CN113105895A - 一种能促进植物生长的荧光粉及其制备方法 - Google Patents
一种能促进植物生长的荧光粉及其制备方法 Download PDFInfo
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- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 3
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- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 2
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 2
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- 229910001940 europium oxide Inorganic materials 0.000 claims description 2
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 claims description 2
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 2
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- 229910000026 rubidium carbonate Inorganic materials 0.000 claims description 2
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 2
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- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
- A01G7/00—Botany in general
- A01G7/06—Treatment of growing trees or plants, e.g. for preventing decay of wood, for tingeing flowers or wood, for prolonging the life of plants
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
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- C01B25/00—Phosphorus; Compounds thereof
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Abstract
本发明公开一种能促进植物生长的荧光粉及其制备方法，荧光粉是Eu2+掺杂于包含Rb+的卤磷酸盐形成的荧光粉，具有Pnma的晶体结构。化学式为RbxK2‑xCa1‑yPO4F:yEu2+。按化学表达式中各化学组分的化学计量比称取各原料，研磨至微米级，混合均匀，得原料粉末；置于通入还原气氛的环境中，升温至850℃，煅烧；自然冷却至室温，研磨，制得能促进植物生长的荧光粉。该荧光粉通过高温固相法烧结而成，在紫外灯或者太阳光紫外到蓝光区域的光照射下，发出有利于植物生长的红光，可提高光能利用率、促进植物生长，且成本低、无污染、效率高、不消耗电能。
Description
技术领域
本发明属于固体发光材料技术领域，涉及一种红色发光材料，特别涉及一种经紫外灯或太阳光照射后发出红光的能促进植物生长的荧光粉；本发明还涉及一种该荧光粉的制备方法。
背景技术
