CN106413917B - Pattern forming method, the substrate with transparent conductive film, device and e-machine - Google Patents
Pattern forming method, the substrate with transparent conductive film, device and e-machine Download PDFInfo
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- CN106413917B CN106413917B CN201580005367.5A CN201580005367A CN106413917B CN 106413917 B CN106413917 B CN 106413917B CN 201580005367 A CN201580005367 A CN 201580005367A CN 106413917 B CN106413917 B CN 106413917B
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- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/12—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns
- H05K3/1241—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns by ink-jet printing or drawing by dispensing
- H05K3/125—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns by ink-jet printing or drawing by dispensing by ink-jet printing
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/119—Deposition methods from solutions or suspensions by printing
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1343—Electrodes
- G02F1/13439—Electrodes characterised by their electrical, optical, physical properties; materials therefor; method of making
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1884—Manufacture of transparent electrodes, e.g. TCO, ITO
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/0286—Programmable, customizable or modifiable circuits
- H05K1/0287—Programmable, customizable or modifiable circuits having an universal lay-out, e.g. pad or land grid patterns or mesh patterns
- H05K1/0289—Programmable, customizable or modifiable circuits having an universal lay-out, e.g. pad or land grid patterns or mesh patterns having a matrix lay-out, i.e. having selectively interconnectable sets of X-conductors and Y-conductors in different planes
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/09—Use of materials for the conductive, e.g. metallic pattern
- H05K1/092—Dispersed materials, e.g. conductive pastes or inks
- H05K1/095—Dispersed materials, e.g. conductive pastes or inks for polymer thick films, i.e. having a permanent organic polymeric binder
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
- H05K2201/01—Dielectrics
- H05K2201/0104—Properties and characteristics in general
- H05K2201/0108—Transparent
Abstract
The present invention provides a kind of pattern forming method, inhibits what is generated when forming linear liquid to swell, can be stably formed the pattern comprising filament, and the get both higher transparency and invisible.Pattern forming method, which is included, sprays the liquid comprising functional material using droplet ejection apparatus (H), and the drop successively sprayed is integrated on substrate (1), the process of the linear liquid (2) comprising functional material is formed as a result,；By making linear liquid (2) evaporation, dry, the process for making functional material selectively be deposited in the edge of linear liquid (2).Become 4.5 × 10 with the drop supply amount of linear liquid- 10~5.5 × 10- 9[m3/ m] mode controlled, and it is controlled in such a way that the contact angle on substrate (1) becomes 10~45 [°] by drop, and with by drop in the case where the diameter of the single land drop on substrate (1) is set as D [m] and the ejection interval on the substrate of drop (1) is set as p [m], with spray frequency f [1/s] relationship meet following formula: fp/D >=150.
Description
Technical field
The present invention relates to be formed in edge part accumulate functional property material film pattern forming method, using by the painting
Substrate with transparent conductive film, device and e-machine obtained from the film that film forming method is formed.
Background technique
In recent years, the multifunction, densification of device are developed, and are seeking to be formed containing functional material
The technology of small pattern, while also requiring cost effective, manufacturing process simplification.
As above-mentioned method for forming pattern, proposes and form pattern using print process.But use various print processes, pole
Limit also only forms 20 μm of line width or so of pattern, it is difficult to meet required miniaturization.
Patent document 1 is described through the convection current using liquid internal, and the solid component contained in liquid is gathered in painting
The peripheral portion of film, so as to form more small electrical wiring pattern compared with film size.
On the other hand, in recent years, with the raising of the demand of slim TV etc., liquid crystal, plasma, organic electroluminescence are developed
The display technology of the various modes such as luminous or Flied emission.In the different all displays of these display modes, transparent electrode is
Required constituent element.In addition, in addition to television set, even if in touch panel, mobile phone, Electronic Paper, various solar-electricities
In pond, various electroluminescent Light modulating devices, transparent electrode is also indispensable technology.
In the past, transparent electrode was mainly made in the transparent substrates such as glass or transparent plastic foil using by sputtering method
Ito transparent electrode made of indium-tin composite oxides (ITO) film.
But the indium used in ITO is rare metal, and at high price, therefore, it is intended that not using indium.In addition, sputtering
The problem of method is long there are the production time, and materials'use efficiency is excessively poor etc, for ito transparent electrode, there are high costs
Such big problem.
Therefore, it is had become a top priority instead of the exploitation of the transparent electrode of ito transparent electrode.
In this regard, describing a kind of transparent conductive film in patent document 2, the convection current of liquid internal is utilized, liquid is included
Some Nano silver grains are gathered in the peripheral portion of film and the small annular patterns being made of Nano silver grain are made to be interconnected
It forms.
A kind of transparent conductive film is described in patent document 3, utilizes the convection current of liquid internal, the carbon that will contain in liquid
Nanotube aggregates the peripheral portion and having of film be made of carbon nanotube it is interconnected made of multiple small cyclic annular figures
Case.
A kind of transparent conductive film is recorded in non-patent literature 1,2, the drop for spraying ink-jet method is combined into one on substrate
Body is formed after linear liquid, and using the convection current of liquid internal, Nano silver grain contained in liquid is gathered in threadiness
The small thread pattern being made of Nano silver grain is configured to mesh-shape as a result, by the peripheral portion of liquid.
