本文選題：超細銅粉 + 銅鹽��； 參考：《昆明理工大學》2017年碩士論文

【摘要】：超細銅粉由于具有小尺寸效應、表面界面效應、量子尺度效應和量子隧道效應等基本特征,因此在力學、電學、化學等領域有許多優(yōu)勢。本論文采用液相兩步還原法來制備超細銅粉,首先采用葡萄糖預還原制得氧化亞銅,然后選用其它還原劑進行二次還原制得超細銅粉。實驗設計兩條技術路線:一條是選用不同銅鹽(乙酸銅、氯化銅、硫酸銅和硝酸銅)制得C1、C2、C3和C4超細銅粉;另一條是選用不同二次還原劑(水合肼、次亞磷酸鈉、抗壞血酸和硼氫化鈉)制備出C5、C6、C7和C8超細銅粉,然后對超細銅粉元素種類、微觀形貌、粒徑分布、松裝密度以及導電性進行表征,從中選擇較佳銅鹽和二次還原劑。研究結果表明:當銅鹽選用硫酸銅時制得C3銅粉為類球形,粒徑分布相對均勻,松裝密度最大可達1.65 g/cm3,電阻最小為0.037Ω;當選擇水合肼為二次還原劑時,制得C5銅粉為球形,粒徑分布均勻,平均粒徑為1.89μm,松裝密度最大可達1.78 g/cm3,電阻最小為6.71mΩ,這為制備抗氧化超細銅粉提供了科學依據(jù)。以銅粉、玻璃粉和有機載體為原料可制備銅導體漿料,經(jīng)過研磨、絲網(wǎng)印刷、流平、烘干、燒結等工藝,可在陶瓷基片上制得銅膜,廣泛應用于現(xiàn)代化技術領域。玻璃粉作為銅導體漿料中不可或缺的一部分,在銅漿燒結時與銅顆粒形成網(wǎng)絡狀結構組織,調(diào)節(jié)銅漿熱膨脹系數(shù),并滿足電極和基板粘結強度要求,因此玻璃粉組成及其含量對銅膜微觀形貌、導電性、附著力、抗氧化性和抗老化性能有重要影響。實驗設計兩條技術路線:一條是選擇四種不同組成玻璃粉(SiO2-B2O3-CaO、SiO2-B2O3-Sb2O3、SiO2-B2O3-ZnO、SiO2-B2O3-TiO2),此時銅漿中玻璃粉含量為1.6wt%,制得G1、G2、G3和G4銅膜:另一條是控制銅漿中玻璃粉含量(1.6wt%、3.2wt%、4.8wt%)制得G3、G5和G6銅膜,然后對銅膜元素種類、微觀形貌、導電性、附著力和氧化增重等性能進行表征,從中選擇最佳玻璃粉組成及其含量。研究結果表明:當玻璃粉組成為SiO2-B2O3-2nO時,制得銅膜G3表面平整,孔洞較少,導電性較好,附著力較大;當玻璃粉含量為4.8wt%時,制得銅膜G6較致密,方阻為9.5mΩ/□,附著力為24N/mm2。為驗證G6銅膜使用可靠性,對其進行抗氧化性和抗老化性能測試,發(fā)現(xiàn)G6銅膜室溫氧化28天后增重率為3.5%,電阻變化率為0.79%;經(jīng)20℃～160℃高溫老化后其電阻變化率為12.63%,氧化增重率為4.63%,具有良好抗氧化性和抗老化性能。
[Abstract]:The ultrafine copper powder has many advantages, such as small size effect, surface interface effect, quantum scale effect and quantum tunneling effect. Therefore, it has many advantages in the fields of mechanics, electricity, chemistry and so on. In this paper, the superfine copper powder was prepared by two step reduction method in liquid phase. First, the copper oxide was prepared by glucose prereduction, and then other reduction was selected. The ultrafine copper powder was prepared by two times reduction. Two technical routes were designed: one was made of copper salts (copper acetate, copper chloride, copper sulfate and copper nitrate) made of C1, C2, C3 and C4 ultrafine copper powder; the other was the preparation of C5, C6, C7 and C8 ultrafine copper with two different reductants (hydrazine, sodium hypophosphite, ascorbic acid and sodium borohydride). Powder, then characterizing the types, micromorphology, particle size distribution, bulk density and conductivity of superfine copper powder, select better copper salt and two reducing agent. The results show that when copper salt is made of copper sulfate, the C3 copper powder is spherical, the particle size distribution is relatively uniform, the bulk density is up to 1.65 g/cm3, and the minimum resistance is 0.03. 7 Omega, when hydrazine hydrate is selected as the two reducing agent, the C5 copper powder is spherical, the particle size distribution is uniform, the average particle size is 1.89 mu m, the bulk density is up to 1.78 g/cm3 and the resistance minimum is 6.71m Omega. This provides a scientific basis for the preparation of antioxidant superfine copper powder. Copper powder, glass powder and organic carrier can be used as raw materials to prepare copper conductor slurry. Grinding, screen printing, leveling, drying, sintering and so on, can be made of copper film on ceramic substrate and widely used in modern technology. As an integral part of the copper conductor paste, glass powder forms a network structure with copper particles during the sintering of copper slurry, regulates the thermal expansion coefficient of copper pulp and satisfies the bonding strength between the electrode and the substrate. The composition and content of glass powder have important influence on the microstructure, conductivity, adhesion, oxidation resistance and aging resistance of the copper film. Two technical routes are designed: one is to choose four different kinds of glass powder (SiO2-B2O3-CaO, SiO2-B2O3-Sb2O3, SiO2-B2O3-ZnO, SiO2-B2O3-TiO2), and the content of glass powder in the copper slurry is 1. .6wt%, G1, G2, G3 and G4 copper films are prepared. The other is to control the glass powder content in the copper slurry (1.6wt%, 3.2wt%, 4.8wt%) to produce G3, G5 and G6 copper films. Then the properties of copper film elements, micromorphology, electrical conductivity, adhesion and oxidation weight gain are characterized, and the optimum composition and content of glass powder are selected. The results show that the composition of glass powder is made up of glass powder. When SiO2-B2O3-2nO, the copper film G3 surface is smooth, the hole is less, the conductivity is better, and the adhesion is great. When the glass powder content is 4.8wt%, the copper film G6 is more compact, the square resistance is 9.5m OMEGA / *, the adhesion is 24N/mm2. to verify the reliability of the G6 copper film, and the oxidation resistance and the aging resistance of the copper film are tested. It is found that the G6 copper film is oxidized at room temperature 28. The weight gain rate is 3.5% and the resistance change rate is 0.79%. The resistance change rate is 12.63% and the oxidation weight gain rate is 4.63% after high temperature aging at 20 ~ 160 C. It has good oxidation resistance and aging resistance.

【學位授予單位】：昆明理工大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：TG146.11;TM241

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