植物通过色素进行光合作用合成碳水化合物作为其生长的基本养料，植物在发芽和果实成熟的过程中需要光提供能量，因此光的调节是调控植物生长的重要手段之一。研究发现，植物对光的吸收主要是通过叶绿素和光敏色素进行，叶绿素主要蓝光（400nm～500nm）和橙红光（600nm～700nm）；光敏色素吸收红光及深红（650nm～750nm）区域的光，分别对应于植物的光向性、光合作用和光形态发生。其中对植物生长最重要的是位于红光区域的光（600nm～700nm），因为红光在植物发育和成熟阶段影响很大。除此之外植物很少吸收太阳中其他范围的光，植物的生长过程中红光接触的比较少，因此对太阳光的利用率很低；并且太阳光中的红光部分相较于蓝光部分更弱。因此，提高植物对光的利用率对植物的生长有着重要的影响，提高植物光能利用率可以大大提高植物的生长速度并且提高产量。到目前为止，对植物的培育大多使用LED植物灯，但是许多植物灯的光谱曲线较窄或者不满足植物光合作用吸收的光谱曲线，光源能量利用率不高，不适于植物生长；除此之外，LED芯片本身价格较高，且需要用电，间接增加了种植成本，难以大范围推广。因此，开发一种价格低廉且可提高植物对太阳辐射能利用率的新型荧光粉材料很有必要。
发明内容
本发明的目的是提供一种能促进植物生长的荧光粉，满足植物生长的需求。
本发明的另一个目的是提供一种上述荧光粉的制备方法。
为实现上述目的，本发明所采用的技术方案是：一种能促进植物生长的荧光粉，是Eu2+掺杂于包含Rb+的卤磷酸盐形成的荧光粉，具有Pnma的晶体结构；该荧光粉的化学式为RbxK2-xCa1-yPO4F:yEu2+，其中，x=0.2、0.4、0.6、0.8、1.0、1.5或2.0；y=0.01～0.06。
本发明所采用的另一个技术方案是：一种上述荧光粉的制备方法，具体按以下步骤进行：
步骤1：按化学表达式RbxK2-xCa1-yPO4F:yEu2+中各化学组分的化学计量比分别称取各原料，所取各原料为各化学组分的化合物；
铷化合物采用碳酸铷（Rb2CO3）、含铷的氢氧化物、含铷的硝酸盐、含铷的碳酸盐、含铷的硫酸盐或含铷的磷酸盐；
钾化合物采用碳酸钾（K2CO3）、含钾的氢氧化物、含钾的硝酸盐、含钾的硫酸盐或含钾的磷酸盐；
钙化合物采用碳酸钙（CaCO3）、含钙的氢氧化物、含钙的硝酸盐、含钙的硫酸盐或含钙的磷酸盐；
磷化合物采用磷酸二氢铵（NH4H2PO4）或含磷的氢氧化物；
氟化合物采用氟化钾（KF）、含氟的氢氧化物、含氟的硝酸盐、含氟的碳酸盐、含氟的硫酸盐或含氟的磷酸盐；
铕化合物采用氧化铕（Eu2O3）、含铕的氢氧化物、含铕的硝酸盐、含铕的碳酸盐、含铕的硫酸盐或含铕的磷酸盐；
将所取各原料研磨至微米级，混合均匀，制得原料粉末；
步骤2：将原料粉末置于通入还原气氛的环境中，以5℃/min的升温速率升温至850℃，煅烧4小时；自然冷却至室温，研磨烧结物，制得能促进植物生长的荧光粉。
还原气氛可以采用三种气体：第一种是氨气（NH3）；第二种是按体积百分比由5～25%的氢气（H2）和95～75%的氮气（N2）组成的混合气体；第三种是按体积百分比由5～25%的一氧化碳（CO）和95～75%的氮气（N2）组成的混合气体。
本发明荧光粉通过高温固相法烧结而成，工艺简单、无污染、无任何有害物质产生、绿色环保、成本低。激发光谱覆盖区域较宽，可吸收太阳光中的紫外光到蓝光区域的管，在红光区有很强的发射强度，可提高光能利用率，更有利于促进植物的生长。该荧光粉发光能力强、效率高，不消耗电能。
附图说明
图1是实施例1制得荧光粉的XRD图与标准卡片的对照图。
图2是实施例1制得的荧光粉的激发和发射光谱图。
图3是实施例1制得荧光粉的电镜扫描图。
图4是实施例1～6制得荧光粉的XRD图与标准卡片的对照图。
图5是实施例1～6制得荧光粉的发射光谱对照图。
图6是实施例7～13制得荧光粉与对比例荧光粉的发射光谱对比图。
图7是实施例7～13制得荧光粉与对比例荧光粉的激发光谱对比图。
具体实施方式
下面结合附图和具体实施方式对本发明进行详细说明。
实施例1