Existing technical literature
Patent document
Patent document 1: Japanese Patent No. 4325343
Patent document 2:WO2011/051952
Patent document 3: Japanese Unexamined Patent Application Publication 2011-502034 bulletin
Non-patent literature 1:V.Bromberg, S.Ma, T.J.Singler, Appl.Phys.Lett.102,214101
(2013)
Non-patent literature 2:Z.Zhang, X, Zhang, Z.Xin, M.Deng, Y.Wen, Y.Song, Advanced
Materials 2013 Vol:25(46):6714-6718
Invent the technical issues of solved
It, can be by when forming longer linear pattern in method for forming pattern documented by patent document 1, non-patent literature 1
It to shrink glomerate power and generate and swell in being influenced by liquid internal pressure, a part of linear liquid is cut off, or
Linearity is disintegrated.As a result, a part for being deposited in the pattern of the functional material of above-mentioned linear liquid end is cut off, or figure
Case shape is uneven, and therefore, the stability that pattern is formed becomes technical problem.
In technology documented by patent document 2,3, in order to form transparent electrode by annular patterns, need to make each ring with
Minimum two rings intersection ensures to be electrically connected, as a result, necessarily being formed multiple points of contact (intersection point) on the electrode of face.Therefore, even
There are rooms for improvement in the viewpoint of the number control of the shape stability and point of contact of node.In addition, when resistance value is reduced to
When specified value, it cannot sufficiently solve the problems, such as that the transparency is also greatly reduced.
In non-patent literature 2, the drop supply amount of above-mentioned threadiness liquid is less, therefore, is deposited in each filament of edge part
Pattern spacing narrows.When therefore, in order to keep visibility minimum and be configured at thread pattern in face, there are the transparencys to be easy to impaired
The problem of.
Therefore, technical problem of the invention is, provides a kind of pattern forming method, inhibits to produce when forming linear liquid
Raw swells, and can be stably formed the pattern comprising filament, and the get both higher transparency and invisible.
In addition, another technical problem of the invention is, the substrate (transparent electrode) with transparent conductive film is provided, has this
The device and e-machine of substrate, the substrate with transparent conductive film with identical resistance value in the case where being compared, tool
The transparency, the excellent characteristics of visibility can be improved by having.
In addition, other technical problems of the invention can be defined by following record.
Solution for solving technical problems
The technical problem is solved by each invention below.
1. a kind of pattern forming method, this method comprises:
The liquid comprising functional material is sprayed by droplet ejection apparatus, and the drop successively sprayed is combined on substrate
One, the process that the linear liquid comprising the functional material is consequently formed；
Make the linear liquid evaporation, drying, so that the functional material be made selectively to be deposited in the linear liquid
The process at the edge of body, wherein
The drop supply amount for controlling the linear liquid is 4.5 × 10-10[m3/ m] more than 5.5 × 10- 9[m3/ m] hereinafter,
And the drop after control ejection is 10 [°] or more, 45 [°] hereinafter, also, after it will spray to the contact angle of the substrate
The drop single land drop on the substrate diameter be set as D [m], by the drop after ejection in the base
In the case that ejection interval on material is set as p [m], control sprays so that D [m], p [m] and the relationship of ejection frequency f [1/s] are full
The condition of foot formula,
[mathematical expression 1]
f·p/D≥150。
2. the pattern forming method as documented by described 1, wherein spray dress using the drop with grey change mechanism
It sets.
3. the pattern forming method as documented by described 1 or 2, wherein when carrying out the drying of the linear liquid, to institute
Substrate is stated to be heated or the substrate is dried using drying machine.
4. the pattern forming method as documented by described any one of 1~3, wherein the liquid before the drying
Functional material containing ratio be 0.1 weight % or more, 5 weight % range below.
5. the pattern forming method as documented by described any one of 1~4, wherein the functional material is electric conductivity
Material or conductive material precursor.
6. a kind of substrate with transparent conductive film has in substrate surface comprising being remembered by described any one of 1~5
The transparent conductive film for the pattern that the pattern forming method of load is formed.
7. a kind of device, with the substrate with transparent conductive film documented by described 6.
8. a kind of e-machine, with device documented by described 7.
Detailed description of the invention
Fig. 1 is the concept map for illustrating method for forming pattern of the invention；
Fig. 2 is the figure for illustrating the ejection condition of pattern forming method of the invention；
Fig. 3 is the schematic diagram for illustrating pattern forming method of the invention；
Fig. 4 is the top view for indicating the example formed according to the pattern that the present invention carries out；
Fig. 5 is the partly enlarged top view for indicating an example of the pattern formed according to the present invention；
Fig. 6 is the vi-vi line profile of Fig. 4；
Fig. 7 is the figure for illustrating embodiment.
Description of symbols
1: substrate
2: linear liquid
3: pattern
30: film section
31,32: filament
H: droplet ejection apparatus
Specific embodiment
Hereinafter, being illustrated to mode for carrying out the present invention.
In method for forming pattern of the invention, the liquid comprising functional material is sprayed by drop spray method, and make shape
At in the linear liquid evaporation on substrate, drying, make as a result, functional material be selectively piled up in linear liquid edge and
Pattern is formed, Fig. 1 shows concept maps.
In Fig. 1, H is droplet ejection apparatus.As droplet ejection apparatus, so-called ink-jet recording apparatus, which can be used, to be had
Ink gun be just not particularly limited but as long as aftermentioned ejection condition of the invention can be realized.As droplet ejection apparatus
Drop emitting mechanism, is not particularly limited, but radiating mode, piezo electrics, continuation mode can be enumerated etc..
1 is substrate, and 2 be the linear liquid comprising functional material, and 3 is by being piled up in functional material selectively
The edge of linear liquid 2 and the pattern formed.
