TW201318734A - A simple method for producing micro silver-copper composite powder - Google Patents
A simple method for producing micro silver-copper composite powder Download PDFInfo
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- TW201318734A TW201318734A TW100139712A TW100139712A TW201318734A TW 201318734 A TW201318734 A TW 201318734A TW 100139712 A TW100139712 A TW 100139712A TW 100139712 A TW100139712 A TW 100139712A TW 201318734 A TW201318734 A TW 201318734A
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- 239000000843 powder Substances 0.000 title claims abstract description 40
- NEIHULKJZQTQKJ-UHFFFAOYSA-N [Cu].[Ag] Chemical compound [Cu].[Ag] NEIHULKJZQTQKJ-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 35
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 claims abstract description 15
- 229910000367 silver sulfate Inorganic materials 0.000 claims abstract description 15
- 239000001509 sodium citrate Substances 0.000 claims abstract description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000035484 reaction time Effects 0.000 claims abstract 2
- 239000002245 particle Substances 0.000 claims description 18
- 239000000725 suspension Substances 0.000 claims description 15
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 230000005070 ripening Effects 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 21
- 238000000034 method Methods 0.000 abstract description 19
- 229910052709 silver Inorganic materials 0.000 abstract description 17
- 239000004332 silver Substances 0.000 abstract description 17
- 229910052802 copper Inorganic materials 0.000 abstract description 13
- 239000010949 copper Substances 0.000 abstract description 13
- 238000001914 filtration Methods 0.000 abstract description 5
- 239000000243 solution Substances 0.000 abstract 2
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 abstract 2
- 229940038773 trisodium citrate Drugs 0.000 abstract 2
- 239000012047 saturated solution Substances 0.000 abstract 1
- 239000002105 nanoparticle Substances 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 5
- 239000002923 metal particle Substances 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000000599 controlled substance Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- JKNZUZCGFROMAZ-UHFFFAOYSA-L [Ag+2].[O-]S([O-])(=O)=O Chemical class [Ag+2].[O-]S([O-])(=O)=O JKNZUZCGFROMAZ-UHFFFAOYSA-L 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- IBOFVQJTBBUKMU-UHFFFAOYSA-N 4,4'-methylene-bis-(2-chloroaniline) Chemical compound C1=C(Cl)C(N)=CC=C1CC1=CC=C(N)C(Cl)=C1 IBOFVQJTBBUKMU-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000003094 microcapsule Substances 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- OGFYIDCVDSATDC-UHFFFAOYSA-N silver silver Chemical compound [Ag].[Ag] OGFYIDCVDSATDC-UHFFFAOYSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 description 1
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- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
Description
本發明係關於一種銀銅複合粉的製作方式，特別是一種對環境較無害且適合放大規模生產的製作程序。The invention relates to a method for preparing a silver-copper composite powder, in particular to a production process which is harmless to the environment and suitable for scale-up production.
微米以及奈米金屬粒子的合成方式，在近幾十年來被廣泛的研究與探討，而一般可將其分為液相、氣相與固相法三大類。其中以液相法合成奈米金屬粒子方面，由於有著相較於氣相及固相法在設置成本上的優勢，故本發明係以液相化學法作為次微米與奈米級銅粉的製作方式。The synthesis of micron and nano metal particles has been extensively studied and discussed in recent decades, and can be generally divided into three categories: liquid phase, gas phase and solid phase method. Among them, the synthesis of nano metal particles by liquid phase method has the advantage of setting cost compared with gas phase and solid phase method, so the present invention uses liquid phase chemical method as the production of submicron and nano copper powder. the way.
