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A kind of process method of preparing rare earth sulfur oxide with alkali metal chloride

A technology of rare earth sulfur oxides and alkali metal chlorides, which is applied in the direction of rare earth metal compounds, rare earth metal sulfides, chemical instruments and methods, etc., can solve the problems of large particles and reduced luminescent performance, so as to reduce production costs and reduce Effect of Particle Range

Active Publication Date: 2016-08-17
南通捷事达新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the rare earth sulfur oxides prepared by the sulfur melting method have large particles and require ball milling, which greatly reduces the luminous performance, and the size distribution of the particles needs to be further improved.

Method used

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  • A kind of process method of preparing rare earth sulfur oxide with alkali metal chloride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 原料组成如表1中1 # 所示,具体制备方法包括下列步骤:

[0020] ①按重量称取18.672g Y 2 o 3 、13.146g Na 2 CO 3 (mol(Na 2 CO 3 ):mol(Y 2 o 3 )=1.5)、9.280g升华硫(mol(升华硫):mol(Y 2 o 3 )=3.5)和0.876gLiCl(mol(LiCl):mol(Y 2 o 3 )=0.25),将称好的物料混合均匀;

[0021] ②将混合均匀的物料装入内外均带盖的套坩埚中,在两坩埚的间隙填充耐高温粉末并压实;

[0022] ③将装有混合料的坩埚以升温速率2℃ / min升温到300℃,并保温1h,然后以升温速率3℃ / min升温至1100℃,烧结3h,然后随炉降温至室温;

[0023] ④烧结后的产物用热水洗涤并搅拌,抽滤;

[0024] ⑤将洗涤后的产物放入恒温鼓风干燥箱中烘干,得到稀土硫氧化物。

[0025] 对该稀土硫氧化物的测试结果如下:

[0026] 将过程⑤中烘干后的粉料用X射线衍射仪(XRD,D / Max2500)进行相组成分析,结果显示主要衍射峰的位置都与六方Y 2 o 2 S相对应,并且没有其他物质相的峰存在;用扫描电子显微镜(SEM,JEOL-6310)进行颗粒形貌分析,并采用软件进行颗粒尺寸统计,结果显示颗粒分布均匀,平均颗粒尺寸为3μm。

Embodiment 2

[0028] ①按重量称取19.060g La 2 o 3 、10.541g Na 2 CO 3 (mol(Na 2 CO 3 ):mol(La 2 o 3 )=1.7)、7.034g升华硫(mol(升华硫):mol(La 2 o 3 )=3.75)和1.709gNaCl(mol(NaCl):mol(La 2 o 3 )=0.5),将称好的物料混合均匀;

[0029] ②将混合均匀的物料装入内外均带盖的套坩埚中,在两坩埚的间隙填充耐高温粉末并压实;

[0030] ③将装有混合料的坩埚以升温速率2.5℃ / min升温到330℃,并保温1.5h,然后以升温速率3.5℃ / min升温至1150℃,烧结4h,然后随炉降温至室温;

[0031] ④烧结后的产物用热水洗涤并搅拌,抽滤;

[0032] ⑤将洗涤后的产物放入恒温鼓风干燥箱中烘干,得到稀土硫氧化物。

[0033] 对该稀土硫氧化物的测试结果如下:

[0034] 将过程⑤中烘干后的粉料用X射线衍射仪(XRD,D / Max2500)进行相组成分析,结果显示主要衍射峰的位置都与六方La 2 o 2S相对应,并且没有其他物质相的峰存在;用扫描电子显微镜(SEM,JEOL-6310)进行颗粒形貌分析,并采用软件进行颗粒尺寸统计,结果显示颗粒分布均匀,平均颗粒尺寸为2.3μm。

Embodiment 3

[0036] 组成如表1中3 # 所示,具体制备方法包括下列步骤:

[0037] ①按重量称取19.151gGd 2 o 3 、10.639g Na 2 CO 3 (mol(Na 2 CO 3 ):mol(Gd 2 o 3 )=1.9)、7.200g升华硫(mol(升华硫):mol(Gd 2 o 3 )=4.25)和2.954gKCl(mol(KCl):mol(Gd 2 o 3 )=0.75),将称好的物料混合均匀;

[0038] ②将混合均匀的物料装入内外均带盖的套坩埚中,在两坩埚的间隙填充耐高温粉末并压实;

[0039] ③将装有混合料的坩埚以升温速率3℃ / min升温到360℃,并保温2h,然后以升温速率4℃ / min升温至1200℃,烧结5h,然后随炉降温至室温;

[0040] ④烧结后的产物用热水洗涤并搅拌,抽滤;