As shown in Fig. 1 (a), scans droplet ejection apparatus H and substrate 1 in opposite directions, sprayed on one side from droplet ejection apparatus H
It out include the liquid of functional material, the drop successively sprayed is integrated on substrate, and being formed as a result, includes functional material
Linear liquid 2.
Then, as shown in Fig. 1 (b), make the linear evaporation of liquid 2, drying, be thus piled up in functional material selectively
The edge of linear liquid 2.
In this way, forming the pattern 3 being made of the filament comprising functional material on substrate 1 as shown in Fig. 1 (c).By 1
The pattern 3 that item threadiness liquid 2 is formed is made of one group of two filament 31,32.
For the present invention, when forming this pattern 3, can get both the higher transparency and invisible, therefore, excellent
Choosing uses.
It should be noted that " transparency " and " invisible " is distinguishing in this specification." transparency " is based on saturating
The transmissivity of the light of pattern is crossed to evaluate.On the other hand, " invisible " based on by visual observation come the difficulty of identification icon come
Evaluation.It cannot see that the filament for constituting pattern, invisible are more excellent.Even if transmittance is identical, invisible also has can
Difference can be generated, the explanation such as carried out below referring to Fig. 4, the present invention not only can be effectively used for radioparent realization, but also can
Effective for the realization of invisible.
Fig. 2 is the figure for illustrating the ejection condition of pattern forming method of the invention.Fig. 2 (a) indicates Fig. 1 from side
(a) drop in sprays the situation of state, and Fig. 2 (b) indicates that the drop in top view 1 (a) sprays the situation of state.
As shown in Fig. 2, making droplet ejection apparatus H and the opposite scanning in the x-direction of substrate 1 comprising function in present embodiment
The drop of energy property material successively sprays, and is integrated on substrate 1, forms linear liquid 2 as a result,.
At this point, the diameter for spraying land drop when drop is landed to substrate 1 is set as D [m], the ejection of drop will be sprayed
When interval is set as p [m], when meeting the relationship indicated by following formula (1), land drop is integrated on substrate 1, is formed linear
Liquid 2.
[mathematical expression 2]
p/D≤1…(1)
In addition, the diameter D [m] of land drop can be according to contact angle θ [rad], the ejection drop for spraying drop and substrate
Measure V [m3] and (2) calculate according to the following formula.In addition, contact angle is static contact angle, it can be by acquiring as follows, such as use association
With the DM-500 of interface science Co., Ltd. manufacture, under 25 DEG C, 50%RH environment, the drop (5 μ l or so) that will measure from
Syringe is injected on substrate 1, and measures the tangent line of drop end and the angle of substrate surface composition.
[mathematical expression 3]
It is integrated on substrate by the drop that drop spray method successively sprays, is thus generated when forming linear liquid
It swells, therefore, a part of linear liquid is cut off sometimes or linearity is disintegrated.It is piled up in as a result, creating the problem that
A part of the pattern of functional material of the end of linear liquid is cut off or pattern form becomes uneven.
The present inventor is conceived to this swell due to behind the scanning direction for landing drop inflow droplet ejection apparatus
It is generated in the linear liquid of side, and finds the line for flowing into scanning direction rear from the land drop for giving by ejection drop
Same or more the liquid measure of liquid measure in shape liquid, it is possible thereby to inhibit to swell generation.
Certain land that composition, droplet ejection apparatus, substrate type according to the liquid comprising functional material is selected
For the diameter D [m] of drop, interval p [m] is sprayed with reducing, land drop flows into the linear liquid at scanning direction rear
Liquid measure become it is more.That is, supplying more liquid measures by reduce the amount for spraying interval p [m] from drop is sprayed, can inhibit and swell.
In method for forming pattern of the invention, it is set as in the diameter of the single land drop by the above-mentioned drop after spraying on above-mentioned substrate
D [m] is sprayed by the above-mentioned drop after ejection in the case where the ejection interval on above-mentioned substrate is set as p [m] by control
So that D [m], p [m] and the relationship of ejection frequency f [1/s] meet the condition of following formula (3), line width can be formed uniformly and linearity
Higher threadiness liquid.
[mathematical expression 1]
f·p/D≥150……(3)
In addition, preferably being driven by gray scale in the case where having used the droplet ejection apparatus that can spray regulation drop amount
To control drop amount.I.e., it is preferable to use the droplet ejection apparatus with grey change mechanism.Grey is that 1 point is squeezed into
Ink droplet number.
Fig. 3 is the schematic diagram for illustrating pattern forming method of the invention.
Linear liquid 2 is during dry on substrate 1, according to the composition of linear liquid 2, substrate 1 and linear liquid 2
The selection of contact angle, functional material concentration and drying condition controls the Convection states of linear liquid 2, thus, it is possible to make function
Property material selectivity it is piled up in the edge of linear liquid 2.
Utilize pair at the edge for illustrating that functional material can be made selectively to be piled up in linear liquid 2 in the present invention Fig. 3
Stream mode.For the drying for the linear liquid 2 being configured on substrate 1, the drying at edge than the fast drying in central portion, with
Dry progress, solid component concentration reach saturated concentration, cause the part of solid component to be precipitated at the edge of linear liquid 2.
Using the solid component of the precipitation, the edge of linear liquid 2 becomes the state being immobilized, and inhibits caused by subsequent drying
Contraction of the linear liquid 2 in width direction.By the effect, it is extrorse right from central portion stream that the liquid of linear liquid 2 is formed
Stream, to supplement the liquid due to evaporating the amount lost at edge.
