TWI555035B - Silver paste and method for manufacturing the same - Google Patents

Silver paste and method for manufacturing the same Download PDF

Info

Publication number
TWI555035B
TWI555035B TW104111661A TW104111661A TWI555035B TW I555035 B TWI555035 B TW I555035B TW 104111661 A TW104111661 A TW 104111661A TW 104111661 A TW104111661 A TW 104111661A TW I555035 B TWI555035 B TW I555035B
Authority
TW
Taiwan
Prior art keywords
solvent
binder solution
thixotropic agent
silver
conductive paste
Prior art date
Application number
TW104111661A
Other languages
Chinese (zh)
Other versions
TW201637026A (en
Inventor
黃欽麟
王福來
鐘宏碩
吳坤陽
Original Assignee
中國鋼鐵股份有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 中國鋼鐵股份有限公司 filed Critical 中國鋼鐵股份有限公司
Priority to TW104111661A priority Critical patent/TWI555035B/en
Publication of TW201637026A publication Critical patent/TW201637026A/en
Application granted granted Critical
Publication of TWI555035B publication Critical patent/TWI555035B/en

Links

Description

銀膠及其製造方法 Silver glue and its manufacturing method

本發明是有關於一種金屬膠,且特別是有關於一種銀膠及其製造方法。 The present invention relates to a metal glue, and more particularly to a silver paste and a method of manufacturing the same.

為提高矽晶太陽能電池之效率,已使得太陽能電池之正面的銀電極朝向細線寬的方向發展。為縮小銀電極之線寬,必須要提高用以製作銀電極之銀膠的黏度。但,銀膠黏度提高的同時,須提高銀膠之觸變性,才不致造成電池效率不升反降的問題。 In order to increase the efficiency of the twinned solar cell, the silver electrode on the front side of the solar cell has progressed toward the direction of the thin line width. In order to reduce the line width of the silver electrode, it is necessary to increase the viscosity of the silver paste used to make the silver electrode. However, while the viscosity of the silver glue is increased, it is necessary to increase the thixotropy of the silver glue so as not to cause the battery efficiency to rise and fall.

提高銀膠之觸變性的方法係將觸變劑加入銀膠中。觸變劑加入含金屬微粒的膠體中時,可使此類膠體在靜止時有較高的稠度,而在外力作用下又可使膠體變成低稠度流體。目前,普遍使用之觸變劑有四大類,包含氣相法製造之二氧化矽、有機膨潤土、氫化篦麻油及聚醯胺蠟。其中,二氧化矽與有機膨潤土會參與或干擾銀膠與矽晶間的反應,因此通常不會使用在矽晶太陽能電池之銀膠中;氫化篦麻油與聚醯胺蠟並無以上之缺點,而常用來提高銀膠之觸變性。 A method of increasing the thixotropy of silver paste is to add a thixotropic agent to the silver paste. When the thixotropic agent is added to the colloid containing the metal particles, the colloid can have a higher consistency at rest, and the colloid can become a low-consistency fluid under the action of external force. At present, there are four types of thixotropic agents commonly used, including gas phase process of cerium oxide, organic bentonite, hydrogenated castor oil and polyamidamine wax. Among them, cerium oxide and organic bentonite will participate in or interfere with the reaction between silver colloid and twin crystal, so it is usually not used in silver gel of twin solar cells; hydrogenated castor oil and polyamide wax have no such disadvantages. It is often used to increase the thixotropy of silver glue.

對於配製太陽能電池用之銀膠而言,氫化篦麻油與聚醯胺蠟雖無參與或干擾銀膠與矽晶間之反應的缺點,但氫化篦麻油與聚醯胺蠟在使用前必須先溶於溶劑中,再按所需比率添加。由於氫化篦麻油與聚醯胺蠟在有機溶劑中有溶解度的限制,為進一步提高銀膠之觸變係數,必須提高觸變劑的添加量,如此一來,會影響其它添加劑的劑量,造成製程的複雜度提高。 For the preparation of silver paste for solar cells, hydrogenated castor oil and polyamide wax do not participate in or interfere with the reaction between silver gel and twin crystal, but hydrogenated castor oil and polyamide wax must be dissolved before use. In a solvent, add in the desired ratio. Due to the solubility limitation of hydrogenated castor oil and polyamidamide wax in organic solvents, in order to further increase the thixotropic coefficient of silver paste, it is necessary to increase the amount of thixotropic agent added, thus affecting the dosage of other additives, resulting in a process. The complexity is improved.

因此,本發明之一目的就是在提供一種銀膠及其製造方法,其係在膠體混煉後,以少量逐次加入的方式添加液態的聚二甲基矽烷於膠體內,藉此不僅可有效提高銀膠之觸變性,且可提供潤滑效果,更具有計量容易與作業方便等優勢。 Therefore, an object of the present invention is to provide a silver paste and a method for producing the same, which is characterized in that after the colloidal kneading, the liquid polydimethyl decane is added to the gel body in a small amount of successively, thereby not only effectively improving The thixotropy of silver gel provides lubrication and is easy to measure and easy to operate.

根據本發明之上述目的,提出一種銀膠適用以製作電極。此銀膠包含導電膠以及觸變劑。導電膠包含黏結劑溶液、玻璃粉、有機分散劑、第二溶劑以及銀粉。黏結劑溶液包含溶質與第一溶劑,其中溶質包含乙基纖維素,且第一溶劑可溶解乙基纖維素。黏結劑溶液之含量為7.0wt%至7.7wt%。玻璃粉混合於黏結劑溶液中,其中玻璃粉包含鉛、硼與矽。玻璃粉之含量為4.2wt%至4.4wt%。有機分散劑混合於黏結劑溶液中。有機分散劑之含量為0.10wt%至0.35wt%。第二溶劑混合於黏結劑溶液中。第二溶劑含量為0wt%至2.0wt%。銀粉混合於黏結劑溶液中,其中銀粉 之含量為84.3wt%至86.5wt%。觸變劑混合於導電膠中,其中觸變劑包含聚二甲基矽烷,且觸變劑之重量為導電膠之總重量的0.02%至2.5%。 In accordance with the above objects of the present invention, a silver paste is proposed for use in the fabrication of electrodes. The silver paste contains a conductive paste and a thixotropic agent. The conductive paste comprises a binder solution, a glass frit, an organic dispersant, a second solvent, and a silver powder. The binder solution comprises a solute and a first solvent, wherein the solute comprises ethylcellulose, and the first solvent dissolves ethylcellulose. The content of the binder solution is from 7.0 wt% to 7.7 wt%. The glass frit is mixed in the binder solution, wherein the glass frit contains lead, boron and antimony. The content of the glass frit is from 4.2% by weight to 4.4% by weight. The organic dispersant is mixed in the binder solution. The content of the organic dispersant is from 0.10% by weight to 0.35% by weight. The second solvent is mixed in the binder solution. The second solvent content is from 0 wt% to 2.0 wt%. Silver powder mixed in a binder solution, in which silver powder The content is from 84.3 wt% to 86.5 wt%. The thixotropic agent is mixed in the conductive paste, wherein the thixotropic agent comprises polydimethyl decane, and the weight of the thixotropic agent is 0.02% to 2.5% of the total weight of the conductive paste.

依據本發明之一實施例,上述之觸變劑為純的聚二甲基矽烷。 According to an embodiment of the invention, the thixotropic agent is pure polydimethyl decane.

依據本發明之另一實施例,上述之溶質更包含潤滑劑。 According to another embodiment of the invention, the solute further comprises a lubricant.

依據本發明之又一實施例,上述之第一溶劑與第二溶劑包含二乙二醇己醚(hexyl carbitol,HC)溶劑與二乙二醇丁醚醋酸酯(butyl carbitol acetate,BCA)溶劑。 According to still another embodiment of the present invention, the first solvent and the second solvent comprise a hexyl carbitol (HC) solvent and a butyl carbitol acetate (BCA) solvent.

依據本發明之再一實施例,上述之第一溶劑更包含松油醇。 According to still another embodiment of the present invention, the first solvent further comprises terpineol.

依據本發明之再一實施例,上述之第一溶劑包含二元酸酯溶劑(DBE)或二乙二醇單丁醚(BC)。 According to still another embodiment of the present invention, the first solvent comprises a dibasic acid ester solvent (DBE) or diethylene glycol monobutyl ether (BC).