[0041] ⑤将洗涤后的产物放入恒温鼓风干燥箱中烘干,得到稀土硫氧化物。

[0042] 对该稀土硫氧化物的测试结果如下:

[0043] 将过程⑤中烘干后的粉料用X射线衍射仪(XRD,D / Max2500)进行相组成分析,结果显示主要衍射峰的位置都与六方Gd 2 o 2 S相对应,并且没有其他物质相的峰存在;用扫描电子显微镜(SEM,JEOL-6310)进行颗粒形貌分析,并采用软件进行颗粒尺寸统计,结果显示颗粒分布均匀,平均颗粒尺寸为1.8μm。

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Abstract

The invention discloses a process method of rare earth oxysulfide by using an alkali chloride. The method comprises the following steps: (1) weighing required materials RE2O2S (wherein RE is one of rare earth elements Y, La, Gd and Sm), Na2CO3, sublimed sulfur and alkali chloride AMCl (wherein AM is one of alkali metal elements Li, Na or K) according to a stoichiometric ratio and uniformly mixing the weighed materials; (2) putting the uniformly mixed materials into inner and outer crucibles, and filling high-temperature powder in the gap between the two crucibles and compacting, where each of the two crucibles has a cover; (3) raising the temperature of the crucibles with the mixed material to 1100-1250 DEG C in a gradient way, sintering for 3-5 hours and then cooling to room temperature along with a furnace; (4) washing the sintered product with hot water, stirring, and carrying out suction filtration; and (5) drying the washed product into a constant-temperature blowing drying box to obtain the rare earth oxysulfide. By taking RE2O3, Na2CO3, sublimed sulfur and alkali chloride AMCl as raw materials, the rare earth oxysulfide is prepared by using a sulfur melting method. The preparation method of the rare earth oxysulfide is simple and easy to operate and the rare earth oxysulfide can be used in the fields of light-emitting materials and photoabsorption materials and the like.

Description

technical field [0001] 本发明涉及一种用碱金属氯化物制备稀土硫氧化物的工艺方法,尤其涉及稀土硫氧化物的硫熔法制备与改性,以及窄颗粒分布稀土硫氧化物的制备与优化。 Background technique [0002] 稀土硫氧化物具有较高的化学稳定性和热稳定性,不溶于水,熔点高达2000~2200℃;禁带宽度为4.6~4.8eV,适合于掺杂离子;其最大声子能量为520cm -1 ,适合于作为发光材料的基质材料,具有非常高的光吸收与传能效率。六角Ln 2 o 2 S晶体结构最大的特点是具有较宽敞的空间结构,允许一定量的阳离子和阴离子空位形成及一定量的间隙离子进入,而晶体结构基本保持不变。其中La 2 o 2 S、Y 2 o 2 S和Gd 2 o 2 S作为发光材料的基质材料,通过掺杂Eu 3+ , Tb 3+ 、Ce 3+ 等发光离子在紫外和真空紫外激发下具有良好的发光性能,而Sm 2 o 2 S作为光学吸收材料,对1.06μm和1.54μm激光具有良好的光吸收特性。因此,稀土硫氧化物作为光学材料得到了广泛的应用。稀土硫氧化物主要的制备方法是硫熔法,适用于工业大规模生产,晶体完整,发光性能优于其他方法制备的产品。但硫熔法的助熔剂用量和种类不固定,还没有一个明确的范围。目前硫熔法制备的稀土硫氧化物,产品的颗粒较大,需要球磨,使得发光性能大大降低,而且颗粒的尺寸分布有待进一步改善。因此优化硫熔法制备稀土硫氧化物的工艺过程,提高稀土硫氧化物的颗粒物性是非常必要的。 Contents of the invention [0003] 本发明要解决的技术问题是克服上述缺陷,通过碱金属氯化物AMCl辅助的硫熔法制备出化学式为RE 2 o 2 S的稀土硫氧化物。 [0004] 为解决上述问题,本发明采用如下技术方案是: [0005] 一种用碱金属氯化物制备稀土硫氧化物的工艺方法,其特征在于,所述碱金属氯化物AMCl中AM为碱金属元素Li、Na或K中的一种;所述稀土硫氧化物化学式为RE 2 o 2 S中RE为稀土元素Y、La、Gd或Sm中的一种;所述的化学式为RE 2 o 2 S的稀土硫氧化物由硫熔法制备,其制备步骤如下: [0006] ①按化学计量比称取所需物料RE 2 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00
CPCC01F17/294C01P2002/72C01P2004/61
Inventor 韩朋德姜晓萍张林涛张长森张其土
Owner 南通捷事达新材料有限公司
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