Immobilization and linear liquid 2 central portion of the convection current due to the contact line of dry caused linear liquid 2 and
The difference of the evaporation capacity at edge and cause, therefore, pass through contact angle, the line according to solid component concentration, linear liquid 2 and substrate 1
Amount, the heating temperature of substrate 1, the configuration density or temperature, humidity, the environmental factor of air pressure of linear liquid 2 of shape liquid 2
It is changed, and adjusts these factors, can control the convection current.
In the present invention, linear liquid 2 is preferably 10 [°] or more 45 [°] range below relative to the contact angle of substrate 1.
When contact angle is lower than 10 [°], it is not easy to cause the immobilization of the contact line of linear liquid 2, when contact angle is more than 45 [°], linear liquid
The difference of the evaporation capacity at 2 central portion of body and edge is smaller, and the slave central portion in linear liquid 2 cannot be promoted to flow to the convection current of edge.?
In above-mentioned contact angular region, it is easy to cause the immobilization of the contact line of linear liquid 2, the central portion of linear liquid 2 and edge
The difference of evaporation capacity also becomes larger, and can promote in linear liquid 2 from the extrorse convection current of central portion stream.As a result, can be obtained further
Promote graph thinning and further increases the effect of the transparency.Linear liquid 2 can pass through the threadiness relative to the contact angle of substrate 1
The surface of the composition of liquid 2 or substrate 1 can setting adjust.
In addition, diffusion path of the difference of the evaporation capacity at linear 2 central portion of liquid and edge to the gas for being formed in droplet surface
Degree impacts.Accordingly, the drop supply amount of linear liquid 2 is clearly helpful for above-mentioned convection current.It is disposably formed in face a plurality of
It is linear due to the influence of adjacent linear liquid 2 when the drop supply quantitative change of linear liquid 2 is more in the case where linear liquid 2
The difference of the evaporation capacity at 2 central portion of liquid and edge becomes smaller, and will not significantly generate makes functional material selectively be piled up in threadiness
The above-mentioned convection current at the edge of liquid 2.As a result, filament width becomes larger, and the residual solids outside the pattern specified position of thin thread part
Ingredient, the damage transparency.
Pass through control drop amount V [m as a result,3] and spray interval p [m] the drop supply amount of linear liquid 2 is become
5.5×10- 9[m3/ m] hereinafter, above-mentioned convection current can be generated significantly.
As shown in the formation example of the pattern of Fig. 4, in face, with one group of the pattern 3 that the drying by linear liquid 2 is formed
Interval I between two thread patterns 31,32 and the thread pattern for being configured at side close to each other in the pattern 3 to adjoin each other
32, the J roughly the same mode in interval between 31 configures filament, as a result, (thoroughly in the case where configuring the identical filament of identical quantity
Penetrating property is identical) when being compared, the minimum effect of the visibility of filament can be obtained.Under same filament width, with one group two
The mode that interval I between thread pattern 31,32 broadens forms pattern, can be obtained maintaining higher radioparent state as a result,
The minimum effect of lower visibility.
Interval I between one group of two thread pattern 31,32 determines according to the line width I ' of linear liquid 2, the threadiness liquid 2
Line width I ' is selected according to the contact angle of the liquid comprising functional material and substrate 1 and drop supply amount.Through the invention
Pattern forming method control contact angular region in, by increasing drop supply amount, can widely design one group two thin
Interval I between line pattern 31,32 forms pattern, so that the visibility of filament be made to become in the state of maintaining higher transmittance
It obtains minimum.Specifically, it is preferable that becoming 4.5 × 10 with drop supply amount- 10[m3/ m] more than mode select drop amount V [m3]
P [m] is spaced with spraying.
According to the present invention, in the state of preventing from swelling generation, by increasing drop supply amount etc., interval I can be increased,
Thus, for example, for the value of interval J for being set to arbitrary value, can by with the close value of value of interval J, preferably substantive
Upper identical value is suitably given to interval I.I.e., it is possible to obtain matching in the state of keeping the stability of filament with desired interval
The advantageous effects set filament and reduce visibility etc..In this way, from the viewpoint of improving the freedom degree that filament is formed, it can also be real
Now significant effect.
As the explanation carried out above makes functional material selectively be piled up in linear liquid in formation according to the present invention
Edge part film method for forming pattern in, by inhibiting what is generated when forming linear liquid to swell, can steadily obtain
To the higher pattern of uniformity of shape, can get both the higher transparency and invisible.
In addition, according to the present invention it is possible to provide the transparency can be improved when comparing with identical resistance value, visibility has
The substrate (transparent electrode) with transparent conductive film of excellent characteristics, the device and e-machine for having the substrate.
Fig. 5 is that the partial enlargement of an example for the pattern for indicating that pattern forming method through the invention is formed on substrate is put down
View.Fig. 6 is the vi-vi line profile in Fig. 5, is one group of two filament being included by pattern along vertical with line segment direction
Direction cutting sectional view (profilograph).
In the present invention, one group of two filament (line segment) 31,32 of the pattern 3 generated by 1 linear liquid do not need be
Mutual completely self-contained island.As shown, 2 line segments 31,32 are formed as the non-individual body connected by film section 30, and film section 30 exists
It is formed between the line segment 31,32 with the height lower than the height of the line segment 31,32, this is also preferred in the present invention.
In the present invention, line width W1, W2 of the line segment 31,32 of pattern 3 is respectively preferably 10 μm or less.If it is 10 μm with
Under, then become generally can not visuognosis level, therefore, from improve the transparency from the viewpoint of, more preferably.If also considered
The stability of each line segment 31,32, then line width W1, W2 of each line segment 31,32 is respectively preferably 2 μm or more 10 μm of ranges below.
