本文選題：溶膠 + 凝膠��； 參考：《蘭州大學(xué)》2010年碩士論文

【摘要】：NiCuZn軟磁鐵氧體具有電阻率大、渦流損耗小、成本低等優(yōu)點,其使用頻率范圍是kHz到將近GHz,寬于MnZn (1MHz以下)和NiZn (1-100MHz)鐵氧體材料,可以實現(xiàn)高頻射頻信號的能量傳輸和阻抗轉(zhuǎn)換,廣泛應(yīng)用于計算機、電視、通訊等領(lǐng)域,主要用于制造電感等元器件,但是到目前為止,成功應(yīng)用于集成電路的高頻NiCuZn軟磁鐵氧體薄膜的制備和研究還較少,能否成功的制備出高飽和磁化強度、低矯頑力的NiCuZn鐵氧體薄膜成為未來其應(yīng)用的一個重要限制因素。在制備薄膜材料的工藝方法中,常用的有濺射、真空蒸發(fā)等工藝。但是濺射方法制備薄膜工藝存在各離子濺射速率不同造成成份偏析以及沉積速率低等缺點,真空蒸發(fā)也存在重復(fù)性差和附著性差等缺點,而且鐵氧體的高熔點使得真空蒸發(fā)工藝的具體實施存在困難。然而另一種制備薄膜的常見方法-溶膠-凝膠旋涂法制備鐵氧體薄膜的報道還比較少。溶膠-凝膠工藝因為其可以使反應(yīng)物達到分子水平的混合、容易控制成分、有效的降低燒結(jié)溫度等優(yōu)點,廣泛應(yīng)用于材料科學(xué)和陶瓷工藝領(lǐng)域。凝膠可以應(yīng)用旋涂法在基片上做膜,其優(yōu)點是條件簡單,并且不受物體外形的限制。本文應(yīng)用溶膠-凝膠旋涂工藝進行了NiCuZn軟磁鐵氧體的粉體和薄膜的制備,采用N,N二甲基甲酰胺作為溶劑,聚乙烯吡咯烷酮作為表面活性劑,研究了成分配比、溶膠凝膠性質(zhì),以及工藝條件等對粉體和薄膜磁性能的影響,在制備出磁性能優(yōu)異的NiCuZn軟磁鐵氧體粉體材料薄膜方面做了積極的探索并獲得了一些有意義的結(jié)果。 1.將穩(wěn)定的凝膠在常溫下自蔓延燃燒,所得到的前驅(qū)粉體在≥750℃下處理,將會生成比較純的尖晶石相。而相應(yīng)成份的薄膜在400℃進行長時間熱處理,沒有尖晶石相生成,當(dāng)熱處理溫度達到600℃左右,即能生成完全的尖晶石相。 2.采用適當(dāng)缺鐵配方的Ni0.4Cu0.2Zn0.4Fe1.9O4制得的粉體,在900℃下保溫三個小時,矯頑力可達90e,飽和磁化強度為72.4 emu/g,繼續(xù)升高溫度,當(dāng)溫度達到1000℃,此時樣品的矯頑力為50e,飽和磁化強度為73.57 emu/g。 3.與未加入醋酸的溶膠相比,加入適量醋酸調(diào)節(jié)pH值為3.2時,在Si基片上得到的薄膜樣品矯頑力較小,可見加酸得到的凝膠的活性更高。 4.將溶膠在不同溫度下陳化,制得樣品的矯頑力Hc隨溶膠陳化放置時間逐漸減小,然后趨于穩(wěn)定,其中由常溫下放置的溶膠制得樣品的矯頑力較小且最先穩(wěn)定。 5.為制得高性能的薄膜樣品,應(yīng)采用Ni0.4Cu0.2Zn0.4Fe2O4的正配比配方,有利的燒結(jié)工藝是在500℃-650℃之間,進行短時間的保溫,抑制晶粒生長,其中處理溫度585℃的樣品,矯頑力達到160e,在更高的溫度下,矯頑力和飽和磁化強度都將升高,飽和磁化強度在較高的溫度可以達到300 emu/cm3。 6.測量較高的溫度下處理粉體和薄膜,測得的電子自旋共振譜中譜線會改變,曲線與橫坐標(biāo)的交點反映出的g值的變化,意味著離子之間占位發(fā)生改變。這可能與應(yīng)用溶膠-凝膠離子與很高的活性,適當(dāng)?shù)母邷貙?dǎo)致Zn元素?fù)]發(fā),導(dǎo)致尖晶石鐵氧體A位缺失的Zn離子將被其他離子取代有關(guān)。
[Abstract]:NiCuZn soft ferrite has the advantages of large resistivity, small eddy current loss and low cost. The use frequency range is from kHz to near GHz, wider than MnZn (1MHz) and NiZn (1-100MHz) ferrite material. It can realize the energy transmission and impedance conversion of high frequency radio frequency signal. It is widely used in the fields of computer, television, communication and so on. It is mainly used in manufacturing. Inductance and other components, but so far, the preparation and research of the high frequency NiCuZn soft ferrite thin films which have been successfully applied to the integrated circuits are still less. The successful preparation of high saturation magnetization and the low coercive force of NiCuZn ferrite thin film become a key limiting factor in future applications. Sputtering, vacuum evaporation and other processes are commonly used in the process. However, there are disadvantages of different sputtering rates and low deposition rate, such as low ion sputtering rate and low deposition rate. The vacuum evaporation also has the disadvantages of poor repeatability and poor adhesion, and the high melting point of ferrite makes the specific implementation of vacuum evaporation process difficult. However, another common method for preparing thin films - sol-gel spin coating method for preparing ferrite thin films is still less. The sol-gel process is widely used in the field of material science and ceramic technology because it can make the reactants at molecular level, easily control components, and reduce the sintering temperature effectively. With the application of spin coating on the