CN103608108A - 二氧化钛光催化剂组合物及其应用 - Google Patents
二氧化钛光催化剂组合物及其应用 Download PDFInfo
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- CN103608108A CN103608108A CN201280030858.1A CN201280030858A CN103608108A CN 103608108 A CN103608108 A CN 103608108A CN 201280030858 A CN201280030858 A CN 201280030858A CN 103608108 A CN103608108 A CN 103608108A
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- titanium dioxide
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- zinc
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Abstract
一种包括锌(Zn)掺杂的二氧化钛(TiO2)纳米颗粒的光催化剂组合物,其中二氧化钛纳米颗粒和锌的比例为约5-约150。所述光催化剂组合物吸收约200纳米-约500纳米波长范围内的电磁辐射,且对波长大于约450纳米的光的吸收度低于对波长小于约350纳米的光的吸收度的50%。还提供一种用于处理或防止植物中微生物疾病和感染的方法,以及一种增加植物的农作物产量的方法,其包括将本文教导的光催化剂组合物应用至植物表面。还提供一种用于处理表面上微生物疾病的方法,其包括将本文教导的光催化剂组合物应用至用人造光照明的表面。
Description
领域
本发明涉及包括二氧化钛(TiO2)纳米颗粒的新型光催化剂组合物,其可用于处理微生物疾病,更具体的,植物中的微生物疾病。
背景
在过去的几十年中,材料性能的开发和探索导致认识了结晶金属氧化物如TiO2的光催化剂性质。在这个领域已经投入了很多力量进行研究,从而得到了很多潜在应用如传感器,光催化剂,和光伏。这种材料的性质取决于它们的化学组成,尺寸和形状。更具体的,当该材料的粒度减小时,因为表面积大量增加,可展现新的物理和化学性质。但是,如陈(Chen)等在TiO2颗粒的合成方法和物理化学的全面综述所讨论的(《化学评论》(Chemical Reviews)卷107,第2891-2959页,2007年),物理性质和光催化活性之间的关系是很复杂的,且优化的条件和结构可随具体情况而变化。
在发现TiO2的光催化一些年之后,研究表明TiO2在紫外(UV)辐射(387纳米)下辐照60-120分钟后,可用作光活性抗微生物涂层;该涂层能对大肠杆菌(Escherichia coli)和嗜酸乳杆菌(Lactobacillus acidophilus)有高效的杀菌作用(松永等人,FEMS微生物快报(FEMS Microbiology Letters),第29卷,第211-214页,1985)。后续的工作导致开发了纳米级的TiO2制剂,其对大量细菌、真菌和病毒组织都有抑制作用(例如,次郎(Tsuang)等,人造器官(Articial Organs),卷32,第167-174页,2008年,以及乔(Choi)等,角矫正医师(Angle Orthodontist),卷79,第528-532页,2009年),包括那些存在于表面时会增加医院获得性感染风险的组织(S.J当斯(Dancer,S.J.),柳叶刀感染病(Lancet infections Diseases),卷8,第101-113页,2008年)。因此,当需要在无生命物体表面减少微生物污染时,可在该表面上应用纳米级的TiO2涂层,随后进行UV辐射。
