TWI518739B - Method for making a conductive substrate - Google Patents
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- TWI518739B TWI518739B TW100139124A TW100139124A TWI518739B TW I518739 B TWI518739 B TW I518739B TW 100139124 A TW100139124 A TW 100139124A TW 100139124 A TW100139124 A TW 100139124A TW I518739 B TWI518739 B TW I518739B
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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
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
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- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F3/00—Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
- G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
- G06F3/03—Arrangements for converting the position or the displacement of a member into a coded form
- G06F3/041—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
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- 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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- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F2203/00—Indexing scheme relating to G06F3/00 - G06F3/048
- G06F2203/041—Indexing scheme relating to G06F3/041 - G06F3/045
- G06F2203/04103—Manufacturing, i.e. details related to manufacturing processes specially suited for touch sensitive devices
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Description
本發明是有關於一種製造導電基材的方法,特別是指一種形成一具有微結構表面之導電基材的方法。This invention relates to a method of making a conductive substrate, and more particularly to a method of forming a conductive substrate having a microstructured surface.
導電基材可以被應用到光電裝置,如顯示器、觸控面板、感測器、電子紙、及光學元件等。The conductive substrate can be applied to photovoltaic devices such as displays, touch panels, sensors, electronic paper, and optical components.
典型的導電基材,例如電阻式或電容式觸控基板,通常具有一基底材,及一形成在基底材之一表面上的金屬或金屬氧化物透明導電層。由於觸控基板以觸控筆進行觸壓劃線時,位於上層之導電層會受外力而產生局部區域形變,進而使得兩彼此間隔導電層間接觸並導通。但由於兩導電層接觸時會產生沾黏現象,當觸壓之外力消失時,位於上層之導電層將回復原狀,此時會使導電層受到一拉扯的力量。故而在重覆觸壓劃線(例如以觸控筆觸壓劃線)下容易導致導電層的破裂剝離,使得導電層的電阻值升高而致電性不穩定情形發生。因此如何改善導電層與基底材的結合強度及導電層本身的結構強度並防止導電層在外力下產生裂縫及剝離是一重要課題。A typical conductive substrate, such as a resistive or capacitive touch substrate, typically has a substrate and a metal or metal oxide transparent conductive layer formed on one surface of the substrate. When the touch substrate is touch-scored with the stylus, the conductive layer located in the upper layer is deformed by an external force to cause local area deformation, thereby causing the two conductive layers to contact and conduct. However, due to the adhesion of the two conductive layers, when the force is lost, the conductive layer in the upper layer will return to its original state, and the conductive layer will be subjected to a pulling force. Therefore, under repeated touch scribe lines (for example, with a stylus touch-pressure scribe line), the conductive layer is easily broken and peeled off, so that the resistance value of the conductive layer is increased and the callability instability occurs. Therefore, how to improve the bonding strength between the conductive layer and the substrate and the structural strength of the conductive layer itself and prevent the conductive layer from cracking and peeling under external force is an important issue.
美國專利早期公開2003/0087119揭露一種透明導電基材,其具有一透明聚合物基底材,一形成在該透明聚合物基底材上的透明導電層,及一覆蓋在該透明導電層上的覆蓋層。該覆蓋層的材料可為金屬氧化物、金屬氮化物、金屬氮氧化物、碳、碳化氮、碳化矽等。藉由該覆蓋層而可以防止透明導電層在外力下產生裂縫或剝離。但由於該覆蓋層要以濺鍍方式形成,因此使得製造該透明導電基材的製程較為複雜。US Patent Publication No. 2003/0087119 discloses a transparent conductive substrate having a transparent polymer substrate, a transparent conductive layer formed on the transparent polymer substrate, and a cover layer overlying the transparent conductive layer. . The material of the cover layer may be a metal oxide, a metal nitride, a metal oxynitride, carbon, nitrogen carbide, tantalum carbide or the like. By the cover layer, it is possible to prevent the transparent conductive layer from being cracked or peeled under an external force. However, since the cover layer is formed by sputtering, the process for manufacturing the transparent conductive substrate is complicated.
美國專利6,629,833揭露一種透明導電基材,其具有一塑膠基底材,一形成在該塑膠基底材上的含離子基團樹脂層,及一形成在該含離子基團樹脂上的透明導電層。藉由該含離子基團樹脂的黏著性,該透明導電層可以牢固地黏合於該塑膠基底材上以防止透明導電層在外力下產生裂縫或剝離。但因為該含離子基團樹脂具有黏著性,使得在製造透明導電基材的過程中容易沾黏灰塵等外來的微粒。U.S. Patent 6,629,833 discloses a transparent conductive substrate having a plastic substrate, an ionic group-containing resin layer formed on the plastic substrate, and a transparent conductive layer formed on the ionic group-containing resin. By the adhesion of the ionic group-containing resin, the transparent conductive layer can be firmly adhered to the plastic substrate to prevent cracking or peeling of the transparent conductive layer under external force. However, since the ionic group-containing resin has adhesiveness, it is easy to adhere to foreign particles such as dust during the process of manufacturing the transparent conductive substrate.
除以上方法外,習知另一類防止導電層在外力下產生裂縫及剝離的方式,係藉由於導電層表面形成凹凸微結構藉以減少兩導電層間之接觸面積,藉此即可有效減少導電層因接觸而沾黏所導致之拉扯力量,進而延長導電層之使用壽命。In addition to the above methods, another conventional method for preventing cracks and peeling of the conductive layer under external force is to reduce the contact area between the two conductive layers by forming a concave-convex microstructure on the surface of the conductive layer, thereby effectively reducing the conductive layer The pulling force caused by contact and adhesion increases the service life of the conductive layer.