根據本發明之上述目的,另提出一種銀膠之製造方法,其包含下列步驟。配製黏結劑溶液,以將溶質溶解於第一溶劑中,其中此溶質包含乙基纖維素。配製導電膠。配製導電膠之步驟包含下列步驟。混合一玻璃粉與一有機分散劑,以形成一混合物,其中玻璃粉之含量為4.2wt%至4.4wt%,有機分散劑之含量為0.10wt%至0.35wt%,且玻璃粉包含鉛、硼與矽。將第二溶劑與黏結劑溶液加入混合物中,其中黏結劑溶液之含量為7.0wt%至7.7wt%,第二溶劑含量為0wt%至2.0wt%。將銀粉加入混有第二溶劑與黏結劑溶液之混合物中,其中銀粉之含量為84.3wt%至 86.5wt%。將觸變劑加入導電膠中,其中觸變劑包含聚二甲基矽烷,且觸變劑之重量為導電膠之總重量的0.02%至2.5%。 According to the above object of the present invention, there is further provided a method for producing a silver paste comprising the following steps. A binder solution is prepared to dissolve the solute in a first solvent, wherein the solute comprises ethylcellulose. Prepare a conductive paste. The step of preparing the conductive paste comprises the following steps. Mixing a glass frit with an organic dispersant to form a mixture in which the content of the glass frit is from 4.2 wt% to 4.4 wt%, the content of the organic dispersant is from 0.10 wt% to 0.35 wt%, and the glass frit contains lead and boron. With 矽. A second solvent and a binder solution are added to the mixture, wherein the binder solution is present in an amount of 7.0 wt% to 7.7% by weight, and the second solvent content is 0 wt% to 2.0 wt%. Adding silver powder to the mixture mixed with the second solvent and the binder solution, wherein the content of the silver powder is 84.3 wt% to 86.5 wt%. The thixotropic agent is added to the conductive paste, wherein the thixotropic agent comprises polydimethyl decane, and the weight of the thixotropic agent is 0.02% to 2.5% of the total weight of the conductive paste.

依據本發明之一實施例,上述之觸變劑為純的聚二甲基矽烷。 According to an embodiment of the invention, the thixotropic agent is pure polydimethyl decane.

依據本發明之另一實施例,上述之第一溶劑與第二溶劑包含二乙二醇己醚(HC)溶劑與二乙二醇丁醚醋酸酯(BCA)。在第一溶劑與第二溶劑中,二乙二醇己醚(HC)溶劑與二乙二醇丁醚醋酸酯(BCA)之重量比為1:1。 According to another embodiment of the present invention, the first solvent and the second solvent comprise a diethylene glycol hexyl ether (HC) solvent and diethylene glycol butyl ether acetate (BCA). In the first solvent and the second solvent, the weight ratio of the diethylene glycol hexyl ether (HC) solvent to the diethylene glycol butyl ether acetate (BCA) is 1:1.

依據本發明之又一實施例,於將銀粉加入混有第二溶劑與黏結劑溶液之混合物中後,上述配製導電膠之步驟更包含利用三滾筒進行複數個混煉處理。 According to still another embodiment of the present invention, after the silver powder is added to the mixture mixed with the second solvent and the binder solution, the step of preparing the conductive paste further comprises performing a plurality of kneading treatments using the three rollers.

依據本發明之再一實施例,上述將觸變劑加入導電膠之步驟包含下列步驟。降低三滾筒之轉速。在導電膠於三滾筒中時,分批加入觸變劑。於觸變劑加入導電膠後,利用此三滾筒進行複數個再次混煉處理。 According to still another embodiment of the present invention, the step of adding the thixotropic agent to the conductive paste comprises the following steps. Reduce the speed of the three rollers. When the conductive paste is in the three rolls, the thixotropic agent is added in portions. After the conductive agent is added to the thixotropy, a plurality of re-kneading treatments are performed using the three rollers.

100‧‧‧步驟 100‧‧‧ steps

102‧‧‧步驟 102‧‧‧Steps

104‧‧‧步驟 104‧‧‧Steps

200‧‧‧步驟 200‧‧‧ steps

202‧‧‧步驟 202‧‧‧Steps

204‧‧‧步驟 204‧‧‧Steps

為讓本發明之上述和其他目的、特徵、優點與實施例能更明顯易懂,所附圖式之說明如下:〔圖1〕係繪示依照本發明之一實施方式的一種銀膠之製造方法的流程圖;以及 〔圖2〕係繪示依照本發明之一實施方式的一種配製導 電膠之流程圖。 The above and other objects, features, advantages and embodiments of the present invention will become more <RTIgt; <RTIgt; </ RTI> <RTIgt; </ RTI> <RTIgt; Flow chart of the method; [Fig. 2] shows a formula guide according to an embodiment of the present invention. Flow chart of electric glue.

有鑑於習知觸變劑有些會參與或干擾銀膠與矽晶間的反應,有些在有機溶劑中的溶解度有限,因此這些習知觸變劑不是不適合添加在用以製作太陽能電池之電極的銀膠中,就是有添加程序複雜的問題。故,本發明在此提出一種銀膠及其製造方法,其採用液態的聚二甲基矽烷來作為銀膠之觸變劑,可提高銀膠之觸變性,並可提供潤滑效果,且計量容易而可簡化觸變劑的添加作業。 In view of the fact that some thixotropic agents may participate in or interfere with the reaction between silver colloid and twin, some of them have limited solubility in organic solvents, so these conventional thixotropic agents are not unsuitable for addition to the silver used to make the electrodes of solar cells. In the glue, there is a problem of adding complicated programs. Therefore, the present invention proposes a silver paste and a method for producing the same, which uses liquid polydimethyl decane as a thixotropic agent for silver gum, which can improve the thixotropy of the silver paste, and can provide a lubricating effect and is easy to measure. It can simplify the addition of thixotropic agents.

在本發明之一實施方式中,銀膠可適用以製作電極,例如太陽能電池之電極,特別是太陽能電池之正面電極。在一些實施例中,銀膠主要包含導電膠以及觸變劑,其中導電膠為主要成分,觸變劑為添加物。舉例而言,在銀膠中,觸變劑之重量可為導電膠之總重量的0.02%至2.5%。 In one embodiment of the invention, silver paste can be used to make electrodes, such as electrodes for solar cells, particularly front electrodes for solar cells. In some embodiments, the silver paste mainly comprises a conductive paste and a thixotropic agent, wherein the conductive paste is a main component and the thixotropic agent is an additive. For example, in silver paste, the weight of the thixotropic agent may be from 0.02% to 2.5% of the total weight of the conductive paste.

在一些例子中,導電膠主要可包含黏結劑溶液、玻璃粉、有機分散劑、第二溶劑以及銀粉。在導電膠中,黏結劑溶液之含量可例如為7.0wt%至7.7wt%。黏結劑溶液可包含有溶質與第一溶劑。此外,黏結劑溶液可為有機溶液。舉例而言,溶質包含乙基纖維素。選擇性地,除了乙基纖維素,溶質還可包含潤滑劑。在溶質包含乙基纖維素的例子中,第一溶劑為可溶解該乙基纖維素之溶劑。第一溶劑可例如包含二乙二醇己醚(HC)溶劑及/或二乙二醇丁醚醋酸 酯(BCA)溶劑。在一些黏結劑溶液之第一溶劑的示範例子中,二乙二醇己醚(HC)溶劑與二乙二醇丁醚醋酸酯(BCA)溶劑之重量比為1:1。然,在其它例子中,二乙二醇己醚(HC)溶劑與二乙二醇丁醚醋酸酯(BCA)溶劑之重量比可不為1:1,而為其它配比。 In some examples, the conductive paste may mainly comprise a binder solution, a glass frit, an organic dispersant, a second solvent, and silver powder. In the conductive paste, the content of the binder solution may be, for example, 7.0% by weight to 7.7% by weight. The binder solution may comprise a solute and a first solvent. Further, the binder solution may be an organic solution. For example, the solute comprises ethyl cellulose. Alternatively, the solute may contain a lubricant in addition to ethyl cellulose. In the case where the solute contains ethyl cellulose, the first solvent is a solvent which can dissolve the ethyl cellulose. The first solvent may, for example, comprise diethylene glycol hexyl ether (HC) solvent and/or diethylene glycol butyl ether acetate Ester (BCA) solvent. In an exemplary embodiment of the first solvent of some of the binder solutions, the weight ratio of the diethylene glycol hexyl ether (HC) solvent to the diethylene glycol butyl ether acetate (BCA) solvent is 1:1. However, in other examples, the weight ratio of the diethylene glycol hexyl ether (HC) solvent to the diethylene glycol butyl ether acetate (BCA) solvent may not be 1:1, but other ratios.

