CN1055104C - 四硼酸锶铕荧光粉的制备 - Google Patents

四硼酸锶铕荧光粉的制备 Download PDF

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CN1055104C
CN1055104C CN96118932A CN96118932A CN1055104C CN 1055104 C CN1055104 C CN 1055104C CN 96118932 A CN96118932 A CN 96118932A CN 96118932 A CN96118932 A CN 96118932A CN 1055104 C CN1055104 C CN 1055104C
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europium
strontium
tetraborate
fluorescent powder
preparation
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CN1186104A (zh
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裴治武
曾庆华
苏锵
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Changchun Institute of Applied Chemistry of CAS
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Changchun Institute of Applied Chemistry of CAS
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Abstract

本发明属于四硼酸锶铕荧光粉的制备方法。
本发明利用该荧光粉基质化合物四硼酸锶在晶体结构上的特点，以碳酸锶、硼酸及氧化铕为原料，在空气或氮气等非还原性气氛中经高温灼烧制备四硼酸锶铕荧光粉。由于在制备过程中无需使用氢气等还原性气体，所以本发明可简化该荧光粉的生产工艺，降低生产成本并提高生产的安全性。

Description

四硼酸锶铕荧光粉的制备
本发明属于四硼酸锶铕荧光粉的制备方法。
四硼酸锶铕是一种在370nm附近可产生高强度短波紫外发光的荧光材料；用该材料制做的荧光灯可广泛地应用于农业，医疗，印刷以及验钞等领域中。该种荧光粉在国际市场上的牌号为NP-802(日本)，L112(德国)。由于该种荧光粉采用二价铕离子激活，而制备时铕的起始原料为氧化铕，其中铕为三价离子，所以目前的制备方法都采用在氢气等还原气氛中高温烧结，以使三价的铕离子还原为二价的铕离子。美国专利US4,719,033(Cl.252-301.4R；CO9K11/465)，C.F.Chenot等人公开了题为“铕激活四硼酸锶紫外发射荧光粉的制备方法”。在该方法中，将摩尔比为1∶4至1∶4.5的碳酸锶和硼酸以及0.003至0.0015的氧化铕在70℃的水中混合，于90℃热煮，分离后在含氢气0.3-3％的氢气/氮气气氛中于800℃烧结。所得磷光体在370nm附近产生强的窄带发射。由于其制备过程要在氢气等还原性气氛中进行，需要氢气的发生及供给系统，所以制备的工艺复杂，成本较高且安全性较差。
本发明的目的是采用碳酸锶，硼酸和氧化铕为原料，在氮气或空气等非还原性气氛中经高温烧结而制备四硼酸锶铕荧光粉。由于无需使用氢气等还原气体，所以本发明可简化生产工艺，降低生产成本并提高生产的安全性。
本发明利用荧光粉基质化合物四硼酸锶本身在结构上的特点，根据非等价取代及化合物保持电中性的原则，通过对反应原料的预处理，对烧结温度及反应时间的控制，在空气或氮气等非还原性气氛中制备四硼酸锶铕荧光粉。铕以其三价高价态的形式参与反应，随着灼烧的进行，四硼酸锶基质化合物晶格逐渐形成，原料中的三价铕离子也同时以取代二价锶离子的形式进入基质晶格；由于三价子比二价子锶离子高出一个正电荷，因此为保持体系的电中性，在三价铕离子周围将同时产生一个带有负电荷的缺陷；此后该负电荷缺陷向三价铕离子给出一个电子使其还原为二价的铕离子。由于基质化合物中由硼氧四面体构成的三维立体网状结构十分稳定，因此当三价铕离子取代二价锶离子并被还原为二价离子以后处于结晶学上十分稳定的九个氧配位的紧密包围中，所以生成的二价铕离子十分稳定，反应的最终产物为四硼酸锶铕荧光粉。
本发明将碳酸锶1.42-1.46克，硼酸2.40-2.80克和氧化铕0.02-0.74克充分研混，先于空气中在300-500℃灼烧2-4小时，研混后，在非还原性气氛包括氮气、空气中于800-900℃灼烧2-4小时，产物经研磨后即得白色粉未状的四硼酸锶铕荧光粉，最大发射波长位于370nm。
本发明提供的实施例如下：
实施例1：
将1.462克碳酸锶，2.547克硼酸和0.018克氧化铕在玛瑙乳钵中充分研混，转入氧化铝坩锅中在电炉内于300℃灼烧4小时，取出研混后，在氮气中于880℃再灼烧4小时，研磨后即得白色四硼酸锶铕荧光粉(Sr0.99B4O7：Eu2+ 0.01)。该荧光粉在254nm激发光的辐照下于370nm附近产生高强度发光。
实施例2：
将1.417克碳酸锶，2.720克硼酸和0.070克氧化铕在玛瑙研钵中充分研混，转入氧化铝坩锅中在电炉内于500℃灼烧2小时，取出研混后再于820℃在空气中灼烧3小时，样品冷却后经研磨即得白色四硼酸锶铕荧光粉(Sr0.96B4O7：Eu2+ 0.04)。该荧光粉在254nm激发光的辐照下于370nm附近产生窄带发光。
实施例3：
将1.445克碳酸锶，2.610克硼酸和0.036克的氧化铕在玛瑙乳钵中充分研混，转入氧化铝坩锅中在电炉内于400℃灼烧3小时，取出研混后，再于850℃在氮气中灼烧2小时，样品冷却后经研磨即得白色四硼酸锶铕荧光粉(Sr0.98B4O7：Eu2+ 0.02)。该荧光粉在254nm激发光的辐照下于370nm附近产生窄带发光。

Claims (1)

1、一种四硼酸锶铕荧光粉的制备方法，其特征在于将碳酸锶1.42-1.46克，硼酸2.40-2.80克和氧化铕0.02-0.74克充分研混，先于空气中在300-500℃灼烧2-4小时，研混后，在非还原性气氛包括氮气、空气中于800-900℃灼烧2-4小时，产物经研磨后即得白色粉末状的四硼酸锶铕荧光粉，最大发射波长位于370nm。
CN96118932A 1996-12-26 1996-12-26 四硼酸锶铕荧光粉的制备 Expired - Fee Related CN1055104C (zh)

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CN102344803B (zh) * 2011-10-17 2014-06-18 江门市科恒实业股份有限公司 一种铕锂激发硼酸锶紫外荧光粉及其制备方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0258545A1 (en) * 1986-08-28 1988-03-09 GTE Products Corporation Europium activated strontium tetraborate UV phosphor and process for producing same
US5078055A (en) * 1988-10-17 1992-01-07 Protoned B.V. Working table
US5378398A (en) * 1991-07-15 1995-01-03 Gte Products Corporation Method of treating europium activated strontium tetraborate phosphor

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0258545A1 (en) * 1986-08-28 1988-03-09 GTE Products Corporation Europium activated strontium tetraborate UV phosphor and process for producing same
US5078055A (en) * 1988-10-17 1992-01-07 Protoned B.V. Working table
US5378398A (en) * 1991-07-15 1995-01-03 Gte Products Corporation Method of treating europium activated strontium tetraborate phosphor

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