在中華民國專利公告I279269號「含有奈米金屬之微胞溶液及其製造方法」中，乃是提及一種利用微胞法或逆微胞法製造奈米金屬聚合體之方式；另中華民國專利公告I280949號「金屬奈米粒子之製造方法」中，主要提到一種利用生物法並透過植物光合作用製造奈米金屬之方式；此外中華民國專利公告I290930號「製備奈米微粒的方法」中，主要提及到以模板法進行奈米金屬之製作；而中華民國專利公告I304101號「金屬奈米粒子之製造方法」中，其特點在於以電化學之型式並添加界面活性劑製作棒狀奈米金屬粒子；而中華民國專利公告I307646號「核-殼型奈米粒子及其製備方法」中，主要探討的內容為核-殼型奈米粒子之製備方式；另中華民國專利公告I307640號「利用奈米級粉末之成形方法」中，主要討論的為奈米金屬粒子後端的應用部分；中華民國專利公告201024004號「含有銅之銀粒子及其製造方法暨使用其等之分散液」中，主要針對奈米銀金屬粒子之合成進行討論，其中該法所合成之奈米銀顆粒中雖含有約1~1000ppm之銅成分，但其添加銅之主要目的為增進銀顆粒的均勻性；中華民國專利公告I304003號「微粒銀粒子附著銀銅複合粉及此微粒銀粒子附著銀銅複合粉之製造方法」中，主要介紹以管制藥品的強還原劑聯胺製造出含銀量介於約30~70%之鍍銀銀銅粉；另中華民國專利公告200925291號「奈米銀銅合金漿液及奈米銀銅合金粉末之製備方法」中，主要介紹於初始溶液中同時添加銀鹽與銅鹽，再搭配昂貴之高分子保護劑以產生奈米級的銀銅合金粉末；另中華民國專利公告200831214號「鍍銀之銅微粉末、使用鍍銀之銅微粉末所製造之導電糊、及鍍銀之銅微粉末之製造方法」中，介紹了利用表面處理藥劑增進鍍銀效率之方式，透過多次的酸洗與鹼洗後，再於鍍銀程序後於還原氣氛下進行鍛燒程序，最後得到一鍍銀銅粉。In the Republic of China Patent Publication No. I279269, "Microcapsule Solution Containing Nano Metals and Its Manufacturing Method", a method of manufacturing a nano metal polymer by a microcell method or an inverse microcell method is mentioned, and a patent of the Republic of China is also provided. Announcement No. I280949 "Manufacturing Method of Metallic Nanoparticles" mainly refers to a method of producing nano-metals by using biological methods and by plant photosynthesis; in addition, in the method of preparing nanoparticles, the Republic of China Patent Publication No. I290930, It is mainly mentioned that the production of nano-metals by the stencil method; and the method of manufacturing the metal nano-particles of the Republic of China Patent Publication No. I304101 is characterized in that the rod-shaped nano-particles are prepared by electrochemical type and adding a surfactant. Metal particles; and in the Republic of China Patent Publication No. I307646 "Nuclear-shell type nanoparticle and its preparation method", the main content of the discussion is the preparation of core-shell type nanoparticles; and the Republic of China Patent Notice No. I307640 "Usage In the method of forming nano-sized powders, the main part is the application part of the back end of nano metal particles; the Republic of China patent announcement 20102400 No. 4 "Silver-containing silver particles and a method for producing the same, and a dispersion thereof," mainly discusses the synthesis of nano-silver metal particles, wherein the nano silver particles synthesized by the method contain about 1~ 1000 ppm of copper component, but the main purpose of adding copper is to improve the uniformity of silver particles; Chinese Patent Publication No. I304003 "Manufacturing method of silver-silver composite powder with particulate silver particles and silver-copper composite powder with silver particles attached thereto" It mainly introduces silver-plated silver-copper powder with a silver content of about 30~70% with the strong reducing agent bisamine of controlled drugs; another Republic of China Patent Announcement 200925291 "Nano silver-copper alloy slurry and nano silver copper In the preparation method of the alloy powder, the silver salt and the copper salt are simultaneously added to the initial solution, and the expensive polymer protective agent is used to produce the nano-scale silver-copper alloy powder; and the Republic of China Patent Publication No. 200831214 In the method for producing silver-based fine powder of silver, a conductive paste made of silver-plated copper micro-powder, and a silver-plated copper micropowder, a method for improving the silver plating efficiency by using a surface treatment agent is described. After pickling and alkaline cleaning through a plurality of times, and then silver-plated in a reducing atmosphere after application program calcined finally obtain a silver plated copper powder.
綜合上述，先前之技術皆與本發明所運用之生產方法有所差異，上述專利所提之製造程序不僅較為繁雜，其中部分亦運用了管制藥品。In summary, the prior art is different from the production method used in the present invention, and the manufacturing procedures mentioned in the above patents are not only complicated, but some of them also use controlled drugs.