選擇性地,除了二乙二醇己醚(HC)溶劑及二乙二醇丁醚醋酸酯(BCA)溶劑外,第一溶劑更可包含松油醇。黏結劑溶液之第一溶劑可包含其它可溶解乙基纖維素的溶劑,例如二元酸酯溶劑(aliphatic dibasic ester mixture,DBE)與二乙二醇單丁醚(butyl carbitol,BC)。此外,在一些黏結劑溶液之示範例子中,溶質與第一溶劑之重量比可為1:10。 Alternatively, the first solvent may further comprise terpineol in addition to the diethylene glycol hexyl ether (HC) solvent and the diethylene glycol butyl ether acetate (BCA) solvent. The first solvent of the binder solution may comprise other solvents that dissolve ethylcellulose, such as an aliphatic dibasic ester mixture (DBE) and butyl carbitol (BC). Further, in some exemplary examples of the binder solution, the weight ratio of the solute to the first solvent may be 1:10.

玻璃粉混合於黏結劑溶液中。在一些例子中,玻璃粉可包含鉛與硼、矽等等其它元素。此外,玻璃粉於導電膠中之含量可例如為4.2wt%至4.4wt%。舉例而言,將玻璃粉混合於黏結劑溶液中之前,可先將玻璃粉與有機分散劑混合,再將玻璃粉與有機分散劑的混合物,一起混合於黏結劑溶液中。於導電膠中,有機分散劑之含量可例如為0.10wt%至0.35wt%。在一些例子中,有機分散劑可為硬脂酸。 The glass frit is mixed in the binder solution. In some examples, the glass frit may contain lead and other elements such as boron, bismuth, and the like. Further, the content of the glass frit in the conductive paste may be, for example, 4.2% by weight to 4.4% by weight. For example, before mixing the glass frit into the binder solution, the glass frit may be mixed with the organic dispersant, and the mixture of the glass frit and the organic dispersant may be mixed together in the binder solution. The content of the organic dispersant may be, for example, from 0.10% by weight to 0.35% by weight in the conductive paste. In some examples, the organic dispersant can be stearic acid.

將玻璃粉與有機分散劑的混合物混合於黏結劑溶液中時,可同時將第二溶劑一起混入。第二溶劑於導電膠中之含量可例如為0wt%至2.0wt%。在一些例子中,第二溶劑可與第一溶劑包含相同之成分。舉例而言,第二溶劑與 第一溶劑均包含二乙二醇己醚(HC)溶劑與二乙二醇丁醚醋酸酯(BCA)溶劑。在第二溶劑中,二乙二醇己醚(HC)溶劑與二乙二醇丁醚醋酸酯(BCA)溶劑之重量比可例如為1:1。在其它例子中,第二溶劑之二乙二醇己醚(HC)溶劑與二乙二醇丁醚醋酸酯(BCA)溶劑可為其它配比。銀粉同樣也混合於黏結劑溶液中。在一些例子中,銀粉於導電膠中之含量可例如為84.3wt%至86.5wt%。 When the mixture of the glass frit and the organic dispersant is mixed in the binder solution, the second solvent may be mixed together at the same time. The content of the second solvent in the conductive paste may be, for example, 0% by weight to 2.0% by weight. In some examples, the second solvent can comprise the same components as the first solvent. For example, the second solvent and The first solvent each contains a diethylene glycol hexyl ether (HC) solvent and a diethylene glycol butyl ether acetate (BCA) solvent. In the second solvent, the weight ratio of the diethylene glycol hexyl ether (HC) solvent to the diethylene glycol butyl ether acetate (BCA) solvent may be, for example, 1:1. In other examples, the second solvent of the diethylene glycol hexyl ether (HC) solvent and the diethylene glycol butyl ether acetate (BCA) solvent may be in other ratios. Silver powder is also mixed in the binder solution. In some examples, the content of the silver powder in the conductive paste may be, for example, 84.3 wt% to 86.5 wt%.

觸變劑混合於導電膠中。在本實施方式中,觸變劑包含聚二甲基矽烷。在一些特定例子中,觸變劑為純的聚二甲基矽烷。觸變劑所選用之聚二甲基矽烷可為黏度較低的,亦可為黏度較高的。 The thixotropic agent is mixed in the conductive paste. In the present embodiment, the thixotropic agent comprises polydimethyldecane. In some specific examples, the thixotropic agent is pure polydimethyl decane. The polydimethyl decane selected for the thixotropic agent may be of lower viscosity or higher viscosity.

請參照圖1,其係繪示依照本發明之一實施方式的一種銀膠之製造方法的流程圖。在本實施方式中,製造銀膠時,可先進行步驟100,以配製黏結劑溶液。配製黏結劑溶液時,係將溶質與第一溶劑混合,再藉由例如靜置與加熱等手段,使溶質溶解於第一溶劑中。所配製之黏結劑溶液可為有機溶液。在一些例子中,溶質包含乙基纖維素。除了乙基纖維素,溶質還可選擇性地包含潤滑劑。在溶質包含乙基纖維素的例子中,第一溶劑為可溶解該乙基纖維素之溶劑。第一溶劑可例如包含二乙二醇己醚(HC)溶劑及/或二乙二醇丁醚醋酸酯(BCA)溶劑。舉例而言,第一溶劑包含二乙二醇己醚(HC)溶劑與二乙二醇丁醚醋酸酯(BCA)溶劑,且二乙二醇己醚(HC)溶劑與二乙二醇丁醚醋酸酯(BCA)溶劑之 重量比為1:1。在其它例子中,二乙二醇己醚(HC)溶劑與二乙二醇丁醚醋酸酯(BCA)溶劑之重量比可為其它配比。 Please refer to FIG. 1 , which is a flow chart of a method for manufacturing a silver paste according to an embodiment of the present invention. In the present embodiment, when manufacturing silver paste, step 100 may be performed first to prepare a binder solution. When the binder solution is prepared, the solute is mixed with the first solvent, and the solute is dissolved in the first solvent by, for example, standing and heating. The prepared binder solution can be an organic solution. In some examples, the solute comprises ethyl cellulose. In addition to ethyl cellulose, the solute may optionally contain a lubricant. In the case where the solute contains ethyl cellulose, the first solvent is a solvent which can dissolve the ethyl cellulose. The first solvent may, for example, comprise a diethylene glycol hexyl ether (HC) solvent and/or a diethylene glycol butyl ether acetate (BCA) solvent. For example, the first solvent comprises a diethylene glycol hexyl ether (HC) solvent and a diethylene glycol butyl ether acetate (BCA) solvent, and the diethylene glycol hexyl ether (HC) solvent and diethylene glycol butyl ether Acetate (BCA) solvent The weight ratio is 1:1. In other examples, the weight ratio of diethylene glycol hexyl ether (HC) solvent to diethylene glycol butyl ether acetate (BCA) solvent can be other ratios.

除了二乙二醇己醚(HC)溶劑及二乙二醇丁醚醋酸酯(BCA)溶劑外,第一溶劑更可選擇性地包含松油醇。黏結劑溶液之第一溶劑亦可包含其它可溶解乙基纖維素的溶劑,例如二元酸酯溶劑(DBE)與二乙二醇單丁醚(BC)。此外,在一些示範例子中,溶質與第一溶劑之重量比可為1:10。 In addition to the diethylene glycol hexyl ether (HC) solvent and the diethylene glycol butyl ether acetate (BCA) solvent, the first solvent more selectively comprises terpineol. The first solvent of the binder solution may also comprise other solvents which dissolve ethylcellulose, such as dibasic acid ester solvent (DBE) and diethylene glycol monobutyl ether (BC). Further, in some exemplary examples, the weight ratio of the solute to the first solvent may be 1:10.

