纳米级铜锌合金薄膜的研制及其基础研究
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摘要
本论文以纳米Cu-Zn合金薄膜的制备为研究内容，采用溅射法制备了纳米Cu-Zn合金薄膜，进行了溅射工艺的研究，并探讨了Cu-Zn合金薄膜的形成机理，提出了一种测定纳米膜厚度的新方法。
实验过程中，研究了溅射电压、靶基距、溅射压力和溅射时间四个主要工艺参数对薄膜成份、薄膜生长速率、薄膜厚度及其表面平整度的影响。在不同实验条件下，Cu-Zn合金薄膜中的Cu含量主要分布范围是70.41～72.01％，略低于Cu-Zn合金靶材中的Cu含量(72.28％)，且各个样品之间的Cu含量相差最大的只有1.6％，因此可认为用溅射法制备Cu-Zn合金薄膜时，薄膜成份受工艺参数的影响不大。随着溅射电压的增大，薄膜的生长速率随之增大，二者近似线性关系。而靶基距的增大则降低了薄膜的生长速率，二者成反比例关系。溅射压力对薄膜生长速率的影响比较复杂，在实验条件下，当溅射压力小于10Pa时，溅射压力的增大对Cu-Zn合金薄膜生长的促进作用占主导地位，因此随着溅射压力的增大，薄膜生长速率增大；当溅射压力大于10Pa时，溅射压力的增大对Cu-Zn薄膜生长的抑制作用占主导地位，故随着溅射压力的增大，薄膜生长速率反而减小。薄膜生长速率的最大值(为3.18nm·min~(-1))在溅射压力为10Pa处取得。在其它工艺参数相同的情况下，薄膜的厚度随着溅射时间的延长而增大。影响合金薄膜表观质量的主要因素是Cu-Zn合金靶材粒子的动能。溅射出的靶材粒子能量越低，对Cu-Zn合金薄膜表面的损伤越小。溅射电压的减小和靶基距的增大，都能减小靶材粒子的动能。虽然溅射压力的增大也能减小靶材粒子的动能，但同时也提高了Cu-Zn合金薄膜内的气体含量，使薄膜中含有更多的气孔而显得比较粗糙。
实验表明溅射法制备Cu-Zn合金纳米薄膜的最优工艺条件为：溅射电压V=1.6Kv，靶基距D=2.5cm，溅射压力P=5Pa，溅射时间T=20min。在此条件下制备得到的Cu-Zn合金薄膜中Cu的平均含量为70.97％，平均膜厚为41.08nm，平均光泽度为136.3Gs。通过原子力显微镜可以观察到薄膜的表面比较平整。
The formation mechanism of Cu-Zn alloy films is studied and a new way to measure the thickness of nanograde Cu-Zn alloy films is developed in this thesis. Laminar Cu-Zn alloy films, which are used for making high grade metal effect pigment, nanograde laminar Cu-Zn powder, are prepared by sputtering technique.
In the paper, the effects made by four primary parameters ?sputtering voltage, target-to-substrate distance, sputtering pressure and sputtering time , on the components, the growth speed, the thickness and the surface quality of Cu-Zn alloy films were discussed according to the experiment results. Under different experiment conditions, the Cu contents of films varied from 70.41% to 72.01%, which were slightly less than that of the target (72.28%). The difference of the Cu contents in the films was no more than 1.6%. Therefore, the effects of technical parameters on the compositions of Cu-Zn alloy films were negligible during sputtering process. With the augment of sputtering voltage, the growth speed of films became higher accordingly and the relation was nearly linear under the experimented conditions. In contrast, the growth speed of films became lower with the increase of target-to-substrate distance. The effects of sputtering pressure on the growth speed of films were rather complicated.
When the sputtering pressure was lower than 1 OPa, the augment of sputtering pressure promoted the growth of films. As a result, the growth speed of films increased as the sputtering pressure grew higher. On the contrary, when the sputtering pressure was higher than 1 OPa, the augment of sputtering pressure inhibited the growth of films and thus the growth speed decreased as sputtering pressure grew higher. The maximum of the growth speed was obtained when sputtering pressure was equal to 10Pa. With the extension of time, the films became thicker. The main factor affecting the surface quality of films was the kinetic energy of Cu-Zn alloy particles. The lower energy of sputtering target particles, the smaller damnification to the surface of Cu-Zn films was. Both the decrease of sputtering voltage and the augment of target-to-substrate distance could reduce the kinetic energy of target
particles. Although the augment of sputtering pressure could cut down the kinetic energy of target particles too, it increased the gas content of Cu-Zn alloy films, which made the surface of films rough because of more holes.
The experiments showed that the suitable technique condition of making Cu-Zn alloy films was as follows: sputtering voltage V = 1.6Kv, target-to-substrate distance D = 2.5cm, sputtering pressure P = 5Pa, sputtering time T = 20min. The average Cu content in Cu-Zn alloy films preparing under this condition was 70.97%, and the mean thickness was 41.08nm. It could be observed that the surface of films whose mean glossiness was 136.3GS, was smooth by atomic force microscope.