一般所習知製作微結構的方法有物理壓印法或化學蝕刻法等,惟該些方法均有其製程所導致之先天缺陷。例如,物理壓印法因壓印力不易均勻,故而易影響微結構之精度及尺寸,且壓印出之微結構多半具有折角狀結構(如鋸齒、直角或梯形結構),此折角之存在會使得導電層更易因應力集中而加速破損或不易形成連續導電層;而美國專利6,036,579中提及之化學蝕刻法,其中所用之蝕刻液價格昂貴,並且會造成環境污染,且蝕刻出之微結構亦多半具有折角,故亦有與物理壓印法相同之問題。Generally, methods for fabricating microstructures include physical imprinting or chemical etching, etc., but these methods all have inherent defects caused by the process. For example, the physical imprint method is not easy to be uniform due to the imprinting force, so it is easy to affect the precision and size of the microstructure, and the imprinted microstructure mostly has a folded-angle structure (such as a sawtooth, a right angle or a trapezoidal structure), and the existence of the chamfer will The conductive layer is more susceptible to stress concentration and is accelerated to break or difficult to form a continuous conductive layer; and the chemical etching method mentioned in U.S. Patent No. 6,036,579, wherein the etching liquid used is expensive and causes environmental pollution, and the etched microstructure is also Most of them have a folding angle, so there are also the same problems as physical imprinting.
基於前述之缺點,工業界上亟需開發出一種無需化學蝕刻液,不易產生具有銳角之微結構,且同時可使導電層與基底材間之黏著性更為提升的技術,以克服前述種種習知技術的問題。Based on the aforementioned shortcomings, there is an urgent need in the industry to develop a technique that does not require a chemical etching solution, is not easy to produce a microstructure having an acute angle, and at the same time, can improve the adhesion between the conductive layer and the substrate, thereby overcoming the above-mentioned various habits. Know the technical problems.
因此,本發明之目的,在提供一種可以防止透明導電層在外力下產生破裂或自基底材剝離,無需化學蝕刻液且製造簡單的導電基材製備方法。Accordingly, an object of the present invention is to provide a method for producing a conductive substrate which can prevent cracking of a transparent conductive layer under external force or peeling from a substrate without requiring a chemical etching solution and which is simple to manufacture.
於是,根據本發明所揭示之一種製造透明導電基材的方法,包含:在一基底材上形成一未固化之光固化材料層,該未固化之光固化材料層係由一可光固化組成物所構成,該可光固化組成物包含至少一種具有複數個反應性官能基之可光固化預聚物,且該可光固化預聚物具有70-700g/mol之官能基當量;提供一圖案化遮蔽層,以局部地遮蔽該未固化之光固化材料層表面,使得該未固化之光固化材料層形成至少一個遮蔽區及至少一個非遮蔽區;使一第一光源通過該圖案化遮蔽層,使得該未固化之光固化材料層中之非遮蔽區的可光固化預聚物產生固化反應,藉以使該未固化之光固化材料層形成一部分區域固化之光固化材料層,其上具有至少一個凸狀固化區與至少一個凹狀未固化區;移除該圖案化遮蔽層;以一第二光源照射,以進一步固化該部分區域固化之光固化材料層,使該部分區域固化之光固化材料層之凹狀未固化區產生固化反應,藉此形成一具有凹凸微結構表面之結構化的光固化材料層;及在該結構化的光固化材料層的微結構表面上形成一導電層。Thus, a method of fabricating a transparent conductive substrate according to the present invention comprises: forming an uncured photocurable material layer on a substrate, the uncured photocurable material layer being a photocurable composition The photocurable composition comprises at least one photocurable prepolymer having a plurality of reactive functional groups, and the photocurable prepolymer has a functional group equivalent weight of 70 to 700 g/mol; providing a patterning Masking layer to partially shield the surface of the uncured photocurable material layer such that the uncured photocurable material layer forms at least one shielding region and at least one non-shadowing region; and a first light source passes through the patterned shielding layer, The photocurable prepolymer of the non-masking region in the uncured photocurable material layer is subjected to a curing reaction, whereby the uncured photocurable material layer forms a portion of the region-cured photocurable material layer having at least one thereon a convex solidified region and at least one concave uncured region; removing the patterned shielding layer; irradiating with a second light source to further cure the solidified light solidification of the partial region a material layer that causes a curing reaction to form a concave uncured region of the partially cured photocurable material layer, thereby forming a structured photocurable material layer having a textured surface; and the structured photocurable material A conductive layer is formed on the microstructured surface of the layer.
本發明之功效在於:利用該結構化的光固化材料層的微結構表面,使得導電層表面形成凹凸微結構,藉此而可以增加導電層與基底材的結合強度及導電層本身的結構強度,從而加強防止透明導電層在外力下產生破裂或自基底材剝離。The effect of the invention is that the microstructure surface of the structured photocurable material layer is used to form a concave-convex microstructure on the surface of the conductive layer, thereby increasing the bonding strength between the conductive layer and the substrate and the structural strength of the conductive layer itself. Thereby, it is possible to enhance the prevention of cracking of the transparent conductive layer under external force or peeling from the substrate.
有關本發明之前述及其他技術內容、特點與功效,在以下配合參考圖式之較佳實施例的詳細說明中,將可清楚的呈現。The foregoing and other objects, features, and advantages of the invention are set forth in the <RTIgt;
在本發明被詳細描述之前,要注意的是,在以下的說明內容中,類似的元件是以相同的編號來表示。Before the present invention is described in detail, it is noted that in the following description, similar elements are denoted by the same reference numerals.