完成黏結劑溶液的配製後,進行步驟102,以利用黏結劑溶液為其中一組成來配製導電膠。請一併參照圖2,其係繪示依照本發明之一實施方式的一種配製導電膠之流程圖。如圖2所示,在一些例子中,配製導電膠時,可先進行步驟200,以將玻璃粉置入一容器,例如鐵氟龍燒杯中,再將有機分散劑加入容器中,並將玻璃粉與有機分散劑充分混合而形成一混合物。在一些例子中,玻璃粉可包含鉛與硼、矽等其它元素。此外,玻璃粉於導電膠中之含量可例如為4.2wt%至4.4wt%。有機分散劑於導電膠中之含量可例如為0.10wt%至0.35wt%。在一些例子中,有機分散劑可為硬脂酸。 After the preparation of the binder solution is completed, step 102 is performed to prepare a conductive paste by using the binder solution as one of the components. Referring to FIG. 2 together, a flow chart of preparing a conductive adhesive according to an embodiment of the present invention is shown. As shown in FIG. 2, in some examples, when preparing the conductive paste, step 200 may be first performed to place the glass frit into a container, such as a Teflon beaker, and then the organic dispersant is added to the container, and the glass is placed. The powder is thoroughly mixed with the organic dispersant to form a mixture. In some examples, the glass frit may contain lead and other elements such as boron, antimony, and the like. Further, the content of the glass frit in the conductive paste may be, for example, 4.2% by weight to 4.4% by weight. The content of the organic dispersant in the conductive paste may be, for example, from 0.10% by weight to 0.35% by weight. In some examples, the organic dispersant can be stearic acid.

接下來,進行步驟202,以將第二溶劑與黏結劑溶液加入容器中,藉此使第二溶劑及黏結劑溶液混合於玻璃粉與有機分散劑的混合物中。第二溶劑於導電膠中之含量可例如為0wt%至2.0wt%。黏結劑溶液於導電膠中之含量可例如為7.0wt%至7.7wt%。在一些例子中,第二溶劑可與 第一溶劑包含相同之成分。舉例而言,第二溶劑與第一溶劑均包含二乙二醇己醚(HC)溶劑與二乙二醇丁醚醋酸酯(BCA)溶劑。在第二溶劑中,二乙二醇己醚(HC)溶劑與二乙二醇丁醚醋酸酯(BCA)溶劑之重量比可例如為1:1。在其它例子中,第二溶劑之二乙二醇己醚(HC)溶劑與二乙二醇丁醚醋酸酯(BCA)溶劑可為其它配比。 Next, step 202 is performed to add the second solvent and the binder solution to the container, thereby mixing the second solvent and the binder solution in the mixture of the glass frit and the organic dispersant. The content of the second solvent in the conductive paste may be, for example, 0% by weight to 2.0% by weight. The content of the binder solution in the conductive paste may be, for example, 7.0% by weight to 7.7% by weight. In some examples, the second solvent can be The first solvent contains the same ingredients. For example, both the second solvent and the first solvent comprise a diethylene glycol hexyl ether (HC) solvent and a diethylene glycol butyl ether acetate (BCA) solvent. In the second solvent, the weight ratio of the diethylene glycol hexyl ether (HC) solvent to the diethylene glycol butyl ether acetate (BCA) solvent may be, for example, 1:1. In other examples, the second solvent of the diethylene glycol hexyl ether (HC) solvent and the diethylene glycol butyl ether acetate (BCA) solvent may be in other ratios.

待玻璃粉於有機分散劑、第二溶劑與黏結劑溶液中完全潤濕後,進行步驟204,以將銀粉加入玻璃粉、有機分散劑、第二溶劑與黏結劑溶液混合物中。銀粉於導電膠中之含量可例如為84.3wt%至86.5wt%。在一些例子中,可先將銀粉、玻璃粉、有機分散劑、第二溶劑與黏結劑溶液充分混合,然後以三滾筒加以混煉兩次或三次以上,而製得導電膠。 After the glass frit is completely wetted in the organic dispersant, the second solvent and the binder solution, step 204 is performed to add the silver powder to the glass frit, the organic dispersant, and the second solvent and the binder solution mixture. The content of the silver powder in the conductive paste may be, for example, from 84.3 wt% to 86.5 wt%. In some examples, the silver powder, the glass frit, the organic dispersant, the second solvent, and the binder solution may be thoroughly mixed, and then kneaded twice or three times with a three-roller to prepare a conductive paste.

完成導電膠的配製後,如圖1所示,進行步驟104,以將觸變劑加入導電膠中,而完成銀膠的配製。在銀膠中,觸變劑之重量可例如為導電膠之總重量的0.02%至2.5%。在本實施方式中,觸變劑包含聚二甲基矽烷。在一些特定例子中,觸變劑為純的聚二甲基矽烷。觸變劑所選用之聚二甲基矽烷可為黏度較低的,亦可為黏度較高的。 After the preparation of the conductive paste is completed, as shown in FIG. 1, step 104 is performed to add the thixotropic agent to the conductive paste to complete the preparation of the silver paste. In the silver paste, the weight of the thixotropic agent may be, for example, 0.02% to 2.5% of the total weight of the conductive paste. In the present embodiment, the thixotropic agent comprises polydimethyldecane. In some specific examples, the thixotropic agent is pure polydimethyl decane. The polydimethyl decane selected for the thixotropic agent may be of lower viscosity or higher viscosity.

在一些例子中,將觸變劑加入導電膠時,可先降低三滾筒之轉速,再分批將觸變劑加入三滾筒中的導電膠。觸變劑加入導電膠之後,再利用此三滾筒對導電膠與觸變劑的混合物進行兩次或三次以上的再次混煉處理。 In some examples, when the thixotropic agent is added to the conductive paste, the rotation speed of the three rollers can be first reduced, and the thixotropic agent is added to the conductive paste in the three rollers in batches. After the thixotropic agent is added to the conductive paste, the mixture of the conductive paste and the thixotropic agent is subjected to re-kneading treatment twice or more times by using the three rollers.

透過採用液態的聚二甲基矽烷來作為觸變劑,可以少量逐次加入的方式來將觸變劑添加於導電膠中,因此本實施方式可提高銀膠之觸變性,並可提供潤滑效果,且計量容易而可簡化觸變劑的添加作業。 By using liquid polydimethyl decane as a thixotropic agent, a thixotropic agent can be added to the conductive adhesive in a small amount of successive additions. Therefore, the embodiment can improve the thixotropy of the silver paste and provide a lubricating effect. Moreover, the metering is easy and the addition of the thixotropic agent can be simplified.

以下利用數個實施例與比較例來說明本發明之優勢。在比較例1中,首先進行黏結劑溶液的配製。配製黏結劑溶液時,先秤取1.60g的乙基纖維素、以及8.0g的二乙二醇己醚(HC)溶劑與8.0g的二乙二醇丁醚醋酸酯(BCA)溶劑。將乙基纖維素與二乙二醇己醚(HC)溶劑及二乙二醇丁醚醋酸酯(BCA)溶劑混合後,置於耐壓玻璃瓶中,並將之密封。接下來,於90℃下加熱至完全乙基纖維素完全溶解。再加入4.0g的油酸聚氧乙烯酯Sinopol 170,並繼續加熱直至所有溶質完全溶解,然後予以冷卻。隨後,加入5.31g的松油醇,並加以攪拌至均勻混合,完成黏結劑溶液的製備。 The advantages of the present invention are illustrated below using a number of examples and comparative examples. In Comparative Example 1, the preparation of the binder solution was first carried out. When preparing the binder solution, 1.60 g of ethylcellulose and 8.0 g of diethylene glycol hexyl ether (HC) solvent and 8.0 g of diethylene glycol butyl ether acetate (BCA) solvent were weighed first. The ethyl cellulose was mixed with a diethylene glycol hexyl ether (HC) solvent and a diethylene glycol butyl ether acetate (BCA) solvent, placed in a pressure-resistant glass bottle, and sealed. Next, it was heated at 90 ° C until completely ethyl cellulose was completely dissolved. An additional 4.0 g of oleic acid polyoxyethylene Sinopol 170 was added and heating was continued until all solutes were completely dissolved and then cooled. Subsequently, 5.31 g of terpineol was added and stirred until homogeneously mixed to complete the preparation of the binder solution.

