- 學位論文
富鎳-鐵-銅之氧化物及氫氧化物製備及電性研究
Preparation and Electrical Property of Nickel rich-Iron-Copper Oxides and Its Hydroxides
摘要
本研究是採用共沉澱法製備以鎳為主之氫氧化物，在共沉澱過pH控制在10，由酸鹼的滴定量計算，成分的誤差約在0.1%以下。然後藉由氫氧化鐵、氫氧化銅添加來形成不同三元合金。將樣品製備成圓錠狀，利用掃描式電子顯微鏡(SEM)來觀察其微觀組織，同時由阻抗分析儀(LCR)來測試電性，除此之外更近一步使用X-光繞射儀(XRD)來分析其相組成。 除了氫氧化物，本研究亦探討其氧化物之特性，其中氧化物是由氫氧化物圓錠直接利用熱處理的方式得到的。而熱處理的條件是550℃下0.5h。而這些熱處理後的氧化物有明顯的收縮，而且吳明顯瑕疵，同時燒節緻密性達90%以上。 至於以鎳為主的氫氧化物及氧化物之物理特性分別歸納如下: 在電性方面: Ni1-XMX(OH)2複合材料的測量頻率為30Hz-1MHz。在常溫的阻抗為3×10-5- 1.0 Ω，隨著測量頻率提高，而其阻抗就愈大。其中Fe的含量增加對阻抗並無明顯的影響；至於Cu的含量增加對阻抗卻有明顯下降的趨勢。至於Fe和Cu同時添加對阻抗亦有明顯下降的趨勢。在Ni1-XMXO複合材料方面測量頻率為30Hz-1MHz，在常溫的阻抗為 4×10-5- 102Ω，隨著測量頻率提高，而其阻抗就愈大。其中Fe的含量增加對阻抗有下降的趨勢。至於Cu的含量增加對阻抗卻有明顯下降的趨勢。至於Fe和Cu同時添加對阻抗亦有明顯下降的趨勢。 在相組成方面:Ni1-XMX(OH)2複合材料的晶體結構，由XRD發現在x=0-0.3時，其晶體結構和純的Ni(OH)2的晶體結構並沒有明顯差異。至於Ni1-XMXO的晶體結構，由XRD發現在x=0-0.3時，Fe含量增加對NiO的晶體結構並無明顯的差異。然而Cu的添加，除了NiO的晶體結構外，還有其他的雜相；目前仍正在近一步探討中。 在微觀組織方面:Ni1-XMX(OH)2複合材料，隨著Fe含量增加其晶粒有形成長條的形狀。至於Cu的含量含量增加，其晶粒俱有等軸晶的形狀，而Fe和Cu同時添加同時添加亦俱有等軸晶粒的形狀。對Ni1-XMXO複合材料，其微觀組織方面，隨著Fe含量增加其晶粒有小部份是長條的形狀。至於Cu的含量含量增加，其晶粒亦有小部份俱有長條的形狀。至於Fe和Cu含量增加對晶粒長條型沒有明顯區別。
並列摘要
A coprecipitation method is used to prepare hydroxide alloys. During coprecipitation, the mixed acid –base solution is controlled at pH=10, and it is expected the error of composition of these coprecipitated specimens is < 0.1 %. Fe(OH)2 and Cu(OH)2 are also introduced in the Ni(OH)2 system to prepare a ternary hydroxide powders. After powder preparation, cylinderical specimens are used to observe their microstructures, electrical propcrties, and phase existence by using SEM,LCR, and XRD respectively. Except for hydroxides, the corresponding oxides are also obtained to determine their physical propecties. However, these oxides are directly prepared from hydroxide cylindrical specimens through a heat treatment at 550oC for 0.5h. By comparing with the initial hydroxide specimens, the sintered oxide specimens show a significant shrinkage without any apparent defects, with the densification up to 90%. The physical propecties of these hydroxides and sintered oxides are summarijed as follows : As to electrical propecties, Ni1-XMX(OH)2 composites are measured from 30 Hz to 1 M Hz. The electrical resistance of these hydroxide specimen is ranged from 3 x 10-5 -1.0 Ω , which increases as the measuring frequency increases. In the alloying effects, electrical resistance seems not affected by the content of Fe(OH)2 , but decreasing by the content of Cu(OH)2 increasing, and also decreasing by Cu(OH)2 plus Fe(OH)2 increasing. In the Ni1-xMxO composite system, its measuring frequency is also set at 30 Hz to 1 M Hz, and its electrical resistance is found at 4x10-5 ~102 at room temperature, which increases as the measuring frequency increases. As to the alloying effects, the electrical resistance decreases as the content of FeO increases, decreases as the content of CuO increases, and also decreases as CuO plus FeO increases. As to the phase existence, Ni1-xMx(OH)2 composites show Ni(OH)2 crystal structure and no any significant phase differences being observed for specimens containing different alloys, from X-ray diffraction (XRD) determination. For the Ni1-xMxO sintered composites, its phase existence slows no significant differences for specimens containing FeO, but it shows other phases for specimens containing CuO, and such extra phases are still under investigation. As to microstructures, in the Ni1-xMx(OH)2 system, specimens with a higher content of Fe(OH)2 show some elongated grains, but equiaxed grains in the specimens with a higher content of Cu(OH)2 , and also equiaxed grains in the specimens with a higher content of Cu(OH)2 plus Fe(OH)2. In the Ni1-xMxO system, some minor elongated grains are observed in the specimens with a content of FeO or CuO, but no elongated grains are observed in the specimens containing FeO plus CuO.