实验过程中，研究了溅射电压、靶基距、溅射压力和溅射时间四个主要工艺参数对薄膜成份、薄膜生长速率、薄膜厚度及其表面平整度的影响。在不同实验条件下，Cu-Zn合金薄膜中的Cu含量主要分布范围是70.41～72.01％，略低于Cu-Zn合金靶材中的Cu含量(72.28％)，且各个样品之间的Cu含量相差最大的只有1.6％，因此可认为用溅射法制备Cu-Zn合金薄膜时，薄膜成份受工艺参数的影响不大。随着溅射电压的增大，薄膜的生长速率随之增大，二者近似线性关系。而靶基距的增大则降低了薄膜的生长速率，二者成反比例关系。溅射压力对薄膜生长速率的影响比较复杂，在实验条件下，当溅射压力小于10Pa时，溅射压力的增大对Cu-Zn合金薄膜生长的促进作用占主导地位，因此随着溅射压力的增大，薄膜生长速率增大；当溅射压力大于10Pa时，溅射压力的增大对Cu-Zn薄膜生长的抑制作用占主导地位，故随着溅射压力的增大，薄膜生长速率反而减小。薄膜生长速率的最大值(为3.18nm·min~(-1))在溅射压力为10Pa处取得。在其它工艺参数相同的情况下，薄膜的厚度随着溅射时间的延长而增大。影响合金薄膜表观质量的主要因素是Cu-Zn合金靶材粒子的动能。溅射出的靶材粒子能量越低，对Cu-Zn合金薄膜表面的损伤越小。溅射电压的减小和靶基距的增大，都能减小靶材粒子的动能。虽然溅射压力的增大也能减小靶材粒子的动能，但同时也提高了Cu-Zn合金薄膜内的气体含量，使薄膜中含有更多的气孔而显得比较粗糙。
实验表明溅射法制备Cu-Zn合金纳米薄膜的最优工艺条件为：溅射电压V=1.6Kv，靶基距D=2.5cm，溅射压力P=5Pa，溅射时间T=20min。在此条件下制备得到的Cu-Zn合金薄膜中Cu的平均含量为70.97％，平均膜厚为41.08nm，平均光泽度为136.3Gs。通过原子力显微镜可以观察到薄膜的表面比较平整。
The formation mechanism of Cu-Zn alloy films is studied and a new way to measure the thickness of nanograde Cu-Zn alloy films is developed in this thesis. Laminar Cu-Zn alloy films, which are used for making high grade metal effect pigment, nanograde laminar Cu-Zn powder, are prepared by sputtering technique.
In the paper, the effects made by four primary parameters ?sputtering voltage, target-to-substrate distance, sputtering pressure and sputtering time , on the components, the growth speed, the thickness and the surface quality of Cu-Zn alloy films were discussed according to the experiment results. Under different experiment conditions, the Cu contents of films varied from 70.41% to 72.01%, which were slightly less than that of the target (72.28%). The difference of the Cu contents in the films was no more than 1.6%. Therefore, the effects of technical parameters on the compositions of Cu-Zn alloy films were negligible during sputtering process. With the augment of sputtering voltage, the growth speed of films became higher accordingly and the relation was nearly linear under the experimented conditions. In contrast, the growth speed of films became lower with the increase of target-to-substrate distance. The effects of sputtering pressure on the growth speed of films were rather complicated.
When the sputtering pressure was lower than 1 OPa, the augment of sputtering pressure promoted the growth of films. As a result, the growth speed of films increased as the sputtering pressure grew higher. On the contrary, when the sputtering pressure was higher than 1 OPa, the augment of sputtering pressure inhibited the growth of films and thus the growth speed decreased as sputtering pressure grew higher. The maximum of the growth speed was obtained when sputtering pressure was equal to 10Pa. With the extension of time, the films became thicker. The main factor affecting the surface quality of films was the kinetic energy of Cu-Zn alloy particles. The lower energy of sputtering target particles, the smaller damnification to the surface of Cu-Zn films was. Both the decrease of sputtering voltage and the augment of target-to-substrate distance could reduce the kinetic energy of target
particles. Although the augment of sputtering pressure could cut down the kinetic energy of target particles too, it increased the gas content of Cu-Zn alloy films, which made the surface of films rough because of more holes.
The experiments showed that the suitable technique condition of making Cu-Zn alloy films was as follows: sputtering voltage V = 1.6Kv, target-to-substrate distance D = 2.5cm, sputtering pressure P = 5Pa, sputtering time T = 20min. The average Cu content in Cu-Zn alloy films preparing under this condition was 70.97%, and the mean thickness was 41.08nm. It could be observed that the surface of films whose mean glossiness was 136.3GS, was smooth by atomic force microscope.
引文
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[13] 郭平译．利用金银粉油墨提高印刷产品的装饰效果．印刷科技情报，1986，(3)：56
[14] 周锦鑫，郑裕生，黄永昌．我国铜金粉生产技术的现状与存在问题浅析．化学世界，1999，40(9)：498-500
[15] 李国胜，易琼．一种雾化铜合金粉及铜粉改性处理的生产方法．中国：1320500，2001．11．07
[16] 周锦鑫，马紫峰，黄永昌，等．氮气保护气氛下鳞片状铜金粉制造工艺．中国：129231，2001．4．25
[17] 周锦鑫．超细铜金粉生产制造工艺优化及改造研究．新技术新工艺，2000，(3)：31-33
[18] 张拥军．年产 1000 吨喷涂用抗氧化仿金铜合金粉．中国科技成果，2003，(9)：27-31
[19] 朱晓云．铜锌合金粉在凹版印刷中的应用．云南冶金，2000，29，(6)：34-36
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[21] Holiday R V, Patterson R J. Method for producing metal powder. U.S. Patent:No. 4343750, 1982.5
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