接著,進行導電膠的配製。配製導電膠時,先秤取2.6g含鉛與碲的玻璃粉,並將玻璃粉置入鐵氟龍燒杯中。再加入0.2g的有機分散劑於鐵氟龍燒杯中,並利用手動方式將玻璃粉與有機分散劑充分混合。接下來,加入0.7g的二乙二醇己醚(HC)/二乙二醇丁醚醋酸酯(BCA)溶劑與4.6g的黏結劑溶液。在此溶劑中,二乙二醇己醚(HC)與二乙二醇丁醚醋酸酯(BCA)的重量比為1:1。於玻璃粉完全潤濕之後,加入51.60g的銀粉,並加以充分混合,再利用三滾筒混煉三次,而製得比較例1之導電膠,也就是比較例1之銀膠。 Next, the preparation of the conductive paste is performed. When preparing conductive paste, first weigh 2.6g of lead powder and lead glass powder, and place the glass powder into the Teflon beaker. Further, 0.2 g of an organic dispersant was added to the Teflon beaker, and the glass frit was thoroughly mixed with the organic dispersant by hand. Next, 0.7 g of diethylene glycol hexyl ether (HC) / diethylene glycol butyl ether acetate (BCA) solvent and 4.6 g of a binder solution were added. In this solvent, the weight ratio of diethylene glycol hexyl ether (HC) to diethylene glycol butyl ether acetate (BCA) was 1:1. After the glass frit was completely wetted, 51.60 g of silver powder was added and thoroughly mixed, and then kneaded three times with a three-roller to obtain a conductive paste of Comparative Example 1, that is, the silver paste of Comparative Example 1.

在各實施例與比較例中,所製得之銀膠均以美國Brookfield公司所提供之黏度計DV-II+Pro viscometer cone/plate version在2rpm及27.0±0.5℃下測定。 In each of the examples and comparative examples, the silver gums obtained were all measured at 2 rpm and 27.0 ± 0.5 ° C using a viscometer DV-II + Pro viscometer cone/plate version supplied by Brookfield, USA.

在比較例2中,黏結劑溶液之配製的前段實驗條件和作業與比較例1之黏結劑溶液的配製大致相同,不同之處在於更加入了5.31g含10%之聚醯胺6500的松油醇溶液,並攪拌至均勻混合。而銀膠之配製步驟和方法與比較例1之銀膠之配製步驟和方法相同,但黏結劑溶液採用本比較例之黏結劑溶液。 In Comparative Example 2, the previous experimental conditions and operation of the preparation of the cement solution were substantially the same as those of the cement solution of Comparative Example 1, except that 5.31 g of pine oil containing 10% polyamine 6500 was further added. The alcohol solution was stirred until homogeneously mixed. The steps and methods for preparing the silver paste are the same as those for the silver paste of Comparative Example 1, but the binder solution is the solution of the binder of the comparative example.

在比較例3中,黏結劑溶液之配製的前段實驗條件和作業與比較例1之黏結劑溶液的配製大致相同,不同之處在於更加入了5.31g含10%之HCO的松油醇溶液,並攪拌至均勻混合。而銀膠之配製步驟和方法與比較例1之銀膠之配製步驟和方法相同,但黏結劑溶液採用本比較例之黏結劑溶液。 In Comparative Example 3, the previous experimental conditions and operation of the preparation of the binder solution were substantially the same as those of the binder solution of Comparative Example 1, except that 5.31 g of a terpineol solution containing 10% of HCO was further added. Stir until homogeneously mixed. The steps and methods for preparing the silver paste are the same as those for the silver paste of Comparative Example 1, but the binder solution is the solution of the binder of the comparative example.

在實施例4中,黏結劑溶液同比較例1。導電膠之配製步驟與方法同比較例1,但在導電膠配製完成後,調慢三滾筒之轉速,並將0.020g的聚二甲基矽烷-1逐次平均加入導電膠上,再以三滾筒再次混煉三次,而製得本實施例之銀膠。 In Example 4, the binder solution was the same as Comparative Example 1. The preparation steps and methods of the conductive adhesive are the same as those of the comparative example 1, but after the preparation of the conductive adhesive is completed, the rotation speed of the three rollers is adjusted, and 0.020 g of polydimethyl decane-1 is successively added to the conductive rubber, and then three rollers are used. The silver paste of this example was obtained by mixing again three times.

在實施例5~14中,黏結劑溶液同比較例1。導電膠之配製步驟與方法同比較例1。觸變劑之添加方法同實施例4,惟聚二甲基矽烷-1的重量改為0.047g~1.20g。 In Examples 5 to 14, the binder solution was the same as Comparative Example 1. The steps and methods for preparing the conductive paste were the same as in Comparative Example 1. The thixotropic agent was added in the same manner as in Example 4 except that the weight of the polydimethyldecane-1 was changed to 0.047 g to 1.20 g.

在實施例15中,黏結劑溶液同比較例1。導電膠之配製步驟與方法同比較例1。觸變劑之添加方法同實施例4,惟觸變劑改為添加0.020g的聚二甲基矽烷-2。其中,聚二甲基矽烷-1的分子量比聚二甲基矽烷-2的分子量高。 In Example 15, the binder solution was the same as Comparative Example 1. The steps and methods for preparing the conductive paste were the same as in Comparative Example 1. The thixotropic agent was added in the same manner as in Example 4 except that the thixotropic agent was changed to add 0.020 g of polydimethylnonane-2. Among them, the molecular weight of polydimethyldecane-1 is higher than the molecular weight of polydimethyldecane-2.

在實施例16~21中,黏結劑溶液同比較例1。導電膠之配製步驟與方法同比較例1。觸變劑之添加方法同實施例15,惟聚二甲基矽烷-2的添加量改為0.095g~1.20g。 In Examples 16 to 21, the binder solution was the same as Comparative Example 1. The steps and methods for preparing the conductive paste were the same as in Comparative Example 1. The method of adding the thixotropic agent was the same as in Example 15, except that the amount of polydimethyldecane-2 added was changed to 0.095 g to 1.20 g.

在比較例22與23中,黏結劑溶液同比較例1。導電膠之配製步驟與方法同比較例1,但追加0.10g且重量比為1:1的二乙二醇己醚(HC)/二乙二醇丁醚醋酸酯(BCA)溶劑。觸變劑之添加方法同前,惟改為添加0.095g或0.379g的改質聚矽氧烷。 In Comparative Examples 22 and 23, the binder solution was the same as Comparative Example 1. The procedure and method for preparing the conductive paste were the same as in Comparative Example 1, except that 0.10 g of a diethylene glycol hexyl ether (HC)/diethylene glycol butyl ether acetate (BCA) solvent having a weight ratio of 1:1 was added. The thixotropic agent was added in the same manner as before, except that 0.095 g or 0.379 g of modified polyoxyalkylene was added.

在比較例24與25中,黏結劑溶液同比較例1。導電膠之配製步驟與方法同比較例1,但因黏度稍高而分別添加0.20g之1:1的HC與BCA混合溶劑稀釋。觸變劑之添加方法同前,惟改為添加0.095g或0.379g的環氧基矽烷。 In Comparative Examples 24 and 25, the binder solution was the same as Comparative Example 1. The procedure and method for preparing the conductive paste were the same as in Comparative Example 1, but 0.20 g of a 1:1 mixture of HC and BCA was added to each other because of a slightly higher viscosity. The thixotropic agent was added in the same manner as before, except that 0.095 g or 0.379 g of epoxy decane was added.

在比較例26與27中,黏結劑溶液同比較例1。導電膠之配製步驟與方法同比較例1,但因黏度超出黏度計可測定範圍而分別添加0.70g及1.20g之1:1的HC與BCA混合溶劑稀釋。觸變劑之添加方法同前,惟改為添加0.095g或0.379g的胺基矽烷。 In Comparative Examples 26 and 27, the binder solution was the same as Comparative Example 1. The procedure and method for preparing the conductive paste were the same as in Comparative Example 1, but the viscosity was outside the range measurable by the viscometer, and 0.70 g and 1.20 g of a 1:1 mixture of HC and BCA were added. The thixotropic agent was added in the same manner as before, except that 0.095 g or 0.379 g of aminodecane was added.

在實施例28與29中,黏結劑溶液之配製方法類似比較例1,惟溶劑中之二乙二醇己醚(HC)與二乙二醇丁醚醋酸酯(BCA)的重量比改為1:3,且未添加松油醇。導電 膠之配製步驟與方法同比較例1,但分散劑1.0g含10%硬酯酸(SA)之溶液,黏結劑溶液改用此實施例之新配溶液,且用量改為4.60g。觸變劑之添加方法同前,惟改為添加0.40g或1.0g的聚二甲基矽烷-1。 In Examples 28 and 29, the preparation method of the binder solution was similar to that of Comparative Example 1, except that the weight ratio of diethylene glycol hexyl ether (HC) to diethylene glycol butyl ether acetate (BCA) in the solvent was changed to 1 : 3, and no terpineol was added. Conductive The preparation steps and methods of the gel were the same as those of Comparative Example 1, except that 1.0 g of the dispersant contained 10% of the solution of stearic acid (SA), and the solution of the binder was changed to the new solution of this example, and the amount was changed to 4.60 g. The thixotropic agent was added in the same manner as before, except that 0.40 g or 1.0 g of polydimethylnonane-1 was added.

