CN101323442A - A method for solvothermally synthesizing lanthanum phosphate nanorods - Google Patents
A method for solvothermally synthesizing lanthanum phosphate nanorods Download PDFInfo
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- LQFNMFDUAPEJRY-UHFFFAOYSA-K lanthanum(3+);phosphate Chemical compound [La+3].[O-]P([O-])([O-])=O LQFNMFDUAPEJRY-UHFFFAOYSA-K 0.000 title claims abstract description 46
- 239000002073 nanorod Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 17
- 230000002194 synthesizing effect Effects 0.000 title abstract description 4
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims abstract description 20
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000007864 aqueous solution Substances 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000001488 sodium phosphate Substances 0.000 claims abstract description 12
- 229910000162 sodium phosphate Inorganic materials 0.000 claims abstract description 12
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 3
- IKNAJTLCCWPIQD-UHFFFAOYSA-K cerium(3+);lanthanum(3+);neodymium(3+);oxygen(2-);phosphate Chemical group [O-2].[La+3].[Ce+3].[Nd+3].[O-]P([O-])([O-])=O IKNAJTLCCWPIQD-UHFFFAOYSA-K 0.000 abstract description 11
- 238000004729 solvothermal method Methods 0.000 abstract description 7
- 239000011259 mixed solution Substances 0.000 abstract description 6
- 239000013078 crystal Substances 0.000 abstract description 5
- 238000003756 stirring Methods 0.000 abstract description 5
- 239000006185 dispersion Substances 0.000 abstract description 4
- 238000001354 calcination Methods 0.000 abstract description 2
- 238000001308 synthesis method Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 9
- 239000002245 particle Substances 0.000 description 9
- 239000012071 phase Substances 0.000 description 9
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 8
- -1 Rare earth phosphates Chemical class 0.000 description 7
- 229910052761 rare earth metal Inorganic materials 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 229910019142 PO4 Inorganic materials 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 235000021317 phosphate Nutrition 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 239000012761 high-performance material Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- KTUQUZJOVNIKNZ-UHFFFAOYSA-N butan-1-ol;hydrate Chemical compound O.CCCCO KTUQUZJOVNIKNZ-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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Abstract
本发明公开了一种溶剂热合成磷酸镧纳米棒的方法。该方法是将浓度为1.0～2.0mol/L氯化镧水溶液和浓度为1.0～2.0mol/L磷酸钠水溶液混合，其中磷酸钠与氯化镧等摩尔比；加入正丁醇溶剂，使水与正丁醇体积比为0.5～2∶1，且氯化镧在混合溶液中的摩尔浓度为0.2～0.5mol/L，搅拌至混合均匀后，用磷酸调节溶液pH＝3～6，在温度为140～220℃条件下溶剂热反应6.0～48h。本发明合成方法简单，环境友好、绿色经济、低温、不需煅烧，可在溶液中直接得到产物，所得磷酸镧纯度高，属于单斜晶系，为独居石结构纳米棒，棒的直径小于10nm、粗细均匀，棒的形貌单一，分散性好。The invention discloses a method for solvothermally synthesizing lanthanum phosphate nanorods. The method is to mix an aqueous solution of lanthanum chloride with a concentration of 1.0 to 2.0 mol/L and an aqueous solution of sodium phosphate with a concentration of 1.0 to 2.0 mol/L, wherein the sodium phosphate and lanthanum chloride have an equimolar ratio; add n-butanol solvent to make water and The volume ratio of n-butanol is 0.5～2:1, and the molar concentration of lanthanum chloride in the mixed solution is 0.2～0.5mol/L, after stirring until uniformly mixed, the pH of the solution is adjusted to 3～6 with phosphoric acid. Solvothermal reaction at 140-220°C for 6.0-48 hours. The synthesis method of the present invention is simple, environment-friendly, green and economical, low temperature, and does not require calcination, and the product can be directly obtained in the solution. The obtained lanthanum phosphate has high purity, belongs to the monoclinic crystal system, and is a monazite structure nanorod, and the diameter of the rod is less than 10nm. , The thickness is uniform, the shape of the rod is single, and the dispersion is good.
Description
技术领域 technical field
本发明属于无机纳米材料技术领域，具体涉及一种溶剂热合成磷酸镧纳米棒的方法。The invention belongs to the technical field of inorganic nanometer materials, and in particular relates to a method for solvothermally synthesizing lanthanum phosphate nanorods.