最近,有几篇报道表明TiO2可应用至植物上以提供某些好处。卡外(Kawai)提出来自TiO2制剂应用的光催化氧化效应降解有机材料,并由此增加在树叶表面局部的CO2浓度,导致植物的糖含量增加,并且还通过氧化植物脂质诱发能减少致病性微生物的内源性植物防御机制,从而在至少某些植物中创建杀菌环境(美国专利6,589,912)。据报道,平均粒度为30纳米的市售光催化纳米级TiO2可以加速开花和结果,并减少某些疾病的发生(日本专利2006-632721)。另一课题组也报道了平均粒度为30纳米的光催化纳米级TiO2可以降低黄瓜叶中两种细菌的疾病程度,还可增加光合作用速率(张(Zhang)等,Nanoscience,卷12(1),第1-6页,2007年;张(Zhang)等,Journal of Inorganic Materials,卷23(1),第55-60页,2008年;崔(Cui)等,NSTI-Nanotech,卷2,第286-289页,2009年)。
纳米级TiO2可以吸收UV范围内的光,但对可见光范围的光的吸收度很少;这个特征使它在防护UV损坏是有帮助的应用中成为一种有用的组分。但是,在某些应用中,优选的需要取得在更长波长的光的光催化效应。例如,室内光一般具有最低的UV能量,这显著减少纳米级TiO2展现光催化的能力。类似的,在农业应用中,更高的光催化效率可降低应用比率和成本,且通过增加光催化剂中俘获的可用太阳辐射的比例会带来多重好处。因此,提高在更高波长的吸收度将使更多应用受益于光催化效应。
许多年的研究已显示TiO2的吸收光谱可通过引入改变其晶体晶格结构的掺杂剂来改变。一篇最新的报道表明其吸收光谱可延伸至整个可见光区,以制备一种人眼看来是黑色的材料(陈(Chen)等,Science Xpress,第1-10页,2011年1月20日在线出版,Science.1200448)。但是,这么宽的吸收光谱并不是植物应用所需的,因为它们靠太阳辐射来进行光合作用。
植物的光合作用效率在整个电磁谱范围都是不同的。提供某一光合作用速率所需的具有给定能力或波长的光子的数量是可以测量的,且当在一个波长范围内确定时,就可以获得作用光谱。对于各种植物物种,已经报道了在多种单色光下的具体作用光谱。已报道了高等植物33个物种的作用光谱的系统研究(伊那达(Inada,K.),Plant and Cell Physiology,卷17,第355-365页,1976年)。感兴趣的发现是所有草本植物的作用光谱基本相似,在500-680纳米范围内有一个高和宽的峰,它的峰肩更低和更窄,延伸至约435纳米,波长更短时则快速下降。草本植物的作用光谱也类似,但在435纳米初峰肩的尺寸比木本植物的更小。
因此,有需要开发一种能有效吸收波长低于约450纳米的电磁能量的高效光催化材料。优化的光催化庄家保护剂和增产剂的其他要求包括低成本、丰富的原料,易于合成和应用,以及尤其是低环境毒性,并因此任意包含所述剂的材料都有好的安全性。
内容
本发明涉及包括掺杂二氧化钛(TiO2)纳米颗粒的光催化剂组合物,其可用于处理和防止微生物疾病和感染,更具体的,植物中的微生物疾病和感染。
在一实施方式中,本发明提供一种包括锌(Zn)掺杂的二氧化钛(TiO2)纳米颗粒的光催化剂组合物,且二氧化钛和锌的比例为约5-约150。
该光催化剂组合物还可包括二氧化硅(SiO2)。二氧化钛和二氧化硅的比例为约1-约500。
所述二氧化钛纳米颗粒的平均粒度优选的为约2纳米-约20纳米。
所述光催化剂组合物吸收约200纳米-约500纳米波长范围内的电磁辐射,且对波长大于约450纳米的光的吸收度低于对波长小于约350纳米的光吸收度的50%。
此外,本发明提供一种用于防止或处理植物中微生物疾病和感染的方法,其包括将本文教导的光催化剂组合物应用至植物表面。本发明还提供一种用于植物农作物保护和增产的方法,其包括将本文教导的光催化剂组合物应用至植物表面。
附图简要说明
图1是各种TiO2组合物俘获太阳能的图像显示。
图2是各种TiO2组合物在354纳米辐照下的光催化活性的图像显示。
图3显示使用UV-A光时,用各种TiO2组合物处理的表面对穿孔疮痂病菌(Xanthomonas perforans)的光催化杀灭。
图4显示在阳光下各种TiO2组合物防止/减少每株植物叶斑病病变数目的效率。
图5显示阳光下用于控制橄榄结的选定处理的效率。
图6显示了阳光下各种TiO2组合物对白粉病的真菌病因试剂耳单丝壳(Sphaerotheca fuliginea)/黄瓜白斑病菌(Erysiphecichoracearum)分生孢子发展的影响。
发明详述