在實施例30與31中,黏結劑溶液同實施例28。導電膠之配製步驟與方法同實施例28。觸變劑之添加方法同前,惟改為添加0.40g或1.0g的聚二甲基矽烷-2。 In Examples 30 and 31, the binder solution was the same as in Example 28. The procedure and method for preparing the conductive paste were the same as those in Example 28. The thixotropic agent was added in the same manner as before, except that 0.40 g or 1.0 g of polydimethylnonane-2 was added.

下表1列示了上述比較例與實施例之各項特性。 Table 1 below lists the characteristics of the above comparative examples and examples.

以下另外利用數個實施例來說明不同溶劑對聚二甲基矽烷之觸變效果的影響。 Several examples are additionally used below to illustrate the effect of different solvents on the thixotropic effect of polydimethyl decane.

在實施例32與33中,黏結劑溶液的配製方法同上述之實施例28,惟溶劑改為二元酸酯溶劑(DBE),且未添加松油醇。導電膠之配製步驟與方法同實施例28。觸變劑為添加0.40g或1.0g的聚二甲基矽烷-1,添加方法同前。 In Examples 32 and 33, the binder solution was prepared in the same manner as in Example 28 above except that the solvent was changed to a dibasic acid ester solvent (DBE), and no terpineol was added. The procedure and method for preparing the conductive paste were the same as those in Example 28. The thixotropic agent was added with 0.40 g or 1.0 g of polydimethylnonane-1 in the same manner as before.

在實施例34與35中,黏結劑溶液的配製方法同實施例32,惟溶劑改為二乙二醇單丁醚(BC)。導電膠之配製步驟與方法同實施例32。觸變劑為添加0.40g或1.0g的聚二甲基矽烷-1,添加方法同前。 In Examples 34 and 35, the binder solution was prepared in the same manner as in Example 32 except that the solvent was changed to diethylene glycol monobutyl ether (BC). The steps and methods for preparing the conductive paste were the same as those in Example 32. The thixotropic agent was added with 0.40 g or 1.0 g of polydimethylnonane-1 in the same manner as before.

在實施例36與37中,黏結劑溶液的配製方法同實施例32。導電膠之配製步驟與方法同實施例32。觸變劑為添加0.40g或1.0g的聚二甲基矽烷-2,添加方法同前。 In Examples 36 and 37, the binder solution was prepared in the same manner as in Example 32. The steps and methods for preparing the conductive paste were the same as those in Example 32. The thixotropic agent was added with 0.40 g or 1.0 g of polydimethylnonane-2 in the same manner as before.

在實施例38與39中,黏結劑溶液的配製方法同實施例32,惟溶劑改為二乙二醇單丁醚(BC)。導電膠之配製步驟與方法同實施例32。觸變劑為添加0.40g或1.0g的聚二甲基矽烷-2,添加方法同前。 In Examples 38 and 39, the binder solution was prepared in the same manner as in Example 32 except that the solvent was changed to diethylene glycol monobutyl ether (BC). The steps and methods for preparing the conductive paste were the same as those in Example 32. The thixotropic agent was added with 0.40 g or 1.0 g of polydimethylnonane-2 in the same manner as before.

下表2列示了實施例32~39之各項特性。 Table 2 below lists the characteristics of Examples 32-39.

在表2中,實施例32、33、36與37係採用二元酸酯溶劑(DBE)當溶劑,其閃火點為100℃。而實施例34、35、38與39係採二乙二醇單丁醚(BC)當溶劑,其閃火點為99℃。實施例32~39所製得之銀膠均以美國Brookfield公司所提供之黏度計DV-II+Pro viscometer cone/plate version在2rpm及27.0±0.5℃下測定。 In Table 2, Examples 32, 33, 36 and 37 used a dibasic acid ester solvent (DBE) as a solvent having a flash point of 100 °C. In Examples 34, 35, 38 and 39, diethylene glycol monobutyl ether (BC) was used as a solvent, and the flash point was 99 °C. The silver gums prepared in Examples 32 to 39 were all measured at 2 rpm and 27.0 ± 0.5 ° C using a viscometer DV-II + Pro viscometer cone/plate version supplied by Brookfield, U.S.A.

由表1可知,比較例1係未添加觸變劑的銀膠的配製方法,觸變係數僅達3.88。比較例2與3分別將聚醯胺(6500)與HCO(氫化箆麻油)添加於黏結劑溶液中,各配製成0.15%聚醯胺或HCO之銀膠,觸變係數分別提升至4.43與4.98。 As can be seen from Table 1, Comparative Example 1 is a method for preparing a silver paste to which no thixotropic agent is added, and the thixotropic coefficient is only 3.88. In Comparative Examples 2 and 3, polydecylamine (6500) and HCO (hydrogenated castor oil) were respectively added to the binder solution, and each was formulated into a silver paste of 0.15% polyamine or HCO, and the thixotropy coefficient was increased to 4.43 and 4.98.

實施例4~14依比較例1之方法配製後,分別添加0.033%~2.50%之聚二甲基矽烷-1,這些實施例之觸變 係數介於4.02~6.74之間,提高銀膠觸變性的效果非常顯著,且兼具提高潤滑作用,且配製之操作容易。 Examples 4 to 14 were prepared according to the method of Comparative Example 1, and 0.033% to 2.50% of polydimethylnonane-1 was added, respectively. The thixotropic of these examples The coefficient is between 4.02 and 6.74, and the effect of improving the thixotropy of the silver gel is very remarkable, and the lubrication effect is improved, and the preparation operation is easy.

實施例15~21之銀膠配製方法同實施例4,惟後續分別添加0.033%~2.5%之分子量較低的聚二甲基矽烷-2,這些實施例之觸變係數介於4.68~6.29之間。 The silver gums of Examples 15 to 21 were prepared in the same manner as in Example 4 except that 0.033% to 2.5% of the lower molecular weight polydimethylnonane-2 was added, and the thixotropic coefficients of these examples ranged from 4.68 to 6.29. between.

比較例22與23依比較例1配製銀膠時,在配製導電膠期間分別追加0.10g與0.20g的溶劑。配製完成後,再分別添加0.16%與0.63%的改質聚矽氧烷。比較例22與23之觸變係數分別為3.37與3.54,並無提高銀膠之觸變性的效果。 In Comparative Examples 22 and 23, when silver paste was prepared in accordance with Comparative Example 1, 0.10 g and 0.20 g of a solvent were added during the preparation of the conductive paste. After the preparation was completed, 0.16% and 0.63% of the modified polyoxyalkylene were separately added. The thixotropy coefficients of Comparative Examples 22 and 23 were 3.37 and 3.54, respectively, and did not improve the thixotropy of the silver paste.

比較例24與25依比較例1配製銀膠時,在配製導電膠期間分別追加0.20g的溶劑。配製完成後,再分別添加0.16%與0.63%的環氧基矽烷。比較例24與25之觸變係數分別為3.41與3.55,並無提高銀膠之觸變性的效果。 In Comparative Examples 24 and 25, when silver paste was prepared in accordance with Comparative Example 1, 0.20 g of a solvent was added during the preparation of the conductive paste. After the preparation was completed, 0.16% and 0.63% of epoxy decane were separately added. The thixotropic coefficients of Comparative Examples 24 and 25 were 3.41 and 3.55, respectively, and did not improve the thixotropy of the silver paste.

比較例26與27依比較例1配製銀膠時,在配製導電膠期間分別追加0.70g與1.20g的溶劑。配製完成後,再分別添加0.16%與0.63%的胺基矽烷。比較例26與27之觸變係數分別為3.43與2.59,並無提高銀膠之觸變性的效果。 In Comparative Examples 26 and 27, when silver paste was prepared according to Comparative Example 1, 0.70 g and 1.20 g of a solvent were added during the preparation of the conductive paste. After the preparation was completed, 0.16% and 0.63% of the amino decane were separately added. The thixotropic coefficients of Comparative Examples 26 and 27 were 3.43 and 2.59, respectively, and did not improve the thixotropy of the silver paste.