本發明係有關一種製作銀銅複合粉(silver-copper composite powder)的方式，首先配置含有0.01~0.45 Wt%、純度為99%以上檸檬酸鈉，與0.1~10 Wt%、中位粒徑(D50)<10μm、純度為99.5%以上之純銅粉懸浮液，並控制攪拌速率為100~1200RPM以保持銅粉顆粒間之分散，在另外配置飽和濃度0.015 M的硫酸銀溶液並於其中分別加入0.05~1 Vol.%且濃度為35%之氫氧化銨與0.05~5 Wt.%且純度為99%以上之檸檬酸鈉，待純銅粉懸浮液與硫酸銀溶液皆配置完成後，將配置好的硫酸銀溶液加入純銅粉懸浮液中，在溫度30~120℃之條件下持續反應5~60分鐘後，利用過濾的方式將液體與銀銅複合粉分開，接著將所得之銀銅複合粉以去離子水清洗2~8次後，再經過0.5~8小時、80~130℃之乾燥製程，最後即可得到粒徑大小分佈均勻的銀銅複合粉產品(粒徑範圍：0.1～10μm)。The invention relates to a method for preparing a silver-copper composite powder, which firstly comprises 0.01 to 0.45 Wt%, a purity of 99% or more of sodium citrate, and 0.1 to 10 Wt%, a median diameter ( D 50 )<10μm, purity of 99.5% or more pure copper powder suspension, and control the stirring rate of 100~1200RPM to maintain the dispersion between the copper powder particles, in addition to a saturated concentration of 0.015 M silver sulfate solution and separately added 0.05~1 Vol.% of ammonium citrate with a concentration of 35% ammonium hydroxide and 0.05~5 Wt.% and a purity of 99% or more. After the pure copper powder suspension and the silver sulfate solution are all configured, they will be properly configured. The silver sulfate solution is added to the pure copper powder suspension, and the reaction is continued for 5 to 60 minutes at a temperature of 30 to 120 ° C, and then the liquid and the silver-copper composite powder are separated by filtration, and then the obtained silver-copper composite powder is After cleaning with deionized water for 2 to 8 times, the drying process of 0.5 to 8 hours and 80 to 130 ° C is carried out, and finally a silver-copper composite powder product having a uniform particle size distribution (particle size range: 0.1 to 10 μm) can be obtained.
本發明之實施方法示於第一圖，以下針對幾種配比之方式進行實施方法之說明，另表1為針對本專利所合成之銀銅複合粉產品與市售純銀產品(瑞士Metalor)之比較，其中比電阻之測試程序為，將不同之粉末以50%固含量調入一特定膠體中，經調膠後均勻塗佈於玻璃機版上後，以100℃烘乾10分鐘後，再以微電阻計測得之比電阻數值。The method for carrying out the invention is shown in the first figure. The following describes the implementation method for several ratios. The other Table 1 is for the silver-copper composite powder product synthesized by the patent and the commercially available pure silver product (Metalor, Switzerland). In comparison, the specific resistance test procedure is: the different powders are transferred into a specific colloid at a solid content of 50%, uniformly coated on a glass plate after being adjusted, and then dried at 100 ° C for 10 minutes, and then The specific resistance value measured by a micro-resistance meter.