In addition, width W1, W2 of line segment 31,32 such as give a definition in the present invention: by the functionality between the line segment 31,32
The height of the most thin thinnest part of material thickness is set as Z, then the projecting height for starting line segment 31,32 from the Z is set as Y1, Y2
When, the width of the line segment 31,32 at the height of the half of Y1, Y2 is defined as width W1, W2.For example, pattern 3 have it is above-mentioned thin
When film portion 30, the height of the thinnest part in the film section 30 can be set as Z.In addition, the functional material between each line segment 31,32
The height of thinnest part when being 0, line width W1, W2 of line segment 31,32 be defined as height h1 of the line segment 31,32 away from 1 surface of substrate,
The width of line segment 31,32 at the height of the half of h2.
In the present invention, constitute the line segment 31,32 of pattern 3 line width W1, W2 be as described above it is superfine, therefore, from true
From the viewpoint of protecting sectional area, realizing low resistance, preferably height h1, h2 higher of the line segment 31,32 away from 1 surface of substrate.Specifically
For, height h1, h2 of line segment 31,32 is preferably 5 μm of ranges below of 50nm or more.
In addition, from the viewpoint of the stability for improving pattern 3, h1/W1 ratio, h2/W2 ratio are respectively preferably in the present invention
0.01 or more 1 range below.
In addition, from the viewpoint of the graph thinning for further increasing pattern 3, in the thickness of 31,32 functional materials of line segment
The height Z of the most thin thinnest part of degree, specifically the height Z of the thinnest part of film section 30 is preferably 10nm model below
It encloses.In order to realize the balance of the get both transparency and stability, most preferably has film section 30 in the range of 0 < Z≤10nm.
In addition, h1/Z ratio, h2/Z ratio are respectively preferably 5 or more, more in order to improve the further graph thinning of pattern 3
Preferably 10 or more, particularly preferably 20 or more.
The interval I of line segment 31,32 can be suitably adjusted, and preferably be adjusted to 10 μm or more 300 μm of ranges below.Separately
Outside, as above-mentioned, interval I is preferably adjusted to the value close with the interval J that illustrates using Fig. 4, be most preferably adjusted to actually with
Every the equal value of J.In addition, in the present invention, the interval I of line segment 31,32 be defined as between each maximum protruding portion of line segment 31,32 away from
From.
In addition, identical shape (area of section of same degree) preferably is assigned to line segment 31 and line segment 32 in the present invention,
Specifically, the height h1 and h2 of line segment 31 and line segment 32 are preferably the value being substantially equal.Equally, it is also preferred that line segment 31 and line
The line width W1 and W2 of section 32 are the value being substantially equal.
In the present invention, line segment 31,32 is not necessarily required to be parallel, as long as at least in certain length L of line segment direction, line segment
31, it 32 does not combine.Preferably at least in certain length L of line segment direction, line segment 31,32 is substantial parallel.
In the present invention, the length L of the line segment direction of line segment 31,32 is preferably 5 times or more of the interval I of line segment 31,32, more
Preferably 10 times or more.Length L and interval I can be set with the formation length and formation width of corresponding pattern (linear liquid) 2
It is fixed.
In the present invention, the formation initial point and terminal of linear liquid 2 (through the initial point and terminal of certain length L of line segment direction)
In, line segment 31,32 connects and is formed as non-individual body, this is also preferred in the present invention.
In addition, its preferred line width W1, W2 of line segment 31,32 is roughly equal, and line width W1, W2 and 2 wire spacings (interval I)
Compared to being very thin.
Additionally, it is preferred that being formed simultaneously the line segment 31 and line segment 32 for constituting the pattern 3 generated by 1 linear liquid.
Particularly preferably each line segment 31,32 of pattern 3 of the invention all meets the condition of following (A)~(D).
(A) height of each line segment 31,32 is set as h1, h2, and the height of the thinnest part between each line segment is set as Z
When, 5≤h1/Z and 5≤h2/Z.
(B) when the width of each line segment 31,32 being set as W1, W2, W1≤10 μm and W2≤10 μm.
(C) when the distance between each line segment 31,32 being set as I, 10 μm≤I≤300 μm.
(D) when the height of each line segment 31,32 being set as h1, h2,5 μm of 50nm < h1 < and 5 μm of < of 50nm < h2.
Including at least pattern forming method through the invention be formed in the pattern of substrate surface with transparent conductive film
Substrate, in the case where being compared with same resistance value, the transparency, the excellent characteristics of invisible can be improved by having.
Substrate used in the present invention is not particularly limited, such as can enumerate: glass, plastics (poly terephthalic acid second two
Alcohol ester, polybutylene terephthalate, polyethylene, polypropylene, acrylic resin, polyester, polyamide etc.), metal (copper, nickel,
Aluminium, iron etc. or their alloy), ceramics etc., they can be used alone, and can also use in the state of fitting.Wherein,
Preferably plastics, and preferably polyolefin as polyethylene terephthalate or polyethylene, polypropylene etc..
Functional material used in the present invention is not particularly limited, but preferably before conductive material or conductive material
Body.Conductive material precursor refers to the material that can become conductive material by implementing proper treatment.
As conductive material, such as preferably enumerate electrically conductive microparticle, electric conductive polymer etc..