實施例28與29之黏結劑溶液之配製方法如比較例1,惟二乙二醇己醚(HC)與二乙二醇丁醚醋酸酯(BCA)之比例改為1:3,且未添加松油醇。分散劑改用1.0g之10%硬酯酸溶液,黏結劑溶液之用量改為4.60g。觸變劑為添加 0.40g與1.0g的聚二甲基矽烷-1。實施例28與29之觸變係數分別為6.39與6.34。 The preparation method of the binder solutions of Examples 28 and 29 was as in Comparative Example 1, except that the ratio of diethylene glycol hexyl ether (HC) to diethylene glycol butyl ether acetate (BCA) was changed to 1:3, and was not added. Terpineol. The dispersant was changed to 1.0 g of a 10% stearic acid solution, and the amount of the binder solution was changed to 4.60 g. Thixotropic agent is added 0.40 g and 1.0 g of polydimethylnonane-1. The thixotropic coefficients of Examples 28 and 29 were 6.39 and 6.34, respectively.

實施例30與31之配製方法如實施例28,惟觸變劑改為分別添加0.40g或1.0g的聚二甲基矽烷-2。實施例30與31之觸變係數分別為6.58與7.20。 The formulation methods of Examples 30 and 31 were as in Example 28 except that the thixotropic agent was changed to 0.40 g or 1.0 g of polydimethylnonane-2, respectively. The thixotropic coefficients of Examples 30 and 31 were 6.58 and 7.20, respectively.

此外,由表2可知,實施例32與33之黏結劑溶液的配製方法同實施例28,惟溶劑改為二元酸酯溶劑(DBE)且不加松油醇。導電膠之配製方法同實施例28。觸變劑分別添加0.40g或1.0g的聚二甲基矽烷-1,添加方法同前。實施例32與33之觸變係數分別為5.89與5.86。 Further, as is apparent from Table 2, the binder solutions of Examples 32 and 33 were prepared in the same manner as in Example 28 except that the solvent was changed to a dibasic acid ester solvent (DBE) and no terpineol was added. The conductive paste was prepared in the same manner as in Example 28. The thixotropic agent was added with 0.40 g or 1.0 g of polydimethylnonane-1, respectively, in the same manner as before. The thixotropic coefficients of Examples 32 and 33 were 5.89 and 5.86, respectively.

實施例36與37之導電膠之配製方法同實施例32,惟觸變劑分別添加0.40g或1.0g的聚二甲基矽烷-2,添加方法同前。實施例36與37之觸變係數分別為6.79與7.88。 The conductive pastes of Examples 36 and 37 were prepared in the same manner as in Example 32 except that the thixotropic agent was added with 0.40 g or 1.0 g of polydimethylnonane-2, respectively, in the same manner as before. The thixotropic coefficients of Examples 36 and 37 were 6.79 and 7.88, respectively.

實施例34與35之黏結劑溶液的配製方法同實施例28,惟溶劑改為二乙二醇單丁醚(BC)。導電膠之配製方法同實施例28。觸變劑分別添加0.40g或1.0g的聚二甲基矽烷-1。實施例34與35之觸變係數分別為5.24與5.23。 The binder solutions of Examples 34 and 35 were prepared in the same manner as in Example 28 except that the solvent was changed to diethylene glycol monobutyl ether (BC). The conductive paste was prepared in the same manner as in Example 28. The thixotropic agent was added with 0.40 g or 1.0 g of polydimethylnonane-1, respectively. The thixotropic coefficients of Examples 34 and 35 were 5.24 and 5.23, respectively.

實施例38與39之銀膠之配製方法同實施例34,惟觸變劑分別改為0.40g或1.0g的聚二甲基矽烷-2。實施例38與39之觸變係數分別為5.44與5.76。 The silver gums of Examples 38 and 39 were prepared in the same manner as in Example 34 except that the thixotropic agent was changed to 0.40 g or 1.0 g of polydimethylnonane-2, respectively. The thixotropic coefficients of Examples 38 and 39 were 5.44 and 5.76, respectively.

由上述之實施方式可知,本發明之優點就是因為本發明於配製銀膠時,在膠體混煉後,以少量逐次加入的方式添加液態的聚二甲基矽烷於膠體內,藉此不僅可有效提 高銀膠之觸變性,且可提供潤滑效果,更具有計量容易與作業方便等優勢。 It can be seen from the above embodiments that the present invention is advantageous in that, in the preparation of the silver paste, the liquid polydimethylsilane is added to the gel body in a small amount after the colloidal mixing, thereby being effective not only effective mention The high-silver gel is thixotropy and provides lubrication, and has the advantages of easy metering and convenient operation.

雖然本發明已以實施例揭露如上,然其並非用以限定本發明,任何在此技術領域中具有通常知識者,在不脫離本發明之精神和範圍內,當可作各種之更動與潤飾,因此本發明之保護範圍當視後附之申請專利範圍所界定者為準。 While the present invention has been described above by way of example, it is not intended to be construed as a limitation of the scope of the invention. Therefore, the scope of the invention is defined by the scope of the appended claims.

100‧‧‧步驟 100‧‧‧ steps

102‧‧‧步驟 102‧‧‧Steps

104‧‧‧步驟 104‧‧‧Steps

Claims (11)