首先配置10 L含有0.01~0.45 Wt%(較佳為0.05~0.18 Wt%，更佳為0.09 Wt%)、純度為99%以上檸檬酸鈉，與0.1~10 Wt%(較佳為0.5~5 Wt%，更佳為2.5 Wt%)、中位粒徑(D50)<10μm、純度為99.5%以上之純銅粉懸浮液11，並控制攪拌速率為100~1200RPM(較佳為300~600 RPM)以保持銅粉顆粒間之分散，在另外配置34 L飽和濃度0.015 M的硫酸銀溶液12並於其中分別加入0.05~1 Vol.%(較佳為0.1~0.25 Vol.%，更佳為0.125 Vol.%)且濃度為35%之氫氧化銨與0.05~5 Wt.%(較佳為0.1~2.5 Wt%，更佳為0.25~1 Wt%)且純度為99%以上之檸檬酸鈉，待純銅粉懸浮液11與硫酸銀溶液12皆配置完成後，將配置好的硫酸銀溶液12加入純銅粉懸浮液11中，在溫度控制2於30~120℃(較佳為40~100℃，更佳為70~80℃)之條件下進行熟化反應3約5~60分鐘(較佳為10~30℃)後，經過濾程序4將液體與銀銅複合粉41分開，接著將所得之銀銅複合粉41透過表面清洗程序5以去離子水清洗2~8次(較佳為4次)後，再經乾燥程序6以0.5~8小時(較佳為1~2小時)、80~130℃進行粉體乾燥後，最終即可得到粒徑大小分佈均勻的且銀銅比例為37：63之銀銅複合粉產品7(粒徑範圍：0.1～10μm)。First, 10 L is contained in a range of 0.01 to 0.45 Wt% (preferably 0.05 to 0.18 Wt%, more preferably 0.09 Wt%), and the purity is 99% or more of sodium citrate, and 0.1 to 10 Wt% (preferably 0.5 to 5). Wt%, more preferably 2.5 Wt%), a pure copper powder suspension having a median diameter (D 50 ) < 10 μm and a purity of 99.5% or more, and controlling the stirring rate to be 100 to 1200 RPM (preferably 300 to 600 RPM). In order to maintain the dispersion between the copper powder particles, a 34 L saturated silver sulfate solution of 0.015 M is additionally disposed and 0.05 to 1 Vol.% (preferably 0.1 to 0.25 Vol.%, more preferably 0.125) is separately added thereto. Vol.%) sodium citrate having a concentration of 35% ammonium hydroxide and 0.05 to 5 Wt.% (preferably 0.1 to 2.5 Wt%, more preferably 0.25 to 1 Wt%) and a purity of 99% or more. After the pure copper powder suspension 11 and the silver sulfate solution 12 are all disposed, the silver sulfate solution 12 is added to the pure copper powder suspension 11 at a temperature of 2 to 30 to 120 ° C (preferably 40 to 100 ° C, More preferably, the aging reaction is carried out for 3 to 60 minutes (preferably 10 to 30 ° C) under the condition of 70 to 80 ° C), and the liquid is separated from the silver-copper composite powder 41 by the filtration procedure 4, and then the obtained silver is obtained. Copper composite powder 41 passes through surface cleaning program 5 with deionized water After washing 2 to 8 times (preferably 4 times), the powder is dried by drying procedure 6 for 0.5 to 8 hours (preferably 1 to 2 hours) and 80 to 130 ° C, and finally the particle size is obtained. A silver-copper composite powder product 7 having a uniform size distribution and a silver-copper ratio of 37:63 (particle size range: 0.1 to 10 μm).
首先配置10 L含有0.01~0.45 Wt%(較佳為0.05~0.18 Wt%，更佳為0.09 Wt%)、純度為99%以上檸檬酸鈉，與0.1~10 Wt%(較佳為0.5~5 Wt%，更佳為2.5 Wt%)、中位粒徑(D50)<10μm、純度為99.5%以上之純銅粉懸浮液11，並控制攪拌速率為100~1200RPM(較佳為300~600 RPM)以保持銅粉顆粒間之分散，在另外配置53 L飽和濃度0.015 M的硫酸銀溶液12並於其中分別加入0.05~1 Vol.%(較佳為0.1~0.25 Vol.%，更佳為0.125 Vol.%)且濃度為35%之氫氧化銨與0.05~5 Wt.%(較佳為0.1~2.5 Wt%，更佳為0.25~1 Wt%)且純度為99%以上之檸檬酸鈉，待純銅粉懸浮液11與硫酸銀溶液12皆配置完成後，將配置好的硫酸銀溶液12加入純銅粉懸浮液11中，在溫度控制2於30~120℃(較佳為40~100℃，更佳為70~80℃)之條件下進行熟化反應3約5~60分鐘(較佳為10~30℃)後，經過濾程序4將液體與銀銅複合粉41分開，接著將所得之銀銅複合粉41透過表面清洗程序5以去離子水清洗2~8次(較佳為4次)後，再經乾燥程序6以0.5~8小時(較佳為1~2小時)、80~130℃進行粉體乾燥後，最終即可得到粒徑大小分佈均勻的且銀銅比例為53：47之銀銅複合粉產品7(粒徑範圍：0.1～10μm)。