按Rb0.2K1.8Ca0.99PO4F:0.01Eu分子式所示的化学计量比，称取0.3464g的Rb2CO3、0.828g的K2CO3、1.485g的CaCO3、1.725g的NH4H2PO4、0.8715g的KF和0.0264g的Eu2O3。将称取的各原料充分研磨并混合均匀后，放入氧化铝坩埚，置于管式炉中，通入按体积比由5%的H2和95%的N2组成的还原气氛，以5℃/min的升温速率升温至850℃，煅烧4小时，随炉冷却至室温，研磨煅烧物，制得能促进植物生长的荧光粉。
实施例2
按Rb0.2K1.8Ca0.98PO4F:0.02Eu化学式所示的化学计量比，称取Rb2CO3、K2CO3、CaCO3、NH4H2PO4、KF和Eu2O3。按实施例1的方法制得能促进植物生长的荧光粉。
实施例3
按Rb0.2K1.8Ca0.97PO4F:0.03Eu化学式所示的化学计量比，称取Rb2CO3、K2CO3、CaCO3、NH4H2PO4、KF和Eu2O3。按实施例1的方法制得能促进植物生长的荧光粉。
实施例4
按Rb0.2K1.8Ca0.96PO4F:0.04Eu化学式所示的化学计量比，称取Rb2CO3、K2CO3、CaCO3、NH4H2PO4、KF和Eu2O3。按实施例1的方法制得能促进植物生长的荧光粉。
实施例5
按Rb0.2K1.8Ca0.95PO4F:0.05Eu化学式所示的化学计量比，称取Rb2CO3、K2CO3、CaCO3、NH4H2PO4、KF和Eu2O3。按实施例1的方法制得能促进植物生长的荧光粉。
实施例6
按Rb0.2K1.8Ca0.94PO4F:0.06Eu化学式所示的化学计量比，称取Rb2CO3、K2CO3、CaCO3、NH4H2PO4、KF和Eu2O3。按实施例1的方法制得能促进植物生长的荧光粉。
实施例1制得荧光粉的XRD图谱，如图1所示。图中各峰峰形、峰位与PDF卡片一一对应，证明制得的粉末的物相为单相。
实施例1制得荧光粉的激发和发射光谱图，见图2，激发光谱为比较宽的吸收光谱(300～450nm)，激发峰峰值位于380nm；发射光谱显示了一个很宽的发射峰，其峰值在650nm处。通过光谱图可以发现，Rb0.2K1.8Ca0.99PO4F:0.01Eu在紫外光300～380nm区域有吸收，从而避免了太阳光中紫外光对植物的损伤。图3为实施例1制备的荧光粉的扫描电镜图，从图中可以看出，荧光粉颗粒粒径在10μm以上，颗粒分布均匀，说明荧光粉结晶性好。
实施例1～6制得荧光粉的XRD图谱，如图4所示，图中各峰峰形、峰位与PDF卡片一一对应，证明实施例1～6制得荧光粉的物相均为单相。
实施例1～6制得荧光粉的发射光谱图，见图5。从图中可以看出，实施例2制得荧光粉的发光强度最高，所产生的橙红光最强，可以为植物提供更强的红光。
实施例7
按Rb0.2K1.8Ca0.98PO4F:0.02Eu化学式所示的化学计量比，称取Rb2CO3、K2CO3、CaCO3、NH4H2PO4、KF和Eu2O3。将所取各原料研磨至微米级，混合均匀，制得原料粉末；将原料粉末置于通入氨气的环境中，以5℃/min的升温速率升温至850℃，煅烧4小时；自然冷却至室温，研磨烧结物，制得能促进植物生长的荧光粉。
实施例8
按Rb0.4K1.6Ca0.98PO4F:0.02Eu化学式所示的化学计量比，称取Rb2CO3、K2CO3、CaCO3、NH4H2PO4、KF和Eu2O3。将所取各原料研磨至微米级，混合均匀，制得原料粉末；将原料粉末置于通入按体积百分比由25%的一氧化碳和75%的氮气组成还原气氛的环境中，以5℃/min的升温速率升温至850℃，煅烧4小时；自然冷却至室温，研磨烧结物，制得荧光粉。
实施例9
按Rb0.6K1.4Ca0.98PO4F:0.02Eu化学式所示的化学计量比，称取Rb2CO3、K2CO3、CaCO3、NH4H2PO4、KF和Eu2O3。将所取各原料研磨至微米级，混合均匀，制得原料粉末；将原料粉末置于通入按体积百分比由5%的一氧化碳和95%的氮气组成还原气氛的环境中，以5℃/min的升温速率升温至850℃，煅烧4小时；自然冷却至室温，研磨烧结物，制得荧光粉。
实施例10
