Al~（3+）掺杂抗静电改性ZnO颜料制备及其质子辐照效应
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摘要
ZnO白漆是一种广泛应用于各类航天器的低吸收-发射比热控涂层,具有良好的光学性能和工艺性能。航天器在轨运行期间,由于空间环境的作用会发生充放电现象,影响航天器的安全运行和使用寿命。在保障涂层光学性能的前提下,对ZnO颜料进行掺杂改性合成低电阻率的颜料,进而制备抗静电热控涂层,具有十分重要的工程应用背景和理论研究价值。
本文综合采用溶胶法和固相法,以异丙醇铝为掺杂剂,氨水作催化剂,对ZnO粉末成功进行了Al3+掺杂改性,合成了低电阻率、低太阳吸收比的导电颜料。并系统研究了ZnO颜料的改性工艺及其质子辐照损伤机理。
研究结果表明,Al3+掺杂ZnO颜料抗静电改性最佳工艺参数为:铝掺杂比例为3%、大气下900℃焙烧3h、Ar2气氛下800℃退火90min。经上述改性工艺处理后的颜料ZnO颜料电阻率从108?.cm下降到105?.cm,下降了3个数量级,同时改性处理后的ZnO颜料太阳吸收比从0.149升高为0.188,约退化了0.039,满足抗静电白漆对颜料光学性能的基本要求。
质子辐照前后,改性颜料太阳吸收比的变化大于纯ZnO颜料。改性ZnO颜料光学性能退化主要发生在可见光区,其吸收峰位置基本与纯ZnO颜料相同。
光致发光光谱(PL)分析表明,质子辐照前后改性颜料中的点缺陷种类与未改性ZnO颜料相同。包括:锌填隙(Zni)、氧填隙(Oi)、锌空位(VZn)、氧空位(VO)等,改性ZnO颜料中缺陷浓度明显提高。
The ZnO-type thermal control coatings possessing low ratio of solar absorptance to emittance factor are commonly used for spacecraft. And possess excellent optical properties. But under the exposure of space charging environment, spacecraft will badly damaged by charging and discharge. Using rational modification technique can alleviate or avoid the problem of its safety under space environment. On condition that keeping their initial optical properties .which have significant applied background in engineering and research meaning in theory.
In this paper, we used Sol-Gel technology and solid state method, where Al(C_3H_7O)_3 was used as the dopant,ammonia as the catalyst, to do research on the technique of coating modification of ZnO pigments used by spacecraft. The effects of Al dopant concentration,thermal treatment temperature and time, annealing temperature,annealing time on the resistivity and optical properties were studied. Furthmore, we did investigation on the damage mechanism of modified pigments under the protons irradiation.
After optimizing the technologic conditions, The results indicated that when the Al concentration was 3at%, the post heat cheating was 900℃and calcined 3 hours, annealing temperature was 800℃and annealing time was 1.5 hour, The resistivity of Al-doped ZnO pigments was decreased form 108?.cm to 105?.cm, meanwhile the solar absorptance were increased form 0.149 to 0.188, which changed about 0.039 can used as the pigment of antistatic thermal control coatings.
Under the protons irradiation,optical degradation of the modified pigment occurred mainly in visible region. The main absorption peak was the same as before irradiation.Δαs of the modified ZnO pigments became bigger than that of the unmodified.
Photoluminescence(PL) spectral analysis indicate that,before and after proton irradiation, the type of point defects in modified ZnO pigments were the same to pure ZnO pigments, included zinc interstitial (Zni), oxygen interstitial (Oi), zinc vacancies (VZn), and oxygen vacancies (VO). In addition, there existed no new type of point defects.
本文综合采用溶胶法和固相法,以异丙醇铝为掺杂剂,氨水作催化剂,对ZnO粉末成功进行了Al3+掺杂改性,合成了低电阻率、低太阳吸收比的导电颜料。并系统研究了ZnO颜料的改性工艺及其质子辐照损伤机理。
研究结果表明,Al3+掺杂ZnO颜料抗静电改性最佳工艺参数为:铝掺杂比例为3%、大气下900℃焙烧3h、Ar2气氛下800℃退火90min。经上述改性工艺处理后的颜料ZnO颜料电阻率从108?.cm下降到105?.cm,下降了3个数量级,同时改性处理后的ZnO颜料太阳吸收比从0.149升高为0.188,约退化了0.039,满足抗静电白漆对颜料光学性能的基本要求。
质子辐照前后,改性颜料太阳吸收比的变化大于纯ZnO颜料。改性ZnO颜料光学性能退化主要发生在可见光区,其吸收峰位置基本与纯ZnO颜料相同。
光致发光光谱(PL)分析表明,质子辐照前后改性颜料中的点缺陷种类与未改性ZnO颜料相同。包括:锌填隙(Zni)、氧填隙(Oi)、锌空位(VZn)、氧空位(VO)等,改性ZnO颜料中缺陷浓度明显提高。
The ZnO-type thermal control coatings possessing low ratio of solar absorptance to emittance factor are commonly used for spacecraft. And possess excellent optical properties. But under the exposure of space charging environment, spacecraft will badly damaged by charging and discharge. Using rational modification technique can alleviate or avoid the problem of its safety under space environment. On condition that keeping their initial optical properties .which have significant applied background in engineering and research meaning in theory.