本发明提供改性的光催化剂组合物,能满足对广泛用于植物的光催化产品的要求,且表明其优于未改性的纳米级TiO2。此外,还评估了适当的应用比率。所述组合物能防止番茄植物的黑色叶斑病,增加商品果实的产率,减少哈密瓜上白粉病分生孢子的形成,以及保护橄榄植物以免其长微生物诱导的肿瘤。所述组合物只包括表征清楚和安全的材料,且可用普通的喷洒设备方便的应用到田间。本发明实施的改进使得包括室内人工照明的低UV辐射环境也能享受光催化活性的好处。
本发明涉及包括锌(Zn)掺杂二氧化钛(TiO2)纳米颗粒的光催化剂组合物,其可用于处理和防止微生物疾病和感染,更具体的,植物中的微生物疾病。
在一实施方式中,本发明提供一种包括锌(Zn)掺杂的二氧化钛(TiO2)纳米颗粒的光催化剂组合物,二氧化钛和锌的比例为约5-约150。二氧化钛和锌的比例优选的为约40-约100。
该光催化剂组合物还可包括二氧化硅(SiO2)。二氧化钛和二氧化硅的比例为约1-约500,优选的约3-约20。
所述二氧化钛纳米颗粒的平均粒度优选的为约2纳米-约20纳米。
本发明的一具体优选的实施方式提供一种光催化剂组合物,其包括:
(A)约5000-约8000ppm的二氧化钛,
(B)约50-约100ppm的锌,以及
(C)约500-约1000ppm的二氧化硅。
所述光催化剂组合物吸收约200纳米-约500纳米波长范围内的电磁辐射,且对波长大于约450纳米的光的吸收度低于对波长小于约350纳米的光吸收度的50%。
本发明的另一实施方式提供一种用于处理或防止植物中微生物疾病和感染的方法,其包括将包括锌(Zn)掺杂的二氧化钛(TiO2)纳米颗粒、二氧化钛和锌的比例为约5-约150的光催化剂组合物应用至植物表面。
可用于处理的植物的示例包括,但不限于:农作物植物,包括草本和木本农作物植物例如番茄植物,黄瓜植物,柑橘属植物,橄榄和其他核果植物,苹果和其他仁果类植物,坚果植物,和观赏植物。
微生物疾病的示例包括,但不限于:叶斑病,橄榄结,火疫病,胡桃疫病,樱桃溃疡和白粉病。
本发明还提供一种用于增加植物的农作物产量的方法,其包括将包括锌(Zn)掺杂的二氧化钛(TiO2)纳米颗粒、二氧化钛和锌的比例为约5-约150的光催化剂组合物应用至植物表面。
本发明还提供一种用于防止或处理表面上微生物疾病或感染的方法,其包括将包括锌(Zn)掺杂的二氧化钛(TiO2)纳米颗粒、二氧化钛和锌的比例为约5-约150的光催化剂组合物应用至用人造光照明的表面。本文所使用的“表面”指无生命物体或包括植物的有生命物体。
此外,本发明提供一种用于防止或处理植物中微生物疾病和感染的方法,其包括将包括至少一种掺杂剂的二氧化钛(TiO2)纳米颗粒光催化剂组合物应用至植物的表面,其中所述掺杂剂的添加增加了对约200纳米-500纳米范围的光的吸收度,且其中对波长大于约450纳米的光的吸收度低于对波长小于约350纳米的光吸收度的50%。优选的,所述掺杂剂的添加增加了对约350纳米-450纳米范围的光的吸收度。可用于所述光催化剂组合物的掺杂剂选自下组:Ag、Zn、Si、C、N、S、Fe、Mo、Ru、Cu、Os、Re、Rh、Sn、Pt、Li、Na、K、及其组合。特别优选的掺杂剂是Zn、Si、和Ag。
此外,本发明提供一种光催化剂组合物,所述光催化剂组合物吸收约200纳米-约500纳米波长范围内的电磁辐射,且对波长大于约450纳米的光的吸收度低于对波长小于约350纳米的光吸收度的50%。所述组合物包括用至少一种掺杂剂掺杂的二氧化钛纳米颗粒,其中所述掺杂剂打乱所述二氧化钛纳米颗粒的晶体晶格结构,并由此改变所述组合物的吸收光谱。
本发明提供光催化材料,所述光催化材料在所选的基本上不干涉光合作用的波长范围内可吸收更高比例的可用电磁能量。但是,应理解本发明的应用不限于农业应用,因为对波长低于500纳米的光能应用的改进可为各种环境带来好处。本发明不限于光催化好处的任意具体的理论或机制,因为光催化可通过多种机制提供好处,且我们没有将本发明限制于某一具体的组合物或某一类型的光催化剂。此外,用于制造这种材料的合成方法也可以变化,且我们没有将本发明限制于某一具体的制造模式。
此外,虽然这里给出的示例都是基于TiO2的,但各种其他光催化剂如Fe2O3也可进行类似的优化,如可包含不同水平的SnO2,且本发明中考虑了其他光催化剂。本发明通过使用将本发明的制剂分散在水中以方便的应用至各种表面来阐述,但本发明的考虑的制剂还可在其他溶剂中分散,也可使用着色剂,分散剂、载体和两性试剂来促进在选定环境中方便或均一的应用。
除非在工作实施例中或者另有说明,本文使用的表示成分用量的所有数字应理解为在所有情况中都用词“约”修饰。