參閱圖1至圖6,本發明一種製造透明導電基材的方法的一較佳實施例包含:Referring to FIGS. 1 through 6, a preferred embodiment of a method of fabricating a transparent conductive substrate of the present invention comprises:
(a) 將一可光固化漿料塗佈在一透明基底材21上以形成一可光固化漿料層,該可光固化漿料具有一可光固化組成物及一溶劑,該可光固化組成物包含一光起始劑及至少一種具有複數個反應性官能基之可光固化預聚物,且該可光固化預聚物具有70-700克/莫耳(g/mol)之官能基當量,該可光固化預聚物可為單體或寡聚合物;(a) applying a photocurable paste to a transparent substrate 21 to form a photocurable paste having a photocurable composition and a solvent, which is photocurable The composition comprises a photoinitiator and at least one photocurable prepolymer having a plurality of reactive functional groups, and the photocurable prepolymer has a functional group of 70-700 g/mole (g/mol) Equivalent, the photocurable prepolymer may be a monomer or an oligopolymer;
(b) 乾燥該可光固化漿料層,以除去該可光固化漿料中的溶劑,使得在該基底材21上形成一具有可光固化預聚物的未固化之光固化材料層22a(如圖1),該反應性官能基可受自由基引發而產生交聯反應;(b) drying the photocurable paste layer to remove the solvent in the photocurable paste such that an uncured photocurable material layer 22a having a photocurable prepolymer is formed on the substrate 21 ( As shown in Figure 1), the reactive functional group can be initiated by a free radical to produce a crosslinking reaction;
(c)提供一圖案化遮蔽層31,以局部地遮蔽該未固化之光固化材料層22a(如圖2),使得該未固化之光固化材料層22a形成至少一個遮蔽區222及至少一個非遮蔽區221;(c) providing a patterned masking layer 31 to partially shield the uncured photocurable material layer 22a (as in FIG. 2) such that the uncured photocurable material layer 22a forms at least one masking region 222 and at least one non- Shading area 221;
(d)使一第一光源(L1)通過該圖案化遮蔽層31,使得該未固化之光固化材料層22a中之非遮蔽區221的可光固化預聚物產生固化反應。上述固化反應是藉由光起始劑裂解產生自由基並因此引發該未固化之光固化材料層22a之非遮蔽區221的光可固化官能基預聚物產生聚合反應,並因此造成非遮蔽區221的可光固化組成物濃度下降,如此使得該未固化之光固化材料層22a之遮蔽區222中的可光固化組成物朝該非遮蔽區221流動,進而使得該未固化之光固化材料層22a形成一具有一凸狀固化區223與一凹狀未固化區224的部分區域固化之光固化材料層22b(如圖3);and (d) a first light source (L 1) through the patterned masking layer 31, such that the uncured photocurable material layer 22a in the non-masked regions 221 may generate a photocurable prepolymer curing reaction. The above curing reaction is a photocurable functional prepolymer which is generated by cleavage of a photoinitiator to generate a radical and thereby initiates the non-masking region 221 of the uncured photocurable material layer 22a, and thus causes a non-masking region. The concentration of the photocurable composition of 221 is decreased such that the photocurable composition in the masking region 222 of the uncured photocurable material layer 22a flows toward the non-masking region 221, thereby causing the uncured photocurable material layer 22a. Forming a partially cured photocurable material layer 22b having a convex solidified region 223 and a concave uncured region 224 (Fig. 3);
(e)移除該圖案化遮蔽層31(如圖4);(e) removing the patterned shielding layer 31 (as shown in Figure 4);
(f)使用一第二光源(L2),照射該部分區域固化之光固化材料層22b(如圖4),使該部分區域固化之光固化材料22b之該凹狀未固化區224固化而形成一凹狀固化區225,並因此而在該基底材21上形成一具有一凹凸微結構化表面220的結構化的光固化材料層22(如圖5);以及(f) using a second light source (L 2 ) to illuminate the partially cured photocurable material layer 22b (Fig. 4) to cure the concave uncured region 224 of the partially cured photocurable material 22b. Forming a concave solidified region 225, and thus forming a structured photocurable material layer 22 having a textured microstructured surface 220 on the substrate 21 (FIG. 5);
(g)以濺鍍或蒸鍍方式在該結構化的光固化材料層22上形成一透明導電層23(如圖6)。(g) Forming a transparent conductive layer 23 on the structured photocurable material layer 22 by sputtering or evaporation (Fig. 6).
該圖案化遮蔽層31具有交替排列的透光區域311與非透光區域312,每兩相鄰透光區域311具有一50μm~250μm的間距(d)。該圖案化遮蔽層31之可透光區域311為用以使該第一光源透過,而該非透光區域312為用以阻擋、吸收或反射光源。The patterned shielding layer 31 has alternating light-transmissive regions 311 and non-transmissive regions 312, and each of the two adjacent light-transmitting regions 311 has a pitch (d) of 50 μm to 250 μm. The permeable region 311 of the patterned shielding layer 31 is for transmitting the first light source, and the non-transmissive region 312 is for blocking, absorbing or reflecting the light source.
可用於做為本發明可光固化預聚物的材料,包含但並不僅限於具有多元醇之丙烯酸或丙烯酸酯的官能性丙烯酸樹脂預聚物、多元醇及丙烯酸或甲基丙烯的羥基烷酯等所合成的官能性胺基甲酸丙烯酸樹脂預聚物、及其組合。較佳下,該預聚物材料為丙烯酸酯樹脂。Materials which can be used as the photocurable prepolymer of the present invention include, but are not limited to, functional acrylic resin prepolymers of acrylic acid or acrylate having a polyol, polyols, and hydroxyalkyl esters of acrylic acid or methacrylic acid. Synthetic functional urethane acrylic acid resin prepolymers, and combinations thereof. Preferably, the prepolymer material is an acrylate resin.