背景技术 Background technique
稀土磷酸盐具有极好的荧光性质、高的量子效率，是一类优良的发光材料，适用于高密度激发和高能量量子激发的环境，可用于特种玻璃、激光技术、紧凑形荧光灯、等离子体平板显示。由于稀土磷酸盐自身的化学物理特性，磷酸镧(LaPO4)常被用作一种掺杂其它稀土离子的良好基质材料，在光学材料中占有举足轻重的地位。同时，稀土磷酸盐LaPO4熔点高，是适合高温使用的氧化物纤维涂层材料，与Al2O3复合高温稳定性好，可制备Al2O3/LaPO4高温可加工复合陶瓷，具有耐高温、耐腐蚀、抗氧化性、电绝缘性好等优点，在工程领域得到广泛的应用。另一方面，由于稀土元素结构的特殊性，LaPO4可用于对分子筛进行改性来调节其表面酸碱性，从而使其在催化化学方面也具有独特的作用。Rare earth phosphates have excellent fluorescent properties and high quantum efficiency, and are a class of excellent luminescent materials, suitable for high-density excitation and high-energy quantum excitation environments, and can be used in special glass, laser technology, compact fluorescent lamps, plasma Flat display. Due to the chemical and physical properties of rare earth phosphates, lanthanum phosphate (LaPO 4 ) is often used as a good host material for doping other rare earth ions, and plays an important role in optical materials. At the same time, the rare earth phosphate LaPO 4 has a high melting point and is suitable for high-temperature use as an oxide fiber coating material. It has good high-temperature stability when combined with Al 2 O 3 , and can prepare Al 2 O 3 /LaPO 4 high-temperature machinable composite ceramics. High temperature, corrosion resistance, oxidation resistance, good electrical insulation, etc., have been widely used in engineering fields. On the other hand, due to the special structure of rare earth elements, LaPO 4 can be used to modify molecular sieves to adjust their surface acidity and alkalinity, so that it also has a unique role in catalytic chemistry.
近年来有关纳米材料研究发现，材料的微结构如粒径大小、颗粒形貌、特殊的表面特性、结晶度及粒径分布、颗粒分散性等对器件的发光效率和分辨率、材料的机械加工性能及催化性质有非常大的影响。合成颗粒细小、分散性好、分布均匀、形貌均一的纳米粉体，是制备高性能材料的前提。为了满足人们对高性能材料需求，制备LaPO4超微粉体的新工艺不断涌现。目前，制备LaPO4的方法主要有高温固相法、沉淀法、水热法等。高温固相法通常长时间加热，最后研磨得到单一相的粉体，晶形好但粉体团聚现象严重，颗粒粒径较大；且球磨破坏了表面结构，影响其性能且能耗大。沉淀法可加入少量表面活性剂改善沉淀过滤性能并改变沉淀颗粒的晶体形状，控制了沉降速率，烧结温度有所降低，可得到微细、均匀的粉体，但沉淀和母液必须陈化，得到的相纯度不高，结晶度不好。水热法在较低的温度下进行，可制备出高纯度物相、结晶完美、分散性较好、粒度分布均匀的纳米颗粒，操作简单，对环境污染小，制备出来的产物不需球磨，但当前用水热法合成磷酸镧纳米棒一般只在水溶液中进行，得到的磷酸镧纳米棒大小不均一，分散性不好。In recent years, research on nanomaterials has found that the microstructure of materials, such as particle size, particle morphology, special surface characteristics, crystallinity, particle size distribution, and particle dispersion, has a great impact on the luminous efficiency and resolution of devices and the mechanical processing of materials Performance and catalytic properties have a very large impact. The synthesis of nanopowders with fine particles, good dispersibility, uniform distribution and uniform shape is the prerequisite for the preparation of high-performance materials. In order to meet people's demand for high-performance materials, new processes for preparing LaPO 4 ultrafine powders are emerging. At present, the methods for preparing LaPO 4 mainly include high-temperature solid-phase method, precipitation method, and hydrothermal method. The high-temperature solid-phase method usually heats for a long time, and finally grinds to obtain a single-phase powder. The crystal shape is good, but the powder agglomeration phenomenon is serious, and the particle size is large; and the ball milling destroys the surface structure, which affects its performance and consumes a lot of energy. In the precipitation method, a small amount of surfactant can be added to improve the filtration performance of the precipitate and change the crystal shape of the precipitated particles. The sedimentation rate is controlled, the sintering temperature is reduced, and a fine and uniform powder can be obtained, but the precipitate and mother liquor must be aged. The phase purity is not high and the crystallinity is not good. The hydrothermal method is carried out at a lower temperature, and can prepare nanoparticles with high purity phase, perfect crystallization, good dispersion, and uniform particle size distribution. The operation is simple, the environmental pollution is small, and the prepared product does not need ball milling. However, the current hydrothermal synthesis of lanthanum phosphate nanorods is generally only carried out in aqueous solution, and the obtained lanthanum phosphate nanorods are not uniform in size and poor in dispersibility.
发明内容 Contents of the invention
本发明的主要目的在于克服现有合成技术的缺点，提供一种溶剂热合成磷酸镧纳米棒的方法，所得磷酸镧属于单斜晶系，为独居石结构纳米棒，棒的直径小于10nm，粗细均匀、形貌单一，其尺寸可通过反应条件来控制。The main purpose of the present invention is to overcome the shortcoming of existing synthetic technology, provide a kind of method of solvothermally synthesized lanthanum phosphate nanorod, gained lanthanum phosphate belongs to monoclinic crystal system, is nanorod of monazite structure, and the diameter of rod is less than 10nm, thickness Uniform, single shape, its size can be controlled by reaction conditions.