如本文所用,术语“至少一种”表示一种或多种,因而包括单个组分以及混合物/组合。
如本文所用,术语“包含”(及其语法变形)表示具“有”或者“包括”的包容性,且不是排他性的“只包括”。
本文中所用术语“一种”和“该”包括复数形式和单数形式。
如本文所使用,术语“掺杂的”或“掺杂”应理解为包括将一种或更多种杂质(如掺杂剂,掺杂试剂)引入一种材料,目的是改性所述材料的性质。
术语“处理(treatment)”和“处理(treating)”包括减少事先存在的微生物疾病或感染。
术语“防止(prevention)”和“防止(prophylaxis)”包括在个体或群体中的疾病或感染的发生或严重程度减少。
通过下面的实施例,将进一步理解本发明,这些实施例用于阐述但不用于限定本发明。
实施例
实施例1:
在350纳米-500纳米的波长范围内,比较了纳米级TiO2与用2种不同锌水平和SiO2掺杂的TiO2的吸收特征。通过改进的溶胶-凝胶法制备纳米颗粒组合物,以制备包含平均尺寸为6-7纳米的锐钛矿TiO2纳米颗粒的制剂。包含锌作为掺杂剂以提供低锌含量(0.125%,相对于TiO2)或高锌含量(1.25%,相对于TiO2)。当SiO2是一种附加掺杂剂时,它以10%(相对于TiO2)的数量存在。干燥所述制剂,且用标准方法测得粉末的扩散反射光谱(DRS)。显示了从ASTM G173-03标准获得的在光谱范围的太阳辐射(半球,37度倾斜)作为参考。(见图1)。
检查后明显的发现,在光谱的近UV区和紫外区,用杂原子掺杂的TiO2吸收比类似的但未掺杂的TiO2更强。在400-450纳米的区域内,掺杂的制剂吸收多于25-35百分数的可用能量,太阳辐射在该区域相对较高,但仍然在植物的主要光合作用光谱之外。
实施例2:UV照明下,用Zn和SiO
2
掺杂的各种TiO
2
制剂的光催
化活性。
在标准化系统中测试了实施例1中所述的4种制剂的光催化活性。将每种制剂以大约8000ppm的浓度悬浮于水中,并用自动化高体积低压喷雾器应用至一玻璃面板,然后干燥24小时。这些面板都连接至玻璃管形成容器,在容器中放入30毫升的甲基蓝水溶液,浓度为在664纳米下的光密度为2.3。用玻璃面板覆盖所述管,并经受提供354纳米紫外照明的灯(GE零件号F18T8/BLB)的照明,能量密度为大约0.5mW/cm2。该灯不提供波长低于300纳米和大于400纳米的光。在48小时的时段内监控每一样品中甲基蓝溶液的光密度,结果如图2所示。
图2显示纳米涂层导致光密度下降,这是由有机染料甲基蓝的光催化降解引起的。具有更高数量掺杂剂的涂层具有最快的下降,与它在UV范围内(354纳米)对来自灯的光更大的吸收度是相一致的。
实施例3:可见光照明下,用Zn和SiO
2
掺杂的各种TiO
2
制剂的
光催化活性。
在第二系统中测试了实施例1中所述的4种制剂的光催化活性,其中实验用的照明变成更加紧密模拟的相关照明如日光或室内光,它们在使用紫外能量的实施例2中是没有的。此外,对于该实施例所述纳米颗粒制剂是在20mM的pH7.2的磷酸盐缓冲溶液中作为胶体悬浮液而不是静态的表面来评估的。实验是在96孔板形式上执行的,其中每个孔都包含甲基蓝(观察到的OD655范围为0.05-0.5)和纳米颗粒制剂或适当的对照,且最终体积为200微升。用来自喜万年格罗鲁斯(Sylvania Gro-Lux)的两灯(型号,F20T12GRO/AQ)照明所述板,距离为20厘米。这些灯在低于400纳米时只发射总发射能量的2%,在380-500纳米之间则发射总发射能量的约36%,峰值在436纳米(参见,技术信息简报“喜万年(Sylvania)荧光灯的光谱功率分布”,欧司朗喜万年(Osram Sylvania),www.sylvania.com)。
用已知分析技术ICP-AES(电感耦合等离子体原子发射光谱法)独立的确认在该实施例中测试的4种制剂的组成,表明它们如实施例1所述,具有相同的TiO2含量,但Si和Zn的组成不同。将所述纳米颗粒制剂在缓冲溶液中稀释至每种制剂的二氧化钛最终浓度为75ppm,每种制剂都有20个重复的孔。在黑暗中短暂的平衡后,将每一板暴露于照明之下,同时摇晃,然后用美谷分子仪器(Molecular Devices)的SpectraMax Plus光谱仪多次测量655纳米处的光密度。测量因为每种制剂而观察到的光密度的线性下降,得到表1所总结的速率:
