print preset figure forms liquid Ag films；
    (3) the liquid Ag films of step (2) in thermal station are cured, obtains silver-colored conductive film.
  2. 2. a kind of method for reducing MOD type silver ink water film defects by adjusting ink droplet spacing according to claim 1, It is characterized in that：Substrate described in step (1) is length and width 1cm × 1cm, the sheet glass of thickness 0.7mm.
  3. 3. a kind of method for reducing MOD type silver ink water film defects by adjusting ink droplet spacing according to claim 1, It is characterized in that：Cleaning described in step (1) refers to successively using isopropanol, tetrahydrofuran, alkaline cleaning fluid, deionized water and different Propyl alcohol is cleaned by ultrasonic.
  4. 4. a kind of method for reducing MOD type silver ink water film defects by adjusting ink droplet spacing according to claim 1, It is characterized in that：Drying temperature described in step (1) is 80~85 DEG C.
  5. 5. a kind of method for reducing MOD type silver ink water film defects by adjusting ink droplet spacing according to claim 1, It is characterized in that：MOD type silver ink waters solid content described in step (2) are 15%, and viscosity is 9~15cps, surface tension for 30~ 32dynes/cm, the solvent used are 130~150 DEG C with reference to sintering temperature for ethyl alcohol, and corresponding resistivity is 4.2 μ Ω cm。
  6. 6. a kind of method for reducing MOD type silver ink water film defects by adjusting ink droplet spacing according to claim 1, It is characterized in that：The parameter of inkjet printing described in step (2) is：1000 μm of nozzle and substrate spacing, 50~55 DEG C of base reservoir temperature, 50~55 DEG C of nozzle temperature.
  7. 7. a kind of method for reducing MOD type silver ink water film defects by adjusting ink droplet spacing according to claim 1, It is characterized in that：Cured temperature described in step (3) is 160~165 DEG C.
  8. 8. a kind of method for reducing MOD type silver ink water film defects by adjusting ink droplet spacing according to claim 1, It is characterized in that：The cured time described in step (3) is 1min.
CN201711323607.3A 2017-12-13 2017-12-13 A kind of method for reducing MOD type silver ink water film defects by adjusting ink droplet spacing Pending CN108231277A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102529479A (en) * 2011-12-23 2012-07-04 中国科学院苏州纳米技术与纳米仿生研究所 Post-treatment method for improving printing evenness of electronic material
US8463116B2 (en) * 2008-07-01 2013-06-11 Tap Development Limited Liability Company Systems for curing deposited material using feedback control
CN106229259A (en) * 2016-08-13 2016-12-14 华南理工大学 The preparation method that a kind of thin film transistor (TFT) prints electrode
CN106585156A (en) * 2016-11-16 2017-04-26 华南理工大学 Ultraviolet light curing post-processing method for printing electrode
CN106752381A (en) * 2016-12-02 2017-05-31 东北大学 Without particle silver inks water and preparation method thereof and transparent silver-colored conductive film and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8463116B2 (en) * 2008-07-01 2013-06-11 Tap Development Limited Liability Company Systems for curing deposited material using feedback control
CN102529479A (en) * 2011-12-23 2012-07-04 中国科学院苏州纳米技术与纳米仿生研究所 Post-treatment method for improving printing evenness of electronic material
CN106229259A (en) * 2016-08-13 2016-12-14 华南理工大学 The preparation method that a kind of thin film transistor (TFT) prints electrode
CN106585156A (en) * 2016-11-16 2017-04-26 华南理工大学 Ultraviolet light curing post-processing method for printing electrode
CN106752381A (en) * 2016-12-02 2017-05-31 东北大学 Without particle silver inks water and preparation method thereof and transparent silver-colored conductive film and preparation method thereof

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