First, 10 L is contained in a range of 0.01 to 0.45 Wt% (preferably 0.05 to 0.18 Wt%, more preferably 0.09 Wt%), and the purity is 99% or more of sodium citrate, and 0.1 to 10 Wt% (preferably 0.5 to 5). Wt%, more preferably 2.5 Wt%), a pure copper powder suspension having a median diameter (D 50 ) < 10 μm and a purity of 99.5% or more, and controlling the stirring rate to be 100 to 1200 RPM (preferably 300 to 600 RPM). In order to maintain the dispersion between the copper powder particles, a 53 L saturated silver sulfate solution of 0.015 M is additionally disposed and 0.05 to 1 Vol.% (preferably 0.1 to 0.25 Vol.%, more preferably 0.125) is separately added thereto. Vol.%) sodium citrate having a concentration of 35% ammonium hydroxide and 0.05 to 5 Wt.% (preferably 0.1 to 2.5 Wt%, more preferably 0.25 to 1 Wt%) and a purity of 99% or more. After the pure copper powder suspension 11 and the silver sulfate solution 12 are all disposed, the silver sulfate solution 12 is added to the pure copper powder suspension 11 at a temperature of 2 to 30 to 120 ° C (preferably 40 to 100 ° C, More preferably, the aging reaction is carried out for 3 to 60 minutes (preferably 10 to 30 ° C) under the condition of 70 to 80 ° C), and the liquid is separated from the silver-copper composite powder 41 by the filtration procedure 4, and then the obtained silver is obtained. Copper composite powder 41 passes through surface cleaning program 5 with deionized water After washing 2 to 8 times (preferably 4 times), the powder is dried by drying procedure 6 for 0.5 to 8 hours (preferably 1 to 2 hours) and 80 to 130 ° C, and finally the particle size is obtained. A silver-copper composite powder product 7 having a uniform size distribution and a ratio of silver to copper of 53:47 (particle size range: 0.1 to 10 μm).
首先配置10 L含有0.01~0.45 Wt%(較佳為0.05~0.18 Wt%，更佳為0.09 Wt%)、純度為99%以上檸檬酸鈉，與0.1~10 Wt%(較佳為0.5~5 Wt%，更佳為2.5 Wt%)、中位粒徑(D50)<10μm、純度為99.5%以上之純銅粉懸浮液11，並控制攪拌速率為100~1200RPM(較佳為300~600 RPM)以保持銅粉顆粒間之分散，在另外配置120 L飽和濃度0.015 M的硫酸銀溶液12並於其中分別加入0.05~1 Vol.%(較佳為0.1~0.25 Vol.%，更佳為0.125 Vol.%)且濃度為35%之氫氧化銨與0.05~5 Wt.%(較佳為0.1~2.5 Wt%，更佳為0.25~1 Wt%)且純度為99%以上之檸檬酸鈉，待純銅粉懸浮液11與硫酸銀溶液12皆配置完成後，將配置好的硫酸銀溶液12加入純銅粉懸浮液11中，在溫度控制2於30~120℃(較佳為40~100℃，更佳為70~80℃)之條件下進行熟化反應3約5~60分鐘(較佳為10~30℃)後，經過濾程序4將液體與銀銅複合粉41分開，接著將所得之銀銅複合粉41透過表面清洗程序5以去離子水清洗2~8次(較佳為4次)後，再經乾燥程序6以0.5~8小時(較佳為1~2小時)、80~130℃進行粉體乾燥後，最終即可得到粒徑大小分佈均勻的且銀銅比例為73：27之銀銅複合粉產品7(粒徑範圍：0.1～10μm)。First, 10 L is contained in a range of 0.01 to 0.45 Wt% (preferably 0.05 to 0.18 Wt%, more preferably 0.09 Wt%), and the purity is 99% or more of sodium citrate, and 0.1 to 10 Wt% (preferably 0.5 to 5). Wt%, more preferably 2.5 Wt%), a pure copper powder suspension having a median diameter (D 50 ) < 10 μm and a purity of 99.5% or more, and controlling the stirring rate to be 100 to 1200 RPM (preferably 300 to 600 RPM). In order to maintain the dispersion between the copper powder particles, 120 L of a silver sulfate solution 12 having a saturated concentration of 0.015 M is additionally disposed and 0.05 to 1 Vol.% (preferably 0.1 to 0.25 Vol.%, more preferably 0.125) is separately added thereto. Vol.%) sodium citrate having a concentration of 35% ammonium hydroxide and 0.05 to 5 Wt.