表1:
试验1 | 试验2 | |
TiO2,低Zn | 0.0017* | 0.0016 |
TiO2,低Zn,高Si | 0.0020 | 未测试 |
TiO2,高Zn,高Si | 0.0019 | 未测试 |
只有TiO2 | 未测试 | 0.0013 |
*所有报告的值都是655纳米处光密度每分钟的下降。
显然,与未掺杂的TiO2制剂相比,所有掺杂的TiO2制剂都具有显著增加的速率(25%-50%)。光催化活性速率增加的量级与400纳米-450纳米范围内光能量吸收的增加高度一致,所述光能量吸收的增加在实施例1所述的光谱中是显而易见的。
实施例4:使用白炽光在表面上光催化杀灭植物病原体穿孔疮痂
病菌(Xanthomonas perforans)。
用0.5毫升的几种类型纳米颗粒悬浮液(TiO2,TiO2/Ag或TiO2/Zn)的一种分别涂覆无菌盖玻片。所述纳米颗粒组合物,可与实施例2的哪些相比拟,是通过改性的溶胶-凝胶方法制备的,从而制备包含平均尺寸为6-7纳米的锐钛矿TiO2纳米颗粒的制剂,且用Ag或Zn掺杂,TiO2与掺杂剂的比例分别为大约400:1和大约800:1。将盖玻片在无菌环境下干燥。将包含107耐铜穿孔疮痂病菌(Xanthomonas perforans)的0.1毫升水的标准化接种物应用至处理的或未处理的盖玻片。然后,所述盖玻片要么在照明密度为3x104勒克斯的白炽光下照明,或维持在黑暗环境中。以一定间隔,将盖玻片放置于含10毫升无菌水的无菌离心管中,并蜗旋。通过离心(14000x g,3分钟)收集回收的细菌,并悬浮于1毫升的无菌水中。在所得悬浮液中存活细菌的数量,通过标准的板稀释法计数。结果见图3。
图3的测试表明纳米颗粒处理导致了时间依赖和光依赖的细菌杀灭,但在未处理的盖玻片中没有观察到所述细菌杀灭。掺杂制剂的杀灭速率比未掺杂TiO2的更快。感兴趣的是未照明的TiO2/Zn和TiO2没有发生细菌杀灭,但TiO2/Ag甚至在未照明时也一些细菌杀灭,同时表明含Ag的材料本身就有更大的毒性,以及需要照明为光催化抗细菌效应提供能量。
实施例5:用光催化材料处理,可减少番茄植物被叶斑病病原体
穿孔疮痂病菌(Xanthomonas perforans)的感染。
植物的许多细菌疾病都是由先前存在的细菌群体的不可控扩张引起的,它们数量低的时候不会引起疾病。因此,在农业中控制这些疾病的一种主要方法是减少存活的细菌群,从而消除可能给所述植物带来损坏和疾病的细菌的过量扩张。番茄的细菌叶斑病是一种经常寻求这种防止方法的疾病系统。
番茄栽培变种BHN602的种子批被自然的用穿孔疮痂病菌(Xanthomonas perforans)菌株Xp1-7感染。当被感染的植物处于3-4叶阶段时,用未稀释的或稀释10倍的纳米颗粒(TiO2,TiO2/Ag和TiO2/Zn)处理。所述纳米颗粒组合物,可与实施例4的哪些相比拟,是通过改性的溶胶-凝胶方法制备的,从而制备包含平均尺寸为6-7纳米的锐钛矿TiO2纳米颗粒的制剂,且用Ag或Zn掺杂,TiO2与掺杂剂的比例分别为大约400:1和大约800:1。如图4所示,所述纳米颗粒以7,500-10,000ppm或5,000-8,000ppm的浓度悬浮于水中。每天灌溉植物,使土壤水分水平保持在85-95%,且每天用水对植物喷雾15分钟,以促进病原体的生长。每种处理都测试3植物,且该实验装置完全采用随机设计。记录处理前后两周的细菌斑点病变。结果见图4。误差棒代表平均值的标准误差。
显然,所有纳米颗粒处理都减少了细菌斑点病变的数目。在本实验中,每种制剂的效应都没有因为稀释10倍而受到明显影响。应注意的是,与未掺杂的TiO2相比,将掺杂剂添加到TiO2纳米颗粒改善了效应,这与增加的光催化活性是一致的。
实施例6:由丁香假单胞菌丁香致病变种(Pseudomonas syringae
pv.savastonoi)引起的橄榄结的防护。
橄榄结是橄榄树的一种疾病,由一种能动革兰氏阴性细菌丁香假单胞菌丁香致病变种(Pseudomonas syringae pv.savastonoi)引起,在橄榄树中创建肿瘤(结)。组织在这些结中幸存,且在潮湿的时候分散,于是所述组织通过伤口进入新的区域,该伤口包括叶和花脱落的疤痕以及由风、修剪或霜等机械伤害诱发的那些伤口。这些结抑制植物的正常生长,并降低果实产量。和植物的许多其他细菌疾病一样,在疾病前减少存活的细菌群可明显的防止或减少橄榄结的发生,且用于减少细菌群的方法是农业中一种常用的方法。