As electrically conductive microparticle, be not particularly limited, can be preferably listed out Au, Pt, Ag, Cu, Ni, Cr, Rh, Pd, Zn,
The particles such as Co, Mo, Ru, W, Os, Ir, Fe, Mn, Ge, Sn, Ga, In, it is especially if micro- using metal as Au, Ag, Cu
Grain, then be capable of forming the circuit pattern that resistance is low and corrosion resistance is strong, it is advantageous to.From cost and the viewpoint of stability
From the point of view of, the metal particle comprising Ag is preferred.The average grain diameter of these metal particles is preferably the range, more excellent of 1~100nm
It is selected as the range of 3~50nm.
In addition, further preferably using carbon particulate as electrically conductive microparticle.As carbon particulate, it is micro- to may be preferably exemplified out graphite
Grain, carbon nanotube, fullerene etc..
It as electric conductive polymer, is not particularly limited, can preferably enumerate pi-conjugated system's electroconductive polymer.
It as pi-conjugated system's electroconductive polymer, is not particularly limited, can use: polythiophene class, multi-metal polypyrrole, poly- Yin
Diindyl class, polycarbazole class, polyaniline compound, polyacetylene class, poly- furans, it is poly- to benzene class, p-phenylene vinylene's class, poly p phenylene sulfide class,
The chains electric conductive polymers such as poly- azulenes class, polyisothianaphthene class, polysulfur nitride class.Wherein, from higher electric conductivity can be obtained
Point from the point of view of, preferably polythiophene class or polyaniline compound.Most preferably polyethylene dioxythiophene.
Electric conductive polymer used in the present invention more preferably include above-mentioned pi-conjugated system's electroconductive polymer and poly- yin from
Son forms.It is high to pi-conjugated system's electric conductivity is formed by the presence of oxidant appropriate and oxidation catalyst, polyanion
The precursor monomer of molecule carries out chemical oxidising polymerisation, and such electric conductive polymer can be easily manufactured.
Polyanion be replace or unsubstituted polyalkylene, substitution or unsubstituted poly- alkenylene, substitution or
Unsubstituted polyimides, substitution or unsubstituted polyamide, substitution or unsubstituted polyester and their copolymer,
Comprising the Component units with anionic group and without the Component units of anionic group.
The polyanion be can make the dissolution of pi-conjugated system's electroconductive polymer in a solvent can soluble high molecular.In addition, poly- yin
The anionic group of ion is functioned as the dopant for pi-conjugated system's electroconductive polymer, improves pi-conjugated system's electric conductivity
High molecular electric conductivity and heat resistance.
As the anionic group of polyanion, as long as can occur to carry out chemistry to pi-conjugated system's electroconductive polymer
The functional group of Oxidation Doping, especially from the viewpoint of the difficulty of manufacture and stability, preferably monosubstituted sulphur
Perester radical, monoalkyl phosphate base, phosphate, carboxyl, sulfonic group etc..In addition, from functional group to pi-conjugated system's electroconductive polymer
Doping effect from the viewpoint of, more preferably sulfonic group, monosubstituted sulfate group, carboxyl.
As the specific example of polyanion, polyvinylsulfonic acid, polystyrolsulfon acid, polyallyl sulphur can be enumerated
Acid, polyacrylic acid ethylsulfonic acid, polyacrylic acid butyl sulfonic acid, poly- 2- acrylamide -2- methyl propane sulfonic acid, polyisoprene
Sulfonic acid, polyvinyl carboxylic acid, polystyrene carboxylic acid, polyallyl carboxylic acid, polyacrylic acid, polymethylacrylic acid, poly- 2- acryloyl
Amine -2- methylpropane carboxylic acid, polyisoprene carboxylic acid, polyacrylic acid etc..Either their homopolymer, be also possible to its 2
Kind or more copolymer.
Furthermore it is also possible to be the polyanion in compound with F (fluorine atom).Specifically, can enumerate containing
Perfluorinated sulfonic acid base Nafion (manufacture of Dupont company), the Flemion that is made of the perfluor type vinyl ethers containing carboxylic acid group
(manufacture of Asahi Glass company) etc..
In them, if it is the compound with sulfonic acid, then ink projects stability when using ink jet printing mode
It is especially good and high electric conductivity can be obtained, so more preferably.
In addition, the particularly preferred polystyrolsulfon acid, polyisoprene sulfonic acid, polyacrylic acid ethylsulfonic acid, poly- in them
Acrylic acid butyl sulfonic acid.Effect as excellent electric conductivity may be implemented in these polyanions.
The degree of polymerization of polyanion is preferably range of the monomeric unit at 10~100000, from solvent solubility and is led
From the point of view of electrical point, more preferably 50~10000 ranges.
Electric conductive polymer further preferably can use commercially available material.For example, for by poly- (3,4- ethylidene dioxy thiophenes
Pheno) and polystyrolsulfon acid constitute electric conductive polymer (referred to as PEDOT/PSS), it is commercially available to have: H.C.Starck company
CLEVIOS series, the PEDOT-PASS483095 of Aldrich, 560598, Nagase Chemtex company
Denatron series.In addition, commercially available polyaniline has: the ORMECON series of Nissan Chemical company.
In the present invention, as the liquid containing functional material, a kind or 2 of water or organic solvent etc. can be applied in combination
Kind or more.
Organic solvent is not particularly limited, such as can example: 1,2- hexylene glycol, 2- methyl -2,4- pentanediol, 1,3- fourth two
Glycols, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether, three such as alcohol, 1,4- butanediol, propylene glycol
Ethers such as glycol monoethyl ether, dipropylene glycol monomethyl ether, dipropylene glycol monoethyl ether etc..
