CN106433616B - 一种紫外荧光材料及其制备方法 - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000463 material Substances 0.000 title claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 18
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 11
- 239000011734 sodium Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 9
- 238000001238 wet grinding Methods 0.000 claims abstract description 8
- 229960004756 ethanol Drugs 0.000 claims abstract description 3
- 235000019441 ethanol Nutrition 0.000 claims abstract description 3
- 238000001354 calcination Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 19
- 238000001816 cooling Methods 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 6
- 231100000252 nontoxic Toxicity 0.000 abstract description 4
- 230000003000 nontoxic effect Effects 0.000 abstract description 4
- 238000003837 high-temperature calcination Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000004973 liquid crystal related substance Substances 0.000 description 17
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 238000005119 centrifugation Methods 0.000 description 6
- 239000004570 mortar (masonry) Substances 0.000 description 6
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- 238000000227 grinding Methods 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 210000002858 crystal cell Anatomy 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000000103 photoluminescence spectrum Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
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- 230000001988 toxicity Effects 0.000 description 1
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Abstract
本发明公开了一种紫外荧光材料及其制备方法。所述荧光材料的分子式为Na3C6N9·3H2O。本发明以三聚氰胺、碳酸钠为原料，将两者用乙醇湿法研磨制得前驱体粉末，再经过高温煅烧和自然冷却得到样品后，将其溶解于去离子水中得到无色透明溶液，加入无水乙醇，物质析出，离心分离干燥得到产物。按本发明技术方案制备得到的紫外荧光材料具有较好的紫外荧光性能。本发明的原料无毒易得，价格低廉，工艺重复性好，且产品制备周期短、成本低。
Description
技术领域
本发明涉及一种紫外荧光材料及其制备方法。
背景技术
液晶显示以其工作电压低、能耗小和无放射性等一系列优良特性而受到人们的广泛青睐。然而, 其存在两个主要的不足，即视角较小和透过率较低，限制了它的亮度和对比度，也一直影响着它的应用与发展。直到1997年英国剑桥的W. A. Crossland等人提出了光致发光液晶显示(Photoluminescent Liquid Crystal Display——— PLLCD)的概念, 把光致发光荧光粉与液晶结合起来, 形成一种全新的液晶显示模式, 为彻底解决这些严重影响液晶显示质量的问题提出了新的途径。光致发光液晶显示有时亦称作液晶调制的光致发光显示(LC-modulated photolum inescent displays)。在这种显示模式中, 液晶单元作为控制背照明光通过与否的光阀, 用三基色荧光粉取代液晶单元前的三色滤光片, 同时用近紫外光代替白光作为液晶的背照明光源, 用以激发液晶单元前的基色荧光粉, 这两项变革既克服了液晶显示的上述缺点,也大大地提高了器件的显示质量。对这种荧光粉的主要要求是能被低压汞蒸气放电有效激发, 产生近紫外发光。它的发射要尽量靠近可见区, 但又尽量不进入可见区, 以免降低色饱和度而影响显示的质量;它的发光带半峰全宽要尽量窄, 以免其短波部分对液晶产生破坏作用。由于这些条件近于苛刻, 只有少数荧光粉能基本满足要求, 研制和开发PLLCD背照明用的紫外荧光粉, 成为各国学者关注的热点之一。
目前，有关于Na3C6N9·3H2O的制备方法仅有一种，即以NaC2N3(双氰胺钠)为原料，高温聚合反应生成。 参见文献“Trimerisierung von Dicyanamid-Ionen C2N3±im FestkoÈ rper ± Synthesen, Kristallstrukturen und Eigenschaften von NaCs2(C2N3)3 undNa3C6N9·3H2O”（ 期刊《Zeitschrift für anorganische und allgemeine Chemie》），采用NaC2N3为原料，在500℃条件下加热，并在水中结晶得到Na3C6N9·3H2O的方法。该方法制备周期较长，成本较高，且原料双氰胺钠有一定毒性。因此，寻求一种经济无毒的方法来制备Na3C6N9·3H2O具有积极的现实意义。