較佳下,該預聚物具有一70~700克/莫耳(g/mol)之官能基當量。預聚物之官能基當量定義如下:Preferably, the prepolymer has a functional group equivalent weight of from 70 to 700 grams per mole (g/mol). The functional group equivalents of the prepolymer are defined as follows:
更佳下,該預聚物之官能基當量為80~600克/莫耳(g/mol),最佳為85~400克/莫耳(g/mol)。該預聚物的光固化反應原理及結構化的光固化材料層22的形成將如下更進一步描述。具有可進行光固化反應的官能基的材料,稱為光固化材料。將光固化材料與光起始劑混合,以塗佈方式形成光固化材料層,再對此層進行紫外光的照射,紫外光會將光起始劑裂解成自由基(free radical),自由基引發光固化材料的官能基產生反應,隨著反應的進行,光固化材料層的分子量與黏度會持續上升,直到光固化材料層的黏度過大,中止光固化反應,而形成乾爽的表面。光固化材料層中的固化區,由於產生光固化反應,需要更多尚未反應的光固化材料來進行光固化反應,因此尚未反應的光固化材料,會由未固化區,往固化區進行流動,以提供尚未反應的光固化材料,使固化區內的光固化反應能持續進行。尚未反應的光固化材料,由未固化區往固化區的流動現象,使光固化材料層的固化區變得較厚,而呈現隆起的山峰狀;同時也使光固化材料層的未固化區變得較薄,而呈現凹陷的山谷狀,使得固化區與未固化區之間出現了厚度上的差異,形成山峰與山谷交替出現的表面微結構。當光固化材料的分子量愈小,尚未反應的光固化材料在光固化材料層中的流動速率愈快,尚未反應的光固化材料能較快由未固化區流動至固化區,使未固化區與固化區之間的Rz值較高,也代表所形成的表面微結構會更為明顯。當光固化材料的官能基數目愈大,光固化材料在進行光固化反應時,其反應程度會更為激烈,使得尚未反應的光固化材料會較快由未固化區流動至固化區,以維持光固化反應之進行,這使未固化區與固化區之間的Rz值較高,也代表所形成的表面微結構會更為明顯。More preferably, the prepolymer has a functional group equivalent weight of from 80 to 600 g/mole (g/mol), most preferably from 85 to 400 g/mole (g/mol). The photocuring reaction principle of the prepolymer and the formation of the structured photocurable material layer 22 will be further described below. A material having a functional group capable of undergoing a photocuring reaction is referred to as a photocurable material. The photocurable material is mixed with a photoinitiator to form a photocurable material layer by coating, and then the layer is irradiated with ultraviolet light, and the ultraviolet light will cleave the photoinitiator into free radicals, free radicals. The functional group of the photocurable material is initiated to react. As the reaction proceeds, the molecular weight and viscosity of the photocurable material layer continue to rise until the viscosity of the photocurable material layer is too large to stop the photocuring reaction and form a dry surface. The curing zone in the photocurable material layer requires more unreacted photocurable material to perform photocuring reaction due to the photocuring reaction, so that the unreacted photocurable material flows from the uncured zone to the curing zone. In order to provide a photocurable material that has not been reacted, the photocuring reaction in the curing zone can be continued. The unreacted photocurable material, the flow phenomenon from the uncured zone to the solidified zone, makes the solidified zone of the photocurable material layer thicker, and presents a ridged mountain shape; at the same time, the uncured zone of the photocurable material layer is also changed. It is thinner and presents a valley shape with a depression, so that a difference in thickness occurs between the solidified zone and the uncured zone, forming a surface microstructure alternately between the mountain and the valley. When the molecular weight of the photocurable material is smaller, the flow rate of the unreacted photocurable material in the photocurable material layer is faster, and the unreacted photocurable material can flow from the uncured region to the solidified region faster, so that the uncured region and the uncured region The higher Rz values between the solidification zones also represent a more pronounced surface microstructure. When the number of functional groups of the photocurable material is larger, the degree of reaction of the photocurable material in the photocuring reaction is more intense, so that the unreacted photocurable material flows from the uncured zone to the solidification zone faster to maintain The photocuring reaction proceeds, which results in a higher Rz value between the uncured zone and the cured zone, and also represents a more pronounced surface microstructure.
這裡須注意的是,在步驟(c)與(e)中的光固化材料的固化程度可以是完全固化或是部份地固化,只要可使得光固化材料不再具有流動性即可,本發明中並無特別的限制。It should be noted here that the degree of curing of the photocurable material in steps (c) and (e) may be fully cured or partially cured as long as the photocurable material can no longer have fluidity, the present invention There are no special restrictions.
可應用於本發明中之溶劑無特別限制,只要能使可光固化材料充分溶解之溶劑皆可使用,可擇自醇類、酮類、酯類、鹵化溶劑、烴類等,例如:丙酮、乙腈、氯仿、氯苯酚、環己烷、環己酮、環戊酮、二氯甲烷、乙酸二乙酯、碳酸二甲酯、乙醇、乙酸乙酯、N,N-二甲基乙醯胺、1,2-丙二醇、2-己酮、甲醇、乙酸甲酯、乙酸丁酯、甲苯及四氫呋喃、及其等組合所構成之群組。The solvent to be used in the present invention is not particularly limited as long as the solvent capable of sufficiently dissolving the photocurable material can be used, and may be selected from alcohols, ketones, esters, halogenated solvents, hydrocarbons, etc., for example, acetone. Acetonitrile, chloroform, chlorophenol, cyclohexane, cyclohexanone, cyclopentanone, dichloromethane, diethyl acetate, dimethyl carbonate, ethanol, ethyl acetate, N,N-dimethylacetamide, A group consisting of 1,2-propanediol, 2-hexanone, methanol, methyl acetate, butyl acetate, toluene, tetrahydrofuran, and the like.
可應用於本發明中之光起始劑並無特別限制,主要能使可光固化樹脂進行光固化反應者皆可使用,可擇自乙烯基苯酮類、二苯甲酮衍生物、米希勒酮、苯炔、苯甲基衍生物、苯偶姻衍生物、苯偶姻甲醚類、α-醯氧基酯、噻噸酮類及蒽醌類、及其等組合所構成之群組。該起始劑之使用量也並無限制,較佳使用量為不低於0.01wt%(以可光固化漿料組成為100wt%時)。The photoinitiator which can be used in the present invention is not particularly limited, and can be used mainly for photocuring of a photocurable resin, and can be selected from vinyl benzophenones, benzophenone derivatives, and Mich. a group consisting of ketones, benzynes, benzyl derivatives, benzoin derivatives, benzoin methyl ethers, α-methoxy esters, thioxanthones and anthraquinones, and combinations thereof . The amount of the initiator to be used is also not limited, and is preferably used in an amount of not less than 0.01% by weight (when the photocurable paste composition is 100% by weight).
較佳下,該可光固化漿料具有一10~80wt%的固含量,若固含量低於10wt%,照射紫外光不易形成凹凸微結構,若固含量大於80wt%則不易進行塗佈,且照射紫外光後光固化材料層易脆裂。更佳下,該可光固化漿料的固含量為15~60wt%,最佳為20~40wt%。Preferably, the photocurable paste has a solid content of 10 to 80% by weight. If the solid content is less than 10% by weight, the ultraviolet light is less likely to form a concave-convex microstructure, and if the solid content is more than 80% by weight, coating is difficult. The layer of photocurable material is easily brittle after exposure to ultraviolet light. More preferably, the photocurable paste has a solid content of 15 to 60% by weight, preferably 20 to 40% by weight.