In addition, table can also be contained in the range of not damaging effect of the present invention as the liquid containing functional material
The various additives such as face activating agent.
By using surfactant, such as when forming linear liquid 2 using droplet ejection apparatus, can adjust
Whole surface tension etc. and realize the stabilisation etc. sprayed.It as surfactant, is not particularly limited, silicon class surface can be used
Activating agent etc..The side chain or terminal that silicon class surfactant refers to dimethyl polysiloxane are through silicon class surface made of polyether-modified
Activating agent, for example, it is commercially available have SHIN-ETSU HANTOTAI's chemical industry manufacture KF-351A, KF-642, BYK Chemie manufacture BYK347,
BYK348 etc..Relative to the total amount for the liquid for forming linear liquid 2, the additive amount of surfactant is preferably 1 weight % or less.
The purposes of substrate with transparent conductive film of the invention is not particularly limited, and can be used for various e-machines and has
Various devices.
From the viewpoint of playing effect of the invention significantly, the substrate of the present invention with transparent conductive film is preferred
Purposes can for example function properly as the displays of the various modes such as liquid crystal, plasma, organic electroluminescent or Flied emission
With transparent electrode or touch panel, mobile phone, Electronic Paper, various solar batteries, various electroluminescent Light modulating devices etc.
Used in transparent electrode.
More particularly it relates to the substrate with transparent conductive film be preferably used as the transparent electrode of device.As
Device is not particularly limited, such as may be preferably exemplified touch panel sensor etc..In addition, as having these devices
E-machine is not particularly limited, such as may be preferably exemplified smart phone, tablet terminal etc..
Embodiment
Hereinafter, being illustrated to the embodiment of the present invention, but the present invention is not limited to embodiments.
(embodiment 1~13, comparative example 1~8)
Utilize ink gun (" KM512L " of Konica Minolta company manufacture；Standard drop amount 42pl, " KM512M "；Mark
Quasi- drop amount 14pl, or " KM512S "；Standard drop amount 4pl), under the conditions of the ink of the composition shown in table 1~5, ejection, with
Drop is ejected to the PS-1M using the manufacture of letter photoelectricity Qi Jizhuan Co., Ltd. by the mode that spacing is 423 μm between nozzle column direction
On the substrate surface for having carried out the PET film of Corona discharge Treatment, glass, COP film (substrate), the linear liquid of striped is formed.
The dry pattern, makes solid component be piled up in edge part, forms many one group of two thread patterns as a result,.Make to be formed with above-mentioned
After the substrate of pattern is rotated by 90 ° relative to ink gun scanning direction, many one group of two filaments are formed again with identical condition
Pattern, to form cancellous pattern as shown in Figure 7.
In addition, Fig. 7 (a), which is shown, is spaced smaller and smaller than the interval J situation of I according to what Fig. 4 illustrated, Fig. 7 (b) indicates interval
I is larger and the case where for interval J close value.In the present embodiment, the spacing of linear liquid is set as 423 μm, by 1 threadiness
Interval I (measured value of aftermentioned " two lines are wide ") between the filament 31,32 in pattern 3 that liquid is formed is sufficiently than (423 μm/2
=) 212 μm of small states are approximate with Fig. 7 (a), it is approximate with Fig. 7 (b) close to 212 μm of states.
(comparative example 9)
Utilize ink-jet printer (Fujifilm DMP-2831printer；Standard drop amount 10pl), the group shown in table 5
At ink, under the conditions of ejection, drop is ejected to using letter photoelectricity gas in such a way that spacing between nozzle column direction becomes 423 μm
The PS-1M of Ji Zhuan Co., Ltd. manufacture has carried out the glass substrate surface of Corona discharge Treatment, forms the linear liquid of striped.It is dry
The dry pattern, makes solid component be piled up in edge part, forms many one group of two thread patterns as a result,.Make to be formed with above-mentioned figure
After the substrate of case is rotated by 90 ° relative to ink gun scanning direction, many one group of two filament figures are formed again with identical condition
Case, and form cancellous pattern as shown in Figure 7.
In above embodiment 1~13, comparative example 1~9, following drying conditions and firing condition are applied.
< drying condition >
Substrate heating means: after liquid coating part is formed, heater plate substrate is used.
Substrate surface temperature: 70 DEG C
< firing condition >
Process for calcining: after liquid coating part is dry, heater plate substrate is used.
Substrate surface temperature: 120 DEG C, 1 hour
Swell that preventing property, two lines are wide, full light transmittance, invisible and sheet resistance to obtained pattern measurement
Value.Result is indicated in table 1~5.
< measuring method, evaluation assessment >
Swell preventing property
For the two lines property shown in the table 1~5, optical microphotograph sem observation is utilized, observes one group of two filament, confirmation
Swell preventing property.The sample swelled will be generated and be evaluated as "×", the sample swelled will not generated and be evaluated as "○".
Two lines are wide
For the two lines width (μm) shown in the table 1~5, using between one group of two filament of optical microscopy Observe and measure
Interval.Measured value is equivalent to above-mentioned interval I.
Transmissivity (full light transmittance)
Transmissivity shown in table 1~5 (full light transmittance) (%T) is manufactured using Tokyo electricity Se company
AUTOMATICHAZEMETER (MODEL TC-HIIIDP), measures value obtained from full light transmittance.In addition, being using not having
There is the substrate of pattern (transparent conductive film) to be modified and the full light transmittance as the pattern (transparent conductive film) after production
Value.