In this paper, we used Sol-Gel technology and solid state method, where Al(C_3H_7O)_3 was used as the dopant,ammonia as the catalyst, to do research on the technique of coating modification of ZnO pigments used by spacecraft. The effects of Al dopant concentration,thermal treatment temperature and time, annealing temperature,annealing time on the resistivity and optical properties were studied. Furthmore, we did investigation on the damage mechanism of modified pigments under the protons irradiation.
After optimizing the technologic conditions, The results indicated that when the Al concentration was 3at%, the post heat cheating was 900℃and calcined 3 hours, annealing temperature was 800℃and annealing time was 1.5 hour, The resistivity of Al-doped ZnO pigments was decreased form 108?.cm to 105?.cm, meanwhile the solar absorptance were increased form 0.149 to 0.188, which changed about 0.039 can used as the pigment of antistatic thermal control coatings.
Under the protons irradiation,optical degradation of the modified pigment occurred mainly in visible region. The main absorption peak was the same as before irradiation.Δαs of the modified ZnO pigments became bigger than that of the unmodified.
Photoluminescence(PL) spectral analysis indicate that,before and after proton irradiation, the type of point defects in modified ZnO pigments were the same to pure ZnO pigments, included zinc interstitial (Zni), oxygen interstitial (Oi), zinc vacancies (VZn), and oxygen vacancies (VO). In addition, there existed no new type of point defects.
引文
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2胡金刚.中国航天器热控制技术进展.航天器工程. 2001,10(1):14~29
3过九镕.通信卫星的热控制技术.中国空间科学技. 1990,10(1):45~51
4 Davis V A,Dun Can L W. Spacecraft Surface Charglng Handbook. 1993
5卢榆孙.卫星表面材料物性与电荷积中国空间科学技术. 1992, 12(6):25~27
6江经善.防止卫星带电的温控涂层.宇航材料工艺1994,1(3):51~56
7杨垂柏,王世金,梁金宝.航天器充放电在轨探测试验的发展.上海航天. 2006,(2):28~31
8杨垂柏,梁金宝,王世金.地球同步轨道卫星表面电位探测一类方法初探.核电子学与探测技术. 2007,27(3):34~36
9中国科学院空间科学与应用研究中心.宇航空间环境手册[M].北京:中国科学技术出版社,2000:25~42
10黄本诚.空间环境工程学.宇航出版社. 1992:54~56
11卢榆孙,李华,蔡纯.星用抗静电导电膜光电性能评价方法.中国空间科学技术. 1992,1(2):21~25
12曾一兵,罗正平,李颖,冯伟泉.防静电白色热控涂层的耐空间环境及工艺性能.宇航材料工艺. 2007,(6):63~70
13曾一兵,张廉正,胡连成.俄罗斯空间有机热控涂层发展的现状及动向.宇航材料工艺. 1999,3(6):3~7
14马宏,孟军锋,谭海龙.高空间稳定低污染防静电有机热控涂层.现代涂料与涂装. 2005,1(7):67~68
15 R. Carruth.Plasma Effects on the Passive Thermal Control Coating of Space Station Freedom. AIAA Paper. 1992, No. 92-1685:1~20
16曾一兵,熊春晓,王慧,刘文言.防静电白色热控涂层的空间环境性能试验.中国空间科学技术. 2002,2(4):21~24
17周松.掺杂氧化锌晶须的聚氨酯涂料抗静电性能研究.涂料工业. 2006,36 (12):8~13
18罗重霄.导电ZAO纳米晶的超声模板法合成、表征及应用. Acta Phys.-Chim.Sin. 2008,24(6):1007-1011
19 Zgur,Ya.I.Alivov,C.Liu.Teke.J. Appl.Phys. 2005,98(04)13~21
20 Claire tonon.Model of Degradation of Thermal Control Coatings in Space Environment.5th International Symposium on Materials in a Space Environment.Arcachon France,2000:57~61
21冯伟泉,丁义刚,闫德葵,刘学超,王伟,李冬梅.地球同步轨道长寿命卫星热控涂层太阳吸收率性能退化研究.中国空间科学技术,2005,13(2):12~15
22杜尚丰,陈运法,梁云.导电氧化锌粉体的掺杂和制备.功能材料. 2004,35(1):968～972
23于晓辉.导电涂料的研制开发与应用[M].昆明理工大学硕士学位论文,2005,43~45
24.万翠凤.氧化锌晶须改性及导电性能研究.中南大学硕士学位论文. 2008, 15~18
25娄霞,朱东敏,张琳,罗发周万成. Al掺杂含量对纳米ZAO粉体性能的影响.功能材料.2008,39(4):667~669
26洪若瑜.纳米ZnO粉体的制备及其表面TiO2包覆改性.精细石油化工. 2005, 3(2):1~4
27吴晓森,张学鹜,吴文健.导电涂料的原理及其军事应用.上海涂料. 2005,43(7):29~33
28 GB1410-89.固体绝缘材料体积电阻率和表面电阻率试验方法[S].1990
29聂攀登,薛涛,张煜,李向军.铝掺杂氧化锌的合成及结构分析.中国科学B缉化学2008(3)8:584~588
30 K.J.Chen,T.H.Fang . The crystallization and physical properties of Al-doped ZnO nanoparticles. Applied Surface Science. 2008,254:5791~5795
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