較佳下,該導電層23的材料為金屬或金屬化合物,該金屬係擇自一由金、銀、鉑、鉛、銅、鋁、鎳、鉻、鈦、鐵、鈷及錫、及其等組合的合金所構成之群組,該金屬化合物係擇自一由氧化銦、氧化錫、氧化鈦、氧化鋁、氧化鋅、氧化鎵及氧化銦錫、及其等組合所構成之群組。更佳下,該金屬化合物為氧化銦錫。Preferably, the material of the conductive layer 23 is a metal or a metal compound selected from the group consisting of gold, silver, platinum, lead, copper, aluminum, nickel, chromium, titanium, iron, cobalt and tin, and the like. A group consisting of a combination of alloys selected from the group consisting of indium oxide, tin oxide, titanium oxide, aluminum oxide, zinc oxide, gallium oxide, and indium tin oxide, and combinations thereof. More preferably, the metal compound is indium tin oxide.
該基底材21可為透明絕緣材料。較佳下,該基底材21的材料為聚合物,該聚合物係擇自一由聚酯系樹脂、聚醚系樹脂、聚碳酸酯系樹脂、聚醯胺系樹脂、聚醯亞胺系樹脂、聚烯烴系樹脂、丙烯酸酯系樹脂、聚氯乙烯系樹脂、聚苯乙烯系樹脂、聚乙烯醇系樹脂、聚芳酯系樹脂、聚苯硫系樹脂、聚二氯亞乙烯系樹脂、甲基丙烯酸酯系樹脂、醋酸纖維素(cellulose acetate)、二醋酸纖維素(diacetyl cellulose)及三醋酸纖維素(triacetyl cellulose)、及其等組合所構成之群組。更佳下,該透明基底材的材料聚對苯二甲酸乙二酯。The base material 21 may be a transparent insulating material. Preferably, the material of the base material 21 is a polymer selected from the group consisting of a polyester resin, a polyether resin, a polycarbonate resin, a polyamide resin, and a polyimide resin. , polyolefin resin, acrylate resin, polyvinyl chloride resin, polystyrene resin, polyvinyl alcohol resin, polyarylate resin, polyphenylene sulfide resin, polydivinylidene resin, A A group consisting of a acrylate resin, a cellulose acetate, a diacetyl cellulose, a triacetyl cellulose, and the like. More preferably, the material of the transparent substrate is polyethylene terephthalate.
該基底材21的厚度雖然並無特別加以限制,但是較佳為在2~300μm的範圍,更佳為在10~130μm的範圍。厚度未達2μm時,作為基底材之機械強度會有不足之虞,使得連續形成透明導電層的作業會變得難以進行。又,若厚度超過300μm時,則捲繞性容易產生問題,透明導電層之捲繞加工會有難以進行之虞。Although the thickness of the base material 21 is not particularly limited, it is preferably in the range of 2 to 300 μm, more preferably in the range of 10 to 130 μm. When the thickness is less than 2 μm, the mechanical strength of the base material may be insufficient, so that the operation of continuously forming the transparent conductive layer may become difficult. Moreover, when the thickness exceeds 300 μm, the winding property is likely to cause a problem, and the winding process of the transparent conductive layer may be difficult.
本發明之導電基材,可使用於觸控面板及顯示器等各種裝置的形成。尤其較佳可使用作為觸控面板用電極板。The conductive substrate of the present invention can be used for the formation of various devices such as touch panels and displays. It is particularly preferable to use it as an electrode plate for a touch panel.
較佳下,光照該未固化之光固化材料層22a的步驟中所使用的第一光源可為紫外光、可見光、電子束或X-射線,更佳為使用紫外光來實現,且其紫外光照射劑量不低於70mJ/cm2,較佳為70~4000 mJ/cm2,照射劑量低於70 mJ/cm2則不易形成微結構,照射劑量高於4000 mJ/cm2則易使基底材21變形。更佳下,照射劑量為100~3500 mJ/cm2,最佳為400~1500mJ/cm2。另外,前述之第二光源亦可為紫外光、可見光、電子束或X-射線,更佳為使用紫外光來實現。於本發明中第二光源之照射劑量,並無特別地限制,只要是可使未固化之光固化材料層22a固化者,皆可被應用於本發明中。此外,第一光源與第二光源可為相同或不同。Preferably, the first light source used in the step of illuminating the uncured photocurable material layer 22a may be ultraviolet light, visible light, electron beam or X-ray, more preferably realized by using ultraviolet light, and ultraviolet light thereof. The irradiation dose is not less than 70 mJ/cm 2 , preferably 70 to 4000 mJ/cm 2 , and the irradiation dose is less than 70 mJ/cm 2 , the microstructure is not easily formed, and the irradiation dose is higher than 4000 mJ/cm 2 to facilitate the substrate. 21 deformation. More preferably, the irradiation dose is 100 to 3500 mJ/cm 2 , and most preferably 400 to 1500 mJ/cm 2 . In addition, the foregoing second light source may also be ultraviolet light, visible light, electron beam or X-ray, and more preferably realized by using ultraviolet light. The irradiation dose of the second light source in the present invention is not particularly limited as long as it can cure the uncured photocurable material layer 22a, and can be applied to the present invention. Furthermore, the first light source and the second light source may be the same or different.