按Rb0.8K1.2Ca0.98PO4F:0.02Eu化学式所示的化学计量比，称取Rb2CO3、K2CO3、CaCO3、NH4H2PO4、KF和Eu2O3。将所取各原料研磨至微米级，混合均匀，制得原料粉末；将原料粉末置于通入按体积百分比由25%的氢气和75%的氮气组成还原气氛的环境中，以5℃/min的升温速率升温至850℃，煅烧4小时；自然冷却至室温，研磨烧结物，制得荧光粉。
实施例11
按Rb1.0K1.0Ca0.98PO4F:0.02Eu化学式所示的化学计量比，称取Rb2CO3、K2CO3、CaCO3、NH4H2PO4、KF和Eu2O3。按实施例7的方法制得荧光粉。
实施例12
按Rb1.5K0.5Ca0.98PO4F:0.02Eu化学式所示的化学计量比，称取Rb2CO3、K2CO3、CaCO3、NH4H2PO4、KF和Eu2O3。按实施例8的方法制得荧光粉。
实施例13
按Rb2.0Ca0.98PO4F:0.02Eu化学式所示的化学计量比，称取Rb2CO3、CaCO3、NH4H2PO4、KF和Eu2O3。按实施例9的方法制得荧光粉。
对比例
取现有技术中的荧光粉K2CaPO4F:Eu。
对比例中的荧光粉K2CaPO4F:Eu具有近紫外光（NUV）激发的LED照明的深红色发射(H. Daicho et al., Chem. Commun., 54 (2018) 884.)。但是荧光粉K2CaPO4F:Eu的发射波长太长（610～750nm），不仅导致LED照明能量损失而且导致植物生长能量损失。为了解决现有技术中存在的问题，本发明在荧光粉K2CaPO4F:Eu中掺杂Rb，用Rb+取代K+位点，使得晶体场强度以及斯托克斯位移变小，从而在不改变激发波长的情况下，使得荧光粉的发射显著地向较短的波长移动，如图6（λex=380nm）和图7（λem=图6中的每个峰值波长）所示。通过这种斯托克斯转变，能够将荧光粉的发射波长调整到最合适的范围，即600～720nm，以便植物在利用NUV和浅蓝色的阳光下生长。
Claims (6)
1.一种能促进植物生长的荧光粉，其特征在于，该荧光粉是Eu2+掺杂于包含Rb+的卤磷酸盐形成的荧光粉，具有Pnma的晶体结构。
2.如权利要求1所述的能促进植物生长的荧光粉，其特征在于，该荧光粉的化学式为RbxK2-xCa1-yPO4F:yEu2+，其中，x=0.2、0.4、0.6、0.8、1.0、1.5或2.0；y=0.01～0.06。
3.一种根据权利要求2所述能促进植物生长的荧光粉的制备方法，其特征在于，具体按以下步骤进行：
步骤1：按化学表达式RbxK2-xCa1-yPO4F:yEu2+中各化学组分的化学计量比分别称取各原料，将所取各原料研磨至微米级，混合均匀，制得原料粉末；
步骤2：将原料粉末置于通入还原气氛的环境中，以5℃/min的升温速率升温至850℃，煅烧4小时；自然冷却至室温，研磨烧结物，制得能促进植物生长的荧光粉。
4.如权利要求3所述的能促进植物生长的荧光粉的制备方法，其特征在于，所述步骤1中，各原料分别为铷化合物、钾化合物、钙化合物、磷化合物、氟化合物和铕化合物。
5.如权利要求4所述的能促进植物生长的荧光粉的制备方法，其特征在于，所述铷化合物采用碳酸铷、含铷的氢氧化物、含铷的硝酸盐、含铷的碳酸盐、含铷的硫酸盐或含铷的磷酸盐；
钾化合物采用碳酸钾、含钾的氢氧化物、含钾的硝酸盐、含钾的硫酸盐或含钾的磷酸盐；
钙化合物采用碳酸钙、含钙的氢氧化物、含钙的硝酸盐、含钙的硫酸盐或含钙的磷酸盐；
磷化合物采用磷酸二氢铵或含磷的氢氧化物；
氟化合物采用氟化钾、含氟的氢氧化物、含氟的硝酸盐、含氟的碳酸盐、含氟的硫酸盐或含氟的磷酸盐；
铕化合物采用氧化铕、含铕的氢氧化物、含铕的硝酸盐、含铕的碳酸盐、含铕的硫酸盐或含铕的磷酸盐。
6.如权利要求3所述的能促进植物生长的荧光粉的制备方法，其特征在于，所述步骤2中的还原气氛为：氨气；或者，按体积百分比由5～25%的氢气和95～75%的氮气组成的混合气体；或者，按体积百分比由5～25%的一氧化碳和95～75%的氮气组成的混合气体。
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