一種銀膠,適用以製作一電極,該銀膠包含:一導電膠,包含:一黏結劑溶液,包含一溶質與一第一溶劑,其中該溶質包含乙基纖維素,且該第一溶劑可溶解該乙基纖維素,該黏結劑溶液之含量為7.0wt%至7.7wt%;一玻璃粉,混合於該黏結劑溶液中,其中該玻璃粉包含鉛、硼與矽,該玻璃粉之含量為4.2wt%至4.4wt%;一有機分散劑,混合於該黏結劑溶液中,其中該有機分散劑之含量為0.10wt%至0.35wt%;一第二溶劑,混合於該黏結劑溶液中,其中該第二溶劑含量為0wt%至2.0wt%;以及一銀粉,混合於該黏結劑溶液中,其中該銀粉之含量為84.3wt%至86.5wt%;以及一觸變劑,混合於該導電膠中,其中該觸變劑包含液態之聚二甲基矽烷,且該觸變劑之重量為該導電膠之總重量的0.02%至2.5%。 A silver paste suitable for forming an electrode, the silver paste comprising: a conductive paste comprising: a binder solution comprising a solute and a first solvent, wherein the solute comprises ethyl cellulose, and the first solvent is Dissolving the ethyl cellulose, the content of the binder solution is 7.0 wt% to 7.7% by weight; a glass frit mixed in the binder solution, wherein the glass frit contains lead, boron and antimony, the content of the glass frit Is from 4.2 wt% to 4.4 wt%; an organic dispersant mixed in the binder solution, wherein the content of the organic dispersant is from 0.10 wt% to 0.35 wt%; a second solvent is mixed in the binder solution Wherein the second solvent content is 0 wt% to 2.0 wt%; and a silver powder mixed in the binder solution, wherein the silver powder is contained in an amount of 84.3 wt% to 86.5 wt%; and a thixotropic agent is mixed in the In the conductive paste, wherein the thixotropic agent comprises liquid polydimethyl decane, and the thixotropic agent has a weight of 0.02% to 2.5% of the total weight of the conductive paste. 如申請專利範圍第1項之銀膠,其中該觸變劑為純的聚二甲基矽烷。 The silver gum of claim 1, wherein the thixotropic agent is pure polydimethyl decane. 如申請專利範圍第1項之銀膠,其中該溶質更包含一潤滑劑。 The silver paste of claim 1, wherein the solute further comprises a lubricant. 如申請專利範圍第1項之銀膠,其中該第一溶劑與該第二溶劑包含二乙二醇己醚(HC)溶劑與二乙二醇丁醚醋酸酯(BCA)溶劑。 The silver paste of claim 1, wherein the first solvent and the second solvent comprise a diethylene glycol hexyl ether (HC) solvent and a diethylene glycol butyl ether acetate (BCA) solvent. 如申請專利範圍第4項之銀膠,其中該第一溶劑更包含松油醇。 The silver paste of claim 4, wherein the first solvent further comprises terpineol. 如申請專利範圍第1項之銀膠,其中該第一溶劑包含二元酸酯溶劑(DBE)或二乙二醇單丁醚(BC)。 The silver paste of claim 1, wherein the first solvent comprises a dibasic acid ester solvent (DBE) or diethylene glycol monobutyl ether (BC). 一種銀膠之製造方法,包含:配製一黏結劑溶液,以將一溶質溶解於一第一溶劑中,其中該溶質包含乙基纖維素;配製一導電膠,其中配製該導電膠之步驟包含:混合一玻璃粉與一有機分散劑,以形成一混合物,其中該玻璃粉之含量為4.2wt%至4.4wt%,該有機分散劑之含量為0.10wt%至0.35wt%,且該玻璃粉包含鉛、硼與矽;將一第二溶劑與該黏結劑溶液加入該混合物中,其中該黏結劑溶液之含量為7.0wt%至7.7wt%,該第二溶劑含量為0wt%至2.0wt%;以及將一銀粉加入混有該第二溶劑與該黏結劑溶液之該混合物中,其中該銀粉之含量為84.3wt%至86.5wt%;以及 將一觸變劑加入該導電膠中,其中該觸變劑包含液態之聚二甲基矽烷,且該觸變劑之重量為該導電膠之總重量的0.02%至2.5%。 A method for producing a silver paste, comprising: preparing a binder solution to dissolve a solute in a first solvent, wherein the solute comprises ethyl cellulose; preparing a conductive paste, wherein the step of preparing the conductive paste comprises: Mixing a glass frit with an organic dispersant to form a mixture, wherein the content of the glass frit is from 4.2 wt% to 4.4 wt%, the content of the organic dispersant is from 0.10 wt% to 0.35 wt%, and the glass frit comprises Lead, boron and bismuth; a second solvent and the binder solution are added to the mixture, wherein the binder solution is contained in an amount of 7.0 wt% to 7.7% by weight, and the second solvent content is 0 wt% to 2.0 wt%; And adding a silver powder to the mixture in which the second solvent and the binder solution are mixed, wherein the content of the silver powder is from 84.3 wt% to 86.5 wt%; A thixotropic agent is added to the conductive paste, wherein the thixotropic agent comprises liquid polydimethyl decane, and the thixotropic agent has a weight of 0.02% to 2.5% of the total weight of the conductive paste. 如申請專利範圍第7項之銀膠之製造方法,其中該觸變劑為純的聚二甲基矽烷。 The method for producing a silver paste according to claim 7, wherein the thixotropic agent is pure polydimethylsilane. 如申請專利範圍第7項之銀膠之製造方法,其中該第一溶劑與該第二溶劑包含二乙二醇己醚(HC)溶劑與二乙二醇丁醚醋酸酯(BCA),且在該第一溶劑與該第二溶劑中,該二乙二醇己醚(HC)溶劑與該二乙二醇丁醚醋酸酯(BCA)之重量比為1:1。 The method for producing a silver paste according to claim 7, wherein the first solvent and the second solvent comprise diethylene glycol hexyl ether (HC) solvent and diethylene glycol butyl ether acetate (BCA), and In the first solvent and the second solvent, the weight ratio of the diethylene glycol hexyl ether (HC) solvent to the diethylene glycol butyl ether acetate (BCA) is 1:1. 如申請專利範圍第7項之銀膠之製造方法,其中於將該銀粉加入混有該第二溶劑與該黏結劑溶液之該混合物中後,配製該導電膠之步驟更包含利用一三滾筒進行複數個混煉處理。 The method for producing a silver paste according to claim 7 , wherein after the silver powder is added to the mixture in which the second solvent and the binder solution are mixed, the step of preparing the conductive paste further comprises using a three-roller Multiple mixing processes. 如申請專利範圍第10項之銀膠之製造方法,其中將該觸變劑加入該導電膠之步驟包含:降低該三滾筒之轉速;在該導電膠於該三滾筒中時,分批加入該觸變劑;以及於該觸變劑加入該導電膠後,利用該三滾筒進行複數個再次混煉處理。 The method for manufacturing a silver paste according to claim 10, wherein the step of adding the thixotropic agent to the conductive paste comprises: reducing a rotation speed of the three rollers; and adding the conductive paste to the three rollers in batches a thixotropic agent; and after the thixotropic agent is added to the conductive paste, a plurality of re-kneading processes are performed using the three rollers.
TW104111661A 2015-04-10 2015-04-10 Silver paste and method for manufacturing the same TWI555035B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
TW104111661A TWI555035B (en) 2015-04-10 2015-04-10 Silver paste and method for manufacturing the same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
TW104111661A TWI555035B (en) 2015-04-10 2015-04-10 Silver paste and method for manufacturing the same

Publications (2)

Publication Number Publication Date
TW201637026A TW201637026A (en) 2016-10-16
TWI555035B true TWI555035B (en) 2016-10-21

Family

ID=57847709

Family Applications (1)

Application Number Title Priority Date Filing Date
TW104111661A TWI555035B (en) 2015-04-10 2015-04-10 Silver paste and method for manufacturing the same

Country Status (1)

Country Link
TW (1) TWI555035B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112037959A (en) * 2020-09-01 2020-12-04 深圳纳弘熠岦光学科技有限公司 Silver paste, silver paste preparation method and solar cell grid line

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TW201412903A (en) * 2012-08-16 2014-04-01 Cima Nanotech Israel Ltd Emulsions for preparing transparent conductive coatings
TW201415491A (en) * 2012-02-28 2014-04-16 Cima Nanotech Israel Ltd Transparent conductive coatings on an elastomeric substrate
TW201425342A (en) * 2012-10-15 2014-07-01 Dow Global Technologies Llc Conductive composition
TW201435927A (en) * 2013-01-22 2014-09-16 Dongjin Semichem Co Ltd Transparent conductive film coating composition, transparent conductive film, and method for manufacturing transparent conductive film
TW201511398A (en) * 2013-07-17 2015-03-16 Nthdegree Tech Worldwide Inc Energy storage device, ink for an electrode of an energy storage device and method of manufacturing an energy storage device

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TW201415491A (en) * 2012-02-28 2014-04-16 Cima Nanotech Israel Ltd Transparent conductive coatings on an elastomeric substrate
TW201412903A (en) * 2012-08-16 2014-04-01 Cima Nanotech Israel Ltd Emulsions for preparing transparent conductive coatings
TW201425342A (en) * 2012-10-15 2014-07-01 Dow Global Technologies Llc Conductive composition
TW201435927A (en) * 2013-01-22 2014-09-16 Dongjin Semichem Co Ltd Transparent conductive film coating composition, transparent conductive film, and method for manufacturing transparent conductive film
TW201511398A (en) * 2013-07-17 2015-03-16 Nthdegree Tech Worldwide Inc Energy storage device, ink for an electrode of an energy storage device and method of manufacturing an energy storage device

Also Published As

Publication number Publication date
TW201637026A (en) 2016-10-16

Similar Documents

Publication Publication Date Title
TWI455328B (en) Paste for producing electrode of solar cell
CN106098138B (en) Conductive paste and method for manufacturing solar cell using the same
CN104741821B (en) A kind of preparation method for the micro-nano copper of electronic module High-temperature Packaging particles filled Sn base soldering paste
CN103400634B (en) A kind of crystal silicon solar energy battery front electrode conductive silver paste and preparation method thereof
TWI576863B (en) A conductive paste containing lead-free glass frit
WO2006126499A1 (en) Conductive paste and wiring board using it
CN102034877A (en) Conductive paste for solar cell and preparation method thereof
JP2007019106A (en) Conductive paste for forming electrode, and photovoltaic cell
CN110714133B (en) Silver palladium alloy powder for conductive composition and preparation method thereof
KR101434167B1 (en) Silver paste composition used in the preparation of an electrode for a solar cell
TWI591652B (en) A conductive paste containing lead-free glass frit
CN106928605A (en) A kind of organic carrier for solar cell positive silver paste and preparation method thereof
JP5934411B1 (en) Conductive paste containing lead-free glass frit
CN106601327B (en) Low solvent volatility conductive slurry for front electrode of solar battery and preparation method
TW201515012A (en) A conductive paste containing lead-free glass frit
TWI555035B (en) Silver paste and method for manufacturing the same
JPH1098242A (en) Silver composition cleanable with water
TWI687401B (en) Nickel paste and manufacturing method of nickel paste
JP6042932B2 (en) Conductive paste containing lead-free glass frit
WO2021125161A1 (en) Silver paste, method for producing same, and method for producing jointed article
TW457495B (en) Method for manufacturing paste for electroconductive thick film, paste for electroconductive thick film and laminated ceramic electronic part
CN106128551A (en) A kind of high efficiency water runs through wiring board conductive silver paste and preparation method thereof
JP2001006436A (en) Conductive paste and manufacture thereof and laminated ceramic capacitor using the same
JP6947280B2 (en) Silver paste and its manufacturing method and joint manufacturing method
CN1189893C (en) Conductive pasty material, method for controlling its viscosity and electronic component using same

Legal Events

Date Code Title Description
MM4A Annulment or lapse of patent due to non-payment of fees