在温室研究中,给叶片疤痕伤口接种105或108的丁香假单胞菌(P.syringae)细菌,然后用手动喷雾器喷洒如实施例1所述的TiO2/低Zn制剂的50倍稀释液,因此提供250ppm的水相悬浮液。也测试了其他的试剂作为对照。这些对照试剂包括:Vantocil B(聚六亚甲基双胍盐酸盐和氯化正烷二甲基铵的组合),购自瑞士巴塞尔的阿克化学公司(Arch Chemicals),该公司现在是龙沙集团公司(Lonza Goup)的一部分;Deccosan321(几种季铵盐的混合物,购自美国加利福尼亚州蒙罗维亚的德克斯拉奇公司(Decco Cerrexagri);Kasumin(春日霉素盐酸盐,购自美国北卡罗琳娜州卡里的亚莉丝塔生命科学公司(ArystaLifescience);Citrox(柠檬油,洗涤剂和过氧化氢的合适的混合物,由美国宾夕法尼州里德的麦克产品公司(Misco Products Corporation)制造;以及Kocide3000(氢氧化铜,购自美国杜邦农作物保护(DuPont CropProtection)。即使这样会减少所述接种区域的光的数量,用单层封口膜包覆接种的区域一天,以维持足够的湿度,从而确保高的感染速率。
一个月后观察到结形成的第一证据,且第一次定量的评估在7星期后执行。在更低的攻击性接种时,纳米颗粒TiO2/低Zn处理(图5中表示为AgriTitan)是完全有效的,与其他大多数测试的试剂类似(图5).在更高的攻击性接种时,用250ppm TiO2/低Zn的喷洒处理继续完全有效,与1000ppm氢氧化铜的现行标准处理类似。所有其他测试的试剂都更没那么有效(图5)。
实施例7:番茄田间实验
在温室实验中使用的用Zn掺杂的TiO2制剂被选定用于田间试验。选择Zn作为进一步研究中的掺杂剂是因为,它已经被美国环境保护署批准为最低风险的杀虫剂,这是其他潜在掺杂剂无法媲美的地位。执行田间试验是为了比较用Zn以800:1的比例掺杂的TiO2(制备为在H2O中的0.7%的胶体悬浮液)和标准处理用于防止或控制番茄植物叶斑病的效率。每个处理组包括48颗植物(12颗每小区,4重复样本),且该试验完全采用随机设计。在水中稀释TiO2/Zn以提供多种应用比率。对照包括单独的硫酸铜制剂,硫酸铜制剂与代森锰(manzate)的结合,以及无处理。
在植入后的第一个星期开始以周为间隔(8次)向植物喷洒测试材料。疾病的严重程度以月为间隔用无量纲的12点量表评级,以评估林冠(canopy)被细菌叶斑病影响的百分数(霍沙夫(Horsfall)等,Phytopathology,卷35,655,摘要,1945年)。将这些值转化成中点-百分数,并用于生成病害发展曲线下面积(AUDPC,Area Under DiseaseProgression Curve)。此外,从田间试验获取基于USDA评级的商品化产率数据,以决定所述纳米级制剂是否对番茄植物有任何除草作用。结果列于表2和表3。
表2:TiO2/Zn对番茄(变种BHN602)发生细菌叶斑病的影响,显示为病害发展曲线下面积(AUDPC)的平均值。
处理 | 稀释 | AUDPCy |
TiO2/Zn | X/10x | 800.6cz |
X/20 | 950.3bc | |
X/40 | 1000.1b | |
X/60 | 1033.4ab | |
X/80 | 933.6bc | |
X/100 | 1050.0ab | |
铜 | 1050.0ab | |
铜+代森锰 | 1033.4ab | |
未处理 | 1181.3a |
x X代表未稀释的TiO2/Zn制剂。
y疾病的严重程度用一种无量纲的12点量表即火沙夫-贝罗特量表(Horsfall-Barratt scale)评级,以评估林冠(canopy)被细菌斑病影响的百分数。将这些值转化成中点-百分数,并用于生成AUDPC。
z具有相同字母的柱平均值表明基于SNK检验(Student NewmanKeuls test)时,它们没有显著不同(P≤0.05)。
表1总结了田间试验的结果,表明TiO2/Zn提供比常规处理更好的对自发叶斑病的防护。在两两对比中,1:10稀释的TiO2/Zn具有统计学差异的好于其他对照处理,其AUDPC减少了20%。此外,当把所有TiO2/Zn稀释液作为一组,和把对照作为一组时,也具有统计学差异(p<0.05)。