% (preferably 0.1 to 2.5 Wt%, more preferably 0.25 to 1 Wt%) and a purity of 99% or more. After the pure copper powder suspension 11 and the silver sulfate solution 12 are all disposed, the silver sulfate solution 12 is added to the pure copper powder suspension 11 at a temperature of 2 to 30 to 120 ° C (preferably 40 to 100 ° C, More preferably, the aging reaction is carried out for 3 to 60 minutes (preferably 10 to 30 ° C) under the condition of 70 to 80 ° C), and the liquid is separated from the silver-copper composite powder 41 by the filtration procedure 4, and then the obtained silver is obtained. Copper composite powder 41 is deionized by surface cleaning procedure 5 After washing 2 to 8 times (preferably 4 times), the powder is dried by drying procedure 6 for 0.5 to 8 hours (preferably 1 to 2 hours) and 80 to 130 ° C, and finally the particle size is obtained. A silver-copper composite powder product 7 having a uniform size distribution and a ratio of silver to copper of 73:27 (particle size range: 0.1 to 10 μm).
為使本發明更加顯現出其在工業上之實用性，茲將本發明之優點列舉如下：In order to make the present invention more apparent in its industrial applicability, the advantages of the present invention are enumerated as follows:
1. 本發明不需添加管制之藥品。1. The invention does not require the addition of controlled drugs.
2. 本發明之操作程序簡單。2. The operating procedure of the present invention is simple.
3. 本發明之產品價格相較銀粉低廉許多深具市場競爭力。3. The price of the product of the invention is much less competitive than the silver powder.
4. 本發明深具量化生產之潛力。4. The invention has the potential to quantify production.
5. 本發明之銀銅複合粉產品可供PCB版、導電膠、導電膏與其他需使用此規格銀銅複合粉之製造業者另一經濟便宜之導電材料來源。5. The silver-copper composite powder product of the invention can be used as a cheap source of conductive materials for PCB plates, conductive adhesives, conductive pastes and other manufacturers who need to use silver-copper composite powder of this specification.
6. 本發明可依據不同產業所求製作出不同比例之銀銅複合粉具產業界上利用價值。6. The invention can produce the utilization value of the silver-copper composite powder with different proportions according to different industries.
綜上所述，本發明誠已符合發明專利之申請要件，並依法提出申請，祈請 鈞局審查委員明鑑，並賜予本發明專利權，實感德便。In summary, the invention has met the application requirements of the invention patent, and filed an application according to law, praying for the examination of the member of the bureau, and granting the patent right of the invention.
11．．．純銅粉懸浮液11. . . Pure copper powder suspension
12．．．硫酸銀溶液12. . . Silver sulfate solution
2．．．溫度控制程序2. . . Temperature control program
3．．．熟化反應3. . . Ripening reaction
4．．．過濾程序4. . . Filter
41．．．銀銅複合粉41. . . Silver-copper composite powder
5．．．表面清洗程序5. . . Surface cleaning program
51．．．清洗後之銀銅複合粉51. . . Silver-copper composite powder after cleaning
6．．．乾燥程序6. . . Drying procedure
7．．．銀銅複合粉產品7. . . Silver-copper composite powder products
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI609381B (en) * | 2016-02-02 | 2017-12-21 | 國立成功大學 | Method of fabricating high-conductivity thick-film copper paste coated with nano-silver for being sintered in the air |
| CN113593772A (en) * | 2021-07-27 | 2021-11-02 | 哈尔滨工业大学（深圳） | Nano silver-copper solid solution and preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI609381B (en) * | 2016-02-02 | 2017-12-21 | 國立成功大學 | Method of fabricating high-conductivity thick-film copper paste coated with nano-silver for being sintered in the air |
| CN113593772A (en) * | 2021-07-27 | 2021-11-02 | 哈尔滨工业大学（深圳） | Nano silver-copper solid solution and preparation method and application thereof |
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