參閱圖6,為根據本發明方法所製得之透明導電基材的一較佳實施例,包含:一基底材21;一結構化的光固化材料層22,形成在該基底材21上,且具有一凹凸微結構化表面220;及一導電層23形成在該結構化的光固化材料層22的凹凸微結構化表面220上。該導電層23具有一與該凹凸微結構化表面220形狀實質上相同的上表面230,該上表面230具有一Rz為0.5μm~3.5μm且Sm為0.05mm~0.35mm的表面粗糙度。Rz值之定義為厚度較厚區(凸區)與厚度較薄區(凹區)之間的厚度差距值之十點平均值(ten-point mean roughness),Sm為相鄰凸區或凹區的平均間距(mean spacing)。Rz與Sm可利用探針式表面分析儀(日本KOSAKA製,型號ET-4000A)進行測試。Referring to FIG. 6, a preferred embodiment of a transparent conductive substrate prepared by the method of the present invention comprises: a substrate 21; a structured photocurable material layer 22 formed on the substrate 21, and A concave-convex microstructured surface 220 is formed; and a conductive layer 23 is formed on the textured microstructured surface 220 of the structured photocurable material layer 22. The conductive layer 23 has an upper surface 230 having substantially the same shape as the uneven microstructured surface 220, and the upper surface 230 has a surface roughness of Rz of 0.5 μm to 3.5 μm and Sm of 0.05 mm to 0.35 mm. The Rz value is defined as the ten-point mean roughness between the thicker thickness region (convex region) and the thinner thickness region (the concave region), and Sm is the adjacent convex region or concave region. Mean spacing. Rz and Sm can be tested using a probe type surface analyzer (manufactured by KOSAKA, Japan, model ET-4000A).
較佳下,該導電層23具有一10nm~300nm的厚度,更佳為10~200nm。厚度若薄於10nm時,則難以成為表面電阻為103 Ω/□以下之具有良好導電性的連續層,若過厚則容易導致透明性的降低等。Preferably, the conductive layer 23 has a thickness of 10 nm to 300 nm, more preferably 10 to 200 nm. When the thickness is thinner than 10 nm, it is difficult to form a continuous layer having a good electrical conductivity of 10 3 Ω/□ or less, and if it is too thick, the transparency is likely to be lowered.
根據本發明所製得之導電基材具有一凹凸微結構化表面,若將此導電基材應用於觸控面板等領域,相較表面平坦之導電基材,因其與另一電極之接觸面積較小,可減少沾黏問題及因觸控筆觸壓劃線對該導電層所造成之拉扯,而使得該導電層破裂,甚至進一步與基底材剝離。另外,本發明所製得之凹凸結構為一波浪狀之微結構,相較於具有折角狀結構(如鋸齒、直角或梯形結構)之導電基材,可減少因外力觸壓使得應力集中於該折角,而使該導電層破裂,造成表面電阻上升之問題。The conductive substrate prepared according to the present invention has a concave-convex microstructured surface. If the conductive substrate is applied to a touch panel or the like, the conductive substrate is flat compared to the surface of the conductive substrate. Smaller, it can reduce the sticking problem and the pulling of the conductive layer by the stylus stroke, so that the conductive layer is broken and even further peeled off from the substrate. In addition, the concave-convex structure obtained by the invention is a wavy microstructure, and the conductive substrate having a folded-angle structure (such as a sawtooth, a right angle or a trapezoidal structure) can reduce stress caused by external force and concentrate on the The angle of the corner causes the conductive layer to rupture, causing a problem of an increase in surface resistance.
以下將以實施例來說明本發明各目的之實施方式與功效。須注意的是,該實施例僅為例示說明之用,而不應被解釋為本發明實施之限制。The embodiments and effects of each object of the present invention will be described below by way of examples. It should be noted that the examples are for illustrative purposes only and are not to be construed as limiting the invention.
導電基材製備Conductive substrate preparation
將0.2g具反應性官能基之可光固化預聚物(Sartomer,型號SR444,丙烯酸酯系,官能基當量為99.3 g/mol),加入甲苯0.8g(Toluene)及光起始劑0.02g(美國Ciba,I-184),以配製成固含量為20wt%的可光固化漿料(1.02g)。0.2 g of a photocurable prepolymer having a reactive functional group (Sartomer, model SR444, acrylate system, functional group equivalent: 99.3 g/mol), adding toluene 0.8 g (Toluene) and photoinitiator 0.02 g ( Ciba, I-184, USA, to prepare a photocurable paste (1.02 g) having a solids content of 20% by weight.
將所配製出的可光固化漿料1.02g,滴於聚酯系基底材上(日本Toyobo,型號A4300,5cm×5cm×100μm),以旋轉塗佈法(Spin Coating,1000rpm,40秒)將漿料均勻展平,置於恆溫80℃的烘箱內,烘烤3分鐘除去溶劑,再移至恆溫100℃的烘箱內,烘烤2分鐘以進行熱處理,最後回復至室溫,形成基底材上方的未固化之光固化材料層。1.02 g of the prepared photocurable slurry was dropped on a polyester base material (Toyobo, Japan, model A4300, 5 cm × 5 cm × 100 μm), and spin coating (1000 rpm, 40 seconds) The slurry was evenly flattened, placed in an oven at a constant temperature of 80 ° C, baked for 3 minutes to remove the solvent, then transferred to an oven at a constant temperature of 100 ° C, baked for 2 minutes for heat treatment, and finally returned to room temperature to form a substrate. A layer of uncured photocurable material.
將線寬50μm,線距50μm的圖案化遮蔽層(光罩)置於塗有未固化之光固化材料層的基底材之上方。A patterned masking layer (photomask) having a line width of 50 μm and a line spacing of 50 μm was placed over the substrate material coated with the uncured photocurable material layer.
使用紫外曝光機(美國Fusion),在氮氣環境下,以紫外光照射塗有未固化之光固化材料層的基底材,照射劑量為520(mJ/cm2),以形成一部分區域固化之光固化材料層。Using a UV exposure machine (Fusion, USA), the substrate coated with the uncured photocurable material layer was irradiated with ultraviolet light under a nitrogen atmosphere at an irradiation dose of 520 (mJ/cm 2 ) to form a partially cured photocuring layer. Material layer.
將光罩移開,在氮氣環境下,再以紫外光直接照射塗有部分區域固化之光固化材料層的基底材,照射劑量為450(mJ/cm2)。該部分區域固化之光固化材料層經過照射後形成一具有凹凸微結構表面的結構化的光固化材料層。The photomask was removed, and the substrate coated with the partially cured photocurable material layer was directly irradiated with ultraviolet light under a nitrogen atmosphere at an irradiation dose of 450 (mJ/cm 2 ). The partially cured photocurable material layer is irradiated to form a structured photocurable material layer having a textured surface.