表3:TiO2/Zn对番茄产率的影响(kg/ha)。
x X代表未稀释的TiO2/Zn制剂。
z具有相同字母的柱平均值表明基于SNK检验(Student NewmanKeuls test)时,它们没有显著不同(P≤0.05)。
表3总结了田间试验的结果,表明TiO2/Zn对可商品化番茄的产率没有不利影响。事实上,对于用TiO2/Zn处理的组,还观察到产率上升;用稀释10倍的TiO2/Zn处理的植物的可商品化总量比任意对照的产率都高出20%以上。虽然因为每一组中的产率有变化使在单独的两两对比时没有统计学的差异,但是当TiO2/Zn的6稀释液的“可商品化总量”结果作为一组,与3对照处理作为一组比较时,是统计学差异的(p<0.05)。
实施例8
在下一个生长季节,重复执行实施例7。方案与实施例7相同,其中,每次用常规的高体积低压压缩空气喷洒器将TiO2/低Zn水溶液的各种稀释液应用至番茄,采用完全随机设计且有适当的对照。下文的表4显示了病害发展的结果,表明对疾病的控制具有浓度依赖性。不幸的是,因为在收获季节前一场冰雹造成了严重的损坏,所以该实验没有得到产率数据。
表4:TiO2/Zn对番茄培育变种‘BHN602’发生细菌斑病的影响,显示为病害发展曲线下面积(AUDPC)的平均值。
x X代表未稀释的TiO2/Zn制剂。
y疾病的严重程度用一种无量纲的12点量表即火沙夫-贝罗特量表(Horsfall-Barratt scale)评级,以评估林冠(canopy)被细菌斑病影响的百分数。将这些值转化成中点-百分数,并用于生成AUDPC。
z具有相同字母的柱平均值表明基于SNK检验(Student NewmanKeuls test)时,它们没有显著不同(P≤0.05)。因为在收获日一周前的一场冰雹造成了严重的损坏,所以没能得到产率数据。
实施例9
在下一生长季节,进行了在番茄斑病系统中的第3次田间试验。基于实施例7和实施例8的结果,我们没有测试更多的TiO2/Zn稀释应用比率,因此清楚测定应用比率关系的能力下降了。但是,总体的结果仍然相同(表5)。
表5:TiO2/Zn对番茄培育变种‘BHN602’发生细菌斑病的影响,显示为病害发展曲线下面积(AUDPC)的平均值,以及番茄果实的产率。
x X代表未稀释的TiO2/Zn制剂。
y疾病的严重程度用一种无量纲的12点量表即火沙夫-贝罗特量表(Horsfall-Barratt scale)评级,以评估林冠(canopy)被细菌斑病影响的百分数。将这些值转化成中点-百分数,并用于生成AUDPC。
z具有相同字母的柱平均值表明基于SNK检验(Student NewmanKeuls test)时,它们没有显著不同(P≤0.05)。
因此,在该第3田间试验中,再次表明以疾病严重程度和果实产率为基础,TiO2/低Zn的应用在控制番茄的细菌斑病上具有活性。稀释比例为1:10时,TiO2/Zn是统计学的优于单一试剂铜或未处理的对照。
实施例10:如实施例7和8所制备的TiO
2
/Zn对白粉病的真菌病
因试剂耳单丝壳(Sphaerotheca fuliginea)/黄瓜白斑病菌(Erysiphe
cichoracearum)分生孢子发展的影响。
在温室中,标记在叶片上具有大约相同数目病变的黄瓜植物,以用于实验。这些叶片用于所有的处理。在图6中,“n”代表在这些叶片中的病变的平均数。所述病变在(0.1-0.6cm)的范围。用手动喷洒器将TiO2/Zn制剂1以1/50和1/100X的浓度喷洒至所述植物。未处理的植物用无菌蒸馏水喷洒。所述植物在温室中保存48小时。从植物中取下叶片,并在显微镜下观察病变,以判断是否存在分生孢子。(见图6)。
这些结果表明,所述光催化制剂的应用显著的降低了对白粉病的繁殖至关重要的产生分生孢子的能力。
需着重指出的是,在示例性实施方式中显示的方法和步骤的构造和排布仅仅是示例性的。虽然,本文只详细的公开了几个本发明的实施方式,本领域技术人员应易于理解,在没有实质上背离所附权利要求书限定的主题内容的新教导和益处的前提下可以有一些改良。因此,所有这样的改良都包括在所附权利要求限定的本发明的范围。任意过程或方法步骤的顺序或序列都可根据替换的实施方式而改变或重新排序。在不偏离所附权利要求表达的本发明的精神的前提下,可在实施方式的设计、运行条件和排布进行其他替代、改良、变化和省略。