发明内容
本发明针对现有制备Na3C6N9·3H2O存在的不足，提供一种原料无毒性、价格低廉，制备方法重复性好、周期短、成本低，能满足光致发光液晶显示背照明光源要求的紫外荧光材料及其制备方法。
实现本发明目的的技术方案是提供一种紫外荧光材料的制备方法，其包括如下步骤：
①前驱体的制备：按质量比1:0.3～1:1，将三聚氰胺与碳酸钠混合，加入乙醇湿磨，得到混合固体前驱体A；
②热处理：将前驱体A在温度为400～650℃的条件下煅烧，得到产物B；
③溶解析出：将产物B溶解于去离子水中，得到无色透明溶液，加入无水乙醇，物质析出，再经离心、干燥处理，得到一种分子式为Na3C6N9·3H2O的紫外荧光材料。
本发明的一个优选方案是：步骤②中，煅烧时间为1～5h。
本发明技术方案还包括按上述制备方法得到的一种紫外荧光材料。它在波长为322nm附近的光激发下，其发射峰在377nm波长附近。
与现有技术相比，本发明的优势在于：原料无毒易得，价格低廉、重复性好，而且制备周期短、成本低；材料满足了光致发光液晶显示背照明光源的要求，具有应用前景。
附图说明
图1是本发明实施例1制备的紫外荧光粉体X射线粉末衍射图谱。
图2是本发明实施例1制备的紫外荧光粉体红外光谱图。
图3是本发明实施例1制备的紫外荧光粉体光致发光谱图。
具体实施方式
下面结合附图和实施例对本发明技术方案作一步的阐述。
实施例1：
称取4g三聚氰胺和1.2g碳酸钠于研钵中，加入无水乙醇湿磨，得到前驱体A，将前驱体A装入氧化铝坩埚，在马弗炉中550℃煅烧2h，随炉冷却后得到样品B，将样品B研磨溶解于50ml去离子水中，得到无色透明溶液，加入50ml无水乙醇，物质析出，离心，放入烘箱70℃干燥12h，得到荧光粉体。
参见附图1，它是本实施例制备的紫外荧光粉体的XRD衍射图谱，从图1中可以看出，衍射峰强度高而且尖锐，说明所合成的耐高温荧光粉体结晶性良好。
参见附图2，它是本实施例制备的紫外荧光粉体的红外光谱图，从图2中可以看出，3615,2945cm-1为OH (H-OH····N)伸缩振动峰，2180cm-1为C≡N的不对称伸缩振动，1663cm-1为H2O的变形振动，1514,1397cm-1为结构环的不对称伸缩振动，1234cm-1为C-N的不对称伸缩振动。
参见附图3，它是本实施例制备的紫外荧光粉体的光致发光谱图，从图3中可以看出，该荧光粉体受322nm左右的光激发，发射峰在377nm左右，满足了光致发光液晶显示背照明光源的要求。
实施例2：
称取4g三聚氰胺和1.6g碳酸钠于研钵中，加入无水乙醇湿磨，得到前驱体A，将前驱体A装入氧化铝坩埚，在马弗炉中550℃煅烧2h，随炉冷却后得到样品B，将样品B研磨溶解于50ml去离子水中，得到无色透明溶液，加入50ml无水乙醇，物质析出，离心，放入烘箱70℃干燥12h，得到荧光粉体。
实施例3：
称取4g三聚氰胺和2g碳酸钠于研钵中，加入无水乙醇湿磨，得到前驱体A，将前驱体A装入氧化铝坩埚，在马弗炉中550℃煅烧2h，随炉冷却后得到样品B，将样品B研磨溶解于50ml去离子水中，得到无色透明溶液，加入50ml无水乙醇，物质析出，离心，放入烘箱70℃干燥12h，得到荧光粉体。
实施例4：
称取4g三聚氰胺和4g碳酸钠于研钵中，加入无水乙醇湿磨，得到前驱体A，将前驱体A装入氧化铝坩埚，在马弗炉中550℃煅烧2h，随炉冷却后得到样品B，将样品B研磨溶解于50ml去离子水中，得到无色透明溶液，加入50ml无水乙醇，物质析出，离心，放入烘箱70℃干燥12h，得到荧光粉体。
实施例5：
称取4g三聚氰胺和2g碳酸钠于研钵中，加入无水乙醇湿磨，得到前驱体A，将前驱体A装入氧化铝坩埚，在马弗炉中400℃煅烧2h，随炉冷却后得到样品B，将样品B研磨溶解于50ml去离子水中，得到无色透明溶液，加入50ml无水乙醇，物质析出，离心，放入烘箱70℃干燥12h，得到荧光粉体。
实施例6：
称取4g三聚氰胺和2g碳酸钠于研钵中，加入无水乙醇湿磨，得到前驱体A，将前驱体A装入氧化铝坩埚，在马弗炉中650℃煅烧2h，随炉冷却后得到样品B，将样品B研磨溶解于50ml去离子水中，得到无色透明溶液，加入50ml无水乙醇，物质析出，离心，放入烘箱70℃干燥12h，得到荧光粉体。
Claims (2)
1.一种紫外荧光材料的制备方法，其特征在于包括如下步骤：
①前驱体的制备：按质量比1:0.3～1:1，将三聚氰胺与碳酸钠混合，加入乙醇湿磨，得到混合固体前驱体A；
②热处理：将前驱体A在温度为400～650℃的条件下煅烧，得到产物B；
③溶解析出：将产物B溶解于去离子水中，得到无色透明溶液，加入无水乙醇，物质析出，再经离心、干燥处理，得到一种分子式为Na3C6N9·3H2O的紫外荧光材料。
2.根据权利要求1所述的一种紫外荧光材料的制备方法，其特征在于：步骤②中，煅烧时间为1～5h。
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| WO2005033000A1 (de) * | 2003-09-16 | 2005-04-14 | Universität Tübingen | Verfahren zur herstellung von röhrchenförmigen kohlenstoffnitriden |
| CN103086332A (zh) * | 2013-01-30 | 2013-05-08 | 华南理工大学 | 一种碳氮化合物荧光粉及其制备方法 |
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| Ionic Liquids Containing the Triply Negatively Charged Tricyanomelaminate Anion and a B(C6F5)3 Adduct Anion;Karsten Voss等;《Chem. Eur. J.》;20111231;13526-13537 * |
| Trimerization of NaC2N3 to Na3C6N9 in the Solid: Ab Initio Crystal Structure Determination of Two Polymorphs of NaC2N3 and of Na3C6N9 from X-ray Powder Diffractomet;Barbara Jurgens等;《Inorg. Chem.》;20001231;665-670 * |
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