將具有結構化的光固化材料層之基底材放置於磁控濺鍍腔體中,以Sn/In+Sn=10wt%之ITO為靶材,腔體真空度抽到3×10-6torr後,通入濺鍍氣體Ar及O2於腔體中,O2/Ar=0.02,工作壓力為5×10-4torr,功率為4KW,基底材溫度為室溫,以在結構化的光固化材料層上形成一厚度為30nm之ITO導電層。The substrate material having the structured photocurable material layer is placed in the magnetron sputtering chamber, and the Sn/In+Sn=10 wt% ITO is used as the target, and the cavity vacuum is drawn to 3×10 -6 torr. , through the sputtering gas Ar and O 2 in the cavity, O 2 /Ar=0.02, working pressure 5×10 -4 torr, power 4KW, substrate temperature is room temperature, in structured photocuring An ITO conductive layer having a thickness of 30 nm was formed on the material layer.
導電基材的表面粗糙度測試:以探針式表面分析儀(日本KOSAKA製,型號ET-4000A)測得實施例1的導電基材的Ra值為0.21μm,Rz值為0.73μm,及Sm值為0.099mm。Ra為中心線平均粗糙度(center line average roughness),Rz為十點平均粗糙度(ten-point mean roughness),及Sm為平均間距(mean spacing)。Surface roughness test of the conductive substrate: The conductive substrate of Example 1 was measured by a probe type surface analyzer (manufactured by KOSAKA, Japan, model ET-4000A) to have an Ra value of 0.21 μm, an Rz value of 0.73 μm, and Sm. The value is 0.099 mm. Ra is a center line average roughness, Rz is a ten-point mean roughness, and Sm is a mean spacing.
導電基材的耐筆劃測試:將導電基材與表面具有間隔物之導電玻璃貼合,以其等的ITO層彼此對向的方式貼合,使用一耐磨測試機(又升科技,型號SDT-009),在導電基材之另一面(不導電面),以R0.8甲醛樹脂筆來回劃線10萬次(來回算一次),劃線長度2cm,荷重250g。 Stroke resistance test of conductive substrate: the conductive substrate is bonded to the conductive glass with spacers on the surface, and the ITO layers are aligned with each other, and a wear-resistant tester is used (again, technology, model SDT) -009), on the other side of the conductive substrate (non-conductive surface), with a R0.8 formaldehyde resin pen back and forth lined 100,000 times (counting back and forth), the length of the scribe line is 2 cm, and the load is 250 g.
導電基材的表面電阻量測:使用三菱油化(股)製Lotest AMCP-T400電阻量測器,根據JIS-K7194為基準以4端子法測定,測量耐筆劃測試之前與之後的導電基材的表面電阻,耐筆劃測試前電阻為Ro,耐筆劃測試後電阻為R,並計算R/Ro電阻變化比值,電阻變化比值愈趨近1代表導電基材的結構愈穩定,透明導電層愈不容易因外力產生裂縫或剝離。導電基材的表面電阻變化比值結果如表1所示。 Surface resistance measurement of conductive substrate : Using a Mitsubishi oil-based (stock) Lotest AMCP-T400 resistance measuring device, measured by a 4-terminal method based on JIS-K7194, measuring the conductive substrate before and after the scratch resistance test Surface resistance, the resistance before the stroke test is Ro, the resistance after the stroke test is R, and the R/Ro resistance change ratio is calculated. The resistance change ratio is closer to 1 and the structure of the conductive substrate is more stable, and the transparent conductive layer is less easy. Cracks or peeling due to external forces. The results of the surface resistance change ratio of the conductive substrate are shown in Table 1.
除了紫外光照射塗有未固化之光固化材料層的基底材的第一次照射劑量不同以外,實施例2-4的導電基材製備的其他條件與實施例1者相同。實施例2-4的照射劑量、光罩的線寬與線距、導電基材的表面粗糙度與表面電阻變化比值結果如表1所示。The other conditions for the preparation of the conductive substrate of Example 2-4 were the same as those of Example 1 except that the first irradiation dose of the base material coated with the uncured photocurable material layer was different by ultraviolet light irradiation. The results of the irradiation dose of Example 2-4, the line width and the line pitch of the reticle, the surface roughness of the conductive substrate, and the surface resistance change ratio are shown in Table 1.
從實施例1-4的表面電阻變化比值(R/Ro)的結果可以看出當Rz低於0.73μm或高於2.82μm時,表面電阻變化比值有漸增的驅勢,顯示Rz的較佳範圍為0.73~2.82μm。導電基材在觸控面板的應用上的要求一般為R/Ro≦1.3。惟表面電阻變化比值可根據不同的應用而有不同的要求。From the results of the surface resistance change ratio (R/Ro) of Examples 1-4, it can be seen that when Rz is lower than 0.73 μm or higher than 2.82 μm, the surface resistance change ratio has an increasing driving force, indicating that Rz is better. The range is from 0.73 to 2.82 μm. The requirements of the conductive substrate in the application of the touch panel are generally R/Ro≦1.3. However, the surface resistance change ratio can have different requirements depending on the application.
除了紫外光照射塗有未固化之光固化材料層的基底材的第一次照射劑量及光罩的線寬與線距不同以外,實施例5-7的導電基材製備的其他條件與實施例1者相同。實施例5-7的照射劑量、光罩的線寬與線距、導電基材的表面粗糙度與表面電阻變化比值結果如表2所示。Other conditions and examples of preparation of the conductive substrate of Examples 5-7 except that the first irradiation dose of the substrate coated with the uncured photocurable material layer and the line width and the line pitch of the reticle were different. 1 is the same. The results of the irradiation doses of Examples 5-7, the line width and the line pitch of the reticle, the surface roughness of the conductive substrate, and the surface resistance change ratio are shown in Table 2.