substrate, the advantage is that the condition is simple and it is not restricted by the shape of the object. In this paper, the preparation of the powder and film of NiCuZn soft ferrite was prepared by the sol-gel spin coating process. N, N two methyl formamide was used as the solvent and polyvinylpyrrolidone was used as a surface active agent. The effects of gel properties and technological conditions on the magnetic properties of powders and films have been actively explored and some meaningful results have been obtained in the preparation of NiCuZn soft magnetic ferrite powder materials with excellent magnetic properties.
1. the stable gel is self propagating at normal temperature. The obtained precursor powder is treated at more than 750 degrees C, and a relatively pure spinel phase will be generated. The film of the corresponding component will be heat treated at 400 C for a long time, without the formation of the spinel stone phase, and the complete spinel phase can be generated when the heat treatment temperature reaches the left right of 600 C.
2. the powder obtained by Ni0.4Cu0.2Zn0.4Fe1.9O4 with proper iron deficiency formula is kept at 900 C for three hours, the coercive force can reach 90E, the saturation magnetization is 72.4 emu/g, and the temperature continues to rise. When the temperature reaches 1000, the coercive force of the sample is 50E, and the saturation magnetization is 73.57 emu/g..
3. compared with the sols without acetic acid, when a proper amount of acetic acid is added to the pH value of 3.2, the film samples obtained on the Si substrate are less coercive, and the activity of the gel obtained with acid is higher.
4. the sols are aging at different temperatures, and the coercive force Hc of the samples decreases gradually with the sol-aging time, and then tends to be stable, in which the coercivity of the samples obtained by the sols placed under the normal temperature is smaller and the first stable.
5. for the preparation of high performance film samples, the positive ratio formula of Ni0.4Cu0.2Zn0.4Fe2O4 should be used. The favorable sintering process is between 500 C and -650 C for short time heat preservation and inhibition of grain growth, in which the samples with temperature 585 C and the coercive force reach 160E, the coercive force and saturation magnetization will be increased at a higher temperature and full saturation magnetization will be increased. And magnetization can reach 300 emu/cm3. at higher temperature.
6. at a higher temperature, the powder and the film are treated. The spectra line in the electron spin resonance spectrum will be changed, the change of the g value reflected by the intersection point between the curve and the abscissa means the change of the occupying position between the ions. This may be associated with the application of the sol-gel ion and high activity. The appropriate high temperature will lead to the volatilization of the Zn element and lead to the spinel. The Zn ions with A deletion in the ferrite will be replaced by other ions.
【學(xué)位授予單位】：蘭州大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2010
【分類號】：TM277

【參考文獻】

相關(guān)期刊論文 前10條

1 李寧,盧迪芬,陳森鳳;溶膠-凝膠法制備薄膜的研究進展[J];玻璃與搪瓷;2004年06期

2 岳麗華,李W，

本文編號：1958328