Invisible
For the invisible shown in the table 1~5, on light table (light table), from the position meat far from 50cm
The sample of eye observation embodiment 1~13, comparative example 1~9, is beyond recognition filament, and invisible is more excellent, specifically,
The sample that cannot recognize filament is evaluated as " A ", filament can will be slightly recognized but the practical upper sample that there is no problem is evaluated as
The sample that can clearly recognize filament is evaluated as " C " by " B ".
Sheet resistance
Sheet resistance shown in table 1~5 (Ω/) is the LORESTAEP manufactured using Dia Instruments society
The value of (MODELMCP-T360 type) array 4 probe detectors (ESP) measurement sheet resistance value.
[table 1]
[table 2]
[table 3]
[table 4]
[table 5]
In above-mentioned table 1~5, " DEGBE " is the abbreviation of diethylene glycol monobutyl ether, and " PET " is polyethylene terephthalate
Abbreviation, " COP " is the abbreviation of cyclic olefin polymer.
< evaluates >
In embodiment 1~13, it is known that swell wide preventing property, two lines, full light transmittance, invisible and sheet resistance
It is worth excellent.
In contrast, it is known that drop supply amount in face (to the drop supply amount on the scanning direction of droplet ejection apparatus)
It being unsatisfactory in the comparative example 1 of the scope of the present invention, invisible is poor, in the comparative example 2 for being more than the scope of the present invention, full light
Transmissivity, invisible, sheet resistance value difference.
In addition, knowing in the comparative example 3,4 for being unsatisfactory for the condition of formula of the invention (3), sheet resistance value difference.
[mathematical expression 4]
f·p/D≥150…(3)
(in above-mentioned formula, D [m] indicates that the diameter of the single land drop on base material of the drop after spraying, p [m] indicate spray
Drop ejection interval on base material after out, f [1/s] indicate to spray frequency.)
It also knows and is unsatisfactory for the comparative example 5 of the scope of the present invention, more than the comparative example 6 of the scope of the present invention in contact angle
In, full light transmittance, invisible, sheet resistance value difference.
It is further known that in the comparative example 7,8 for being unsatisfactory for the condition of above-mentioned formula (3), sheet resistance value difference, the liquid in face
Drop supply amount (to the drop supply amount on the scanning direction of droplet ejection apparatus) is unsatisfactory in the comparative example 9 of the scope of the invention,
Invisible is poor.In addition, these comparative examples 7~9 are the examples based on condition documented by non-patent literature 1,2.
Claims (5)
1. a kind of pattern forming method, this method comprises:
The liquid containing functional material is sprayed by droplet ejection apparatus, and the drop successively sprayed is combined into one on substrate
Body, the process that the linear liquid comprising the functional material is consequently formed；
Make the linear liquid evaporation, drying, so that the functional material be made selectively to be deposited in the linear liquid
The process at edge,
Wherein,
Drop supply amount control by the linear liquid is 4.5 × 10-10m3/ m or more 5.5 × 10-9m3/ m will be hereinafter, and will spray
The contact angle control of the drop and the substrate afterwards is for 10 ° or more 45 ° hereinafter, also, the drop after it will spray
The diameter of single land drop on the substrate is set as D, will be between the ejection of the drop on the substrate after ejection
When being set as p, control sprays so that the relationship of D, p and ejection frequency f meet the condition of following formula, and the unit of the diameter D is m,
The unit for spraying interval p is m, and the unit for spraying frequency f is 1/s,
[mathematical expression 1]
f·p/D≥150。
2. pattern forming method as described in claim 1, wherein
Use the droplet ejection apparatus with grey change mechanism.
3. pattern forming method as claimed in claim 1 or 2, wherein
When carrying out the drying of the linear liquid, the substrate is heated to dry the linear liquid or using dry
Dry machine dries the linear liquid.
4. pattern forming method as claimed in claim 1 or 2, wherein
The functional material containing ratio of the liquid before the drying is 0.1 weight % or more, 5 weight % range below.
5. pattern forming method as claimed in claim 1 or 2, wherein
The functional material is conductive material or conductive material precursor.
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| JP2014-011726 | 2014-01-24 | ||
| JP2014011726 | 2014-01-24 | ||
| PCT/JP2015/051924 WO2015111731A1 (en) | 2014-01-24 | 2015-01-23 | Pattern formation method, substrate provided with transparent electroconductive film, device, and electronic instrument |
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| WO2015199201A1 (en) * | 2014-06-25 | 2015-12-30 | コニカミノルタ株式会社 | Method for forming mesh-shaped functional pattern, mesh-shaped functional pattern, and functional substrate |
| JP6540698B2 (en) * | 2014-06-25 | 2019-07-10 | コニカミノルタ株式会社 | Pattern forming method, substrate with transparent conductive film, device and electronic device |
| WO2016140284A1 (en) * | 2015-03-02 | 2016-09-09 | コニカミノルタ株式会社 | Pattern formation method, transparent conductive film-equipped substrate, device, and electronic apparatus |
| WO2020044404A1 (en) | 2018-08-27 | 2020-03-05 | コニカミノルタ株式会社 | Method for forming conductive thin wire, method for producing transparent conductor, method for producing device, and set of conductive ink and base material |
| CN112349871B (en) * | 2019-12-09 | 2023-02-07 | 广东聚华印刷显示技术有限公司 | Metal grid electrode and preparation method thereof |
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| JP6508062B2 (en) | 2019-05-08 |
| CN106413917A (en) | 2017-02-15 |
| JPWO2015111731A1 (en) | 2017-03-23 |
| WO2015111731A1 (en) | 2015-07-30 |
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