本说明书引用的所有出版物、专利及专利申请均通过引用纳入本说明书,一如各出版物、专利或专利申请具体且单独地通过引用纳入本说明书。如若出现不一致,则以本发明为准。
Claims (24)
1.一种光催化剂组合物,所述光催化剂组合物包括锌(Zn)掺杂的二氧化钛(TiO2)纳米颗粒,二氧化钛和锌的比例为约5-约150。
2.如权利要求1所述的光催化剂组合物,其特征在于,所述二氧化钛纳米颗粒的平均粒度为约2纳米-约20纳米。
3.一种光催化剂组合物,所述光催化剂组合物包括锌(Zn)掺杂的二氧化钛(TiO2)纳米颗粒,以及二氧化硅(SiO2),二氧化钛和锌的比例为约5-约150,以及二氧化钛和二氧化硅的比例为约1-约500。
4.如权利要求3所述的光催化剂组合物,其特征在于,所述二氧化钛和二氧化硅的比例为约3-约20。
5.如权利要求3所述的光催化剂组合物,其特征在于,所述二氧化钛纳米颗粒的平均粒度为约2纳米-约20纳米。
6.如权利要求3所述的光催化剂组合物,其特征在于,所述组合物包括:
(A)约5000-约8000ppm的二氧化钛,
(B)约50-约100ppm的锌,以及
(C)约500-约1000ppm的二氧化硅。
7.一种用于处理或防止农作物或观赏植物中微生物疾病和感染的方法,其包括:将包括锌掺杂的二氧化钛纳米颗粒、且二氧化钛和锌的比例为约5-约150的光催化剂组合物应用至农作物或观赏植物的表面。
8.如权利要求7所述的方法,其特征在于,所述二氧化钛纳米颗粒的平均粒度为约2纳米-约20纳米。
9.如权利要求7所述的方法,其特征在于,所述光催化剂组合物还包括二氧化硅(SiO2)。
10.如权利要求9所述的方法,其特征在于,所述二氧化钛和二氧化硅的比例为约1-约500。
11.如权利要求9所述的方法,其特征在于,所述二氧化钛和二氧化硅的比例为约3-约20。
12.如权利要求9所述的方法,其特征在于,所述二氧化钛纳米颗粒的平均粒度为约2纳米-约20纳米。
13.如权利要求9所述的方法,其特征在于,所述光催化剂组合物包括:
(A)约5000-约8000ppm的二氧化钛,
(B)约50-约100ppm的锌,以及
(C)约500-约1000ppm的二氧化硅。
14.一种用于增加植物的农作物产量的方法,其包括:将包括锌(Zn)掺杂的二氧化钛(TiO2)纳米颗粒、二氧化钛和锌的比例为约5-约150的光催化剂组合物应用至植物的表面。
15.如权利要求14所述的方法,其特征在于,所述二氧化钛纳米颗粒的平均粒度为约2纳米-约20纳米。
16.一种用于处理或防止表面微生物感染的方法,其包括:将包括锌(Zn)掺杂的二氧化钛(TiO2)纳米颗粒、二氧化钛和锌的比例为约5-约150的光催化剂组合物应用至用人造光照明的表面。
17.如权利要求16所述的方法,其特征在于,所述光催化剂组合物还包括二氧化硅,其中所述二氧化钛和二氧化硅的比例为约1-约500。
18.如权利要求17所述的方法,其特征在于,所述二氧化钛和二氧化硅的比例为约3-约20。
19.如权利要求17所述的方法,其特征在于,所述二氧化钛纳米颗粒的平均粒度为约2纳米-约20纳米。
20.如权利要求17所述的光催化剂组合物,其特征在于,所述组合物包括:
(A)约5000-约8000ppm的二氧化钛,
(B)约50-约100ppm的锌,以及
(C)约500-约1000ppm的二氧化硅。
21.如权利要求16所述的方法,其特征在于,所述表面是非生命物体。
22.一种用于处理或防止植物中微生物疾病和感染的方法,其包括:将包括用至少一种掺杂剂掺杂的二氧化钛(TiO2)纳米颗粒的光催化剂组合物应用至植物的表面,其中所述掺杂剂的添加增加了对约200纳米-500纳米范围的光的吸收度,且其中对波长大于约450纳米的光的吸收度低于对波长小于约350纳米的光吸收度的50%。
23.如权利要求22所述的方法,其特征在于,所述掺杂剂的添加增加了对约350纳米-450纳米范围的光的吸收度。
24.如权利要求22所述的方法,其特征在于,所述至少一种掺杂剂选自下组:Ag、Zn、Si、C、N、S、Fe、Mo、Ru、Cu、Os、Re、Rh、Sn、Pt、Li、Na和K。
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