從實施例2及5-7的表面電阻變化比值(R/Ro)的結果可以看出當Sm低於0.1mm或高於0.22mm時,表面電阻變化比值有漸增的驅勢,顯示Sm的較佳範圍為0.1~0.22mm。From the results of the surface resistance change ratio (R/Ro) of Examples 2 and 5-7, it can be seen that when Sm is less than 0.1 mm or higher than 0.22 mm, the surface resistance change ratio has an increasing driving force, indicating Sm. The preferred range is from 0.1 to 0.22 mm.
比較例1的導電基材的製備是直接將透明基底材放置於磁控濺鍍腔體中,以Sn/In+Sn=10wt%之ITO為靶材,腔體真空度抽到3×10-6torr後,通入濺鍍氣體Ar及O2於腔體中,O2/Ar=0.02,工作壓力為5×10-4torr,功率為4KW,基底材溫度為室溫,以在基底材上形成一厚度為30nm之ITO導電層。比較例1的導電基材的表面粗糙度與表面電阻變化比值結果如表2所示。The conductive substrate of Comparative Example 1 was prepared by directly placing the transparent substrate in a magnetron sputtering chamber, and using Sn/In+Sn=10 wt% of ITO as a target, and the cavity vacuum was pumped to 3×10 − After 6 torr, the sputtering gas Ar and O 2 are introduced into the cavity, O 2 /Ar=0.02, the working pressure is 5×10 -4 torr, the power is 4KW, and the substrate temperature is room temperature to be used in the substrate. An ITO conductive layer having a thickness of 30 nm was formed thereon. The results of the surface roughness and surface resistance change ratio of the conductive substrate of Comparative Example 1 are shown in Table 2.
從表1及表2的實驗結果可以看出具有結構化的光固化材料層22的導電基材(實施例1-7)比沒有結構化的光固化材料層22的導電基材(比較例1)具有較趨近於1的表面電阻變化比值,此結果也進一步說明本發明利用結構化的光固化材料層22而可以加強透明導電層與基底材的結合強度及導電層本身的結構強度,從而加強防止透明導電層在外力下產生裂縫或自基底材剝離。From the experimental results of Tables 1 and 2, it can be seen that the conductive substrate having the structured photocurable material layer 22 (Examples 1-7) is more conductive than the conductive substrate without the structured photocurable material layer 22 (Comparative Example 1) ) having a surface resistance change ratio closer to 1, which further demonstrates that the present invention utilizes the structured photocurable material layer 22 to enhance the bonding strength of the transparent conductive layer to the substrate and the structural strength of the conductive layer itself, thereby Strengthening prevents the transparent conductive layer from cracking or peeling off from the substrate under external force.
惟以上所述者,僅為本發明之較佳實施例而已,當不能以此限定本發明實施之範圍,即大凡依本發明申請專利範圍及發明說明內容所作之簡單的等效變化與修飾,皆仍屬本發明專利涵蓋之範圍內。The above is only the preferred embodiment of the present invention, and the scope of the invention is not limited thereto, that is, the simple equivalent changes and modifications made by the scope of the invention and the description of the invention are All remain within the scope of the invention patent.
21...基底材twenty one. . . Base material
22...結構化的光固化材料層twenty two. . . Structured layer of photocurable material
22a...未固化之光固化材料層22a. . . Uncured photocurable material layer
22b...部分區域固化之光固化材料層22b. . . Partially cured photocurable material layer
220...凹凸微結構化表面220. . . Concave microstructured surface
221...非遮蔽區221. . . Unmasked area
222...遮蔽區222. . . Shading area
223...凸狀固化區223. . . Convex solidification zone
224...凹狀未固化區224. . . Concave uncured zone
225...凹狀固化區225. . . Concave solidification zone
23...透明導電層twenty three. . . Transparent conductive layer
230...上表面230. . . Upper surface
31...圖案化遮蔽層31. . . Patterned masking layer
311...透光區域311. . . Light transmissive area
312...非透光區域312. . . Non-transparent area
L1...第一光源L 1 . . . First light source
L2...第二光源L 2 . . . Second light source
d...間距d. . . spacing
圖1是一側視示意圖,說明本發明一較佳實施例之在一基材上形成一未固化之光固化材料層的步驟;1 is a side elevational view showing a step of forming an uncured photocurable material layer on a substrate according to a preferred embodiment of the present invention;
圖2是一側視示意圖,說明本發明一較佳實施例之使用一光罩以圖案化地遮蔽該未固化之光固化材料層的步驟;2 is a side elevational view showing a step of patterning the uncured photocurable material layer using a photomask according to a preferred embodiment of the present invention;
圖3是一側視示意圖,說明本發明一較佳實施例之經圖案化地曝光該未固化的光固化材料層之後所形成的部分區域固化之光固化材料層;3 is a side elevational view showing a partially cured photocurable material layer formed by patterning a layer of the uncured photocurable material after a preferred embodiment of the present invention;
圖4是一側視示意圖,說明本發明一較佳實施例之同時曝光部分區域固化之光固化材料層之固化區與未固化區的步驟;4 is a side elevational view showing the steps of simultaneously exposing a cured region and an uncured region of a partially cured photocurable material layer in accordance with a preferred embodiment of the present invention;
圖5是一側視示意圖,說明本發明一較佳實施例經圖4步驟後所得到一具有凹凸微結構表面之結構化的光固化材料層;及Figure 5 is a side elevational view showing a structured photocurable material layer having a textured surface having irregularities according to a step of Figure 4;
圖6是一側視示意圖,說明本發明一較佳實施例在圖5所形成的結構化的光固化材料層上濺鍍一層透明導電層而得到一導電基材的步驟。Figure 6 is a side elevational view showing a step of sputtering a transparent conductive layer on the structured photocurable material layer formed in Figure 5 to obtain a conductive substrate in accordance with a preferred embodiment of the present invention.
21...基底材twenty one. . . Base material
22...結構化的光固化材料層twenty two. . . Structured layer of photocurable material
220...凹凸微結構化表面220. . . Concave microstructured surface
23...透明導電層twenty three. . . Transparent conductive layer
230...上表面230. . . Upper surface
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