本发明是在水热法基础上，添加有机溶剂正丁醇或正丙醇，采用溶剂热法来合成磷酸镧，得到了相纯的独居石结构纳米棒，棒的直径小于10nm，粗细均匀、形貌单一，是目前合成的最细的且分散性最好的磷酸镧纳米棒。基于材料的性能一般会随粒径的减少而优化，因此，我们所得到的细小且分散性好的磷酸镧纳米棒，有望提高磷酸镧的稳定性、光学及催化等物化性质，从而加强其在工程领域中的应用。The present invention is based on the hydrothermal method, adding organic solvent n-butanol or n-propanol, adopting solvothermal method to synthesize lanthanum phosphate, and obtaining phase-pure monazite structure nanorods, the diameter of the rods is less than 10nm, the thickness is uniform, It has a single shape and is the thinnest and best dispersed lanthanum phosphate nanorods synthesized so far. Based on the performance of the material, the performance is generally optimized with the decrease of the particle size. Therefore, the fine and well-dispersed lanthanum phosphate nanorods we obtained are expected to improve the stability, optical and catalytic properties of lanthanum phosphate, thereby enhancing its performance in applications in engineering.
本发明的目的通过如下技术方案实现：The purpose of the present invention is achieved through the following technical solutions:
一种溶剂热合成磷酸镧纳米棒的方法：将浓度为1.0～2.0mol/L氯化镧水溶液和浓度为1.0～2.0mol/L磷酸钠水溶液混合，其中磷酸钠与氯化镧等摩尔比；加入正丁醇溶剂，使水与正丁醇体积比为0.5～2∶1，且氯化镧在混合溶液中的摩尔浓度为0.2～0.5mol/L，搅拌至混合均匀后，用磷酸调节溶液pH＝3～6，在温度为140～220℃条件下溶剂热反应6.0～48h，得磷酸镧纳米棒。A method for solvothermally synthesizing lanthanum phosphate nanorods: mixing an aqueous solution of lanthanum chloride with a concentration of 1.0 to 2.0 mol/L and an aqueous solution of sodium phosphate with a concentration of 1.0 to 2.0 mol/L, wherein the sodium phosphate and lanthanum chloride have an equimolar ratio; Add n-butanol solvent so that the volume ratio of water and n-butanol is 0.5-2:1, and the molar concentration of lanthanum chloride in the mixed solution is 0.2-0.5mol/L, stir until the mixture is uniform, and adjust the solution with phosphoric acid pH = 3-6, solvothermal reaction at a temperature of 140-220° C. for 6.0-48 hours to obtain lanthanum phosphate nanorods.
为进一步实现本发明的目的，所述溶剂热反应是在带有聚四氟乙烯内衬的高压釜中进行。To further realize the object of the present invention, the solvothermal reaction is carried out in an autoclave with a polytetrafluoroethylene liner.
所述溶剂热反应的温度优选180～220℃。The temperature of the solvothermal reaction is preferably 180-220°C.
所述氯化镧在混合溶液中的浓度为0.3～0.4mol/L。The concentration of the lanthanum chloride in the mixed solution is 0.3-0.4 mol/L.
所述反应溶液的pH优选为4～6。The pH of the reaction solution is preferably 4-6.
相对于现有合成技术，本发明具有如下优点和有益效果：Compared with existing synthetic technology, the present invention has following advantage and beneficial effect:
(1)本发明采用溶剂热法合成磷酸镧纳米棒，与其它化学合成方法相比具有环境友好、绿色经济、低温、不需煅烧可在溶液中直接得到产物、重复性好等优点。(1) The present invention uses a solvothermal method to synthesize lanthanum phosphate nanorods. Compared with other chemical synthesis methods, it has the advantages of environmental friendliness, green economy, low temperature, product can be directly obtained in solution without calcination, and good repeatability.
(2)本发明所得磷酸镧纯度高，属于单斜晶系，为独居石结构纳米棒，棒的直径小于10nm，粗细均匀，形貌单一，分散性好。(2) The lanthanum phosphate obtained in the present invention has high purity, belongs to the monoclinic crystal system, and is a monazite structure nanorod, the diameter of the rod is less than 10 nm, the thickness is uniform, the shape is single, and the dispersion is good.
附图说明 Description of drawings
图1为本发明实验例1～6所制备的磷酸镧纳米棒的XRD图。FIG. 1 is an XRD pattern of lanthanum phosphate nanorods prepared in Experimental Examples 1-6 of the present invention.
图2为本发明实施例2所制备的磷酸镧纳米棒的透射电镜照片(JEOL2010型高分辨透射电镜扫描仪，100kV)。FIG. 2 is a transmission electron micrograph (JEOL2010 high-resolution transmission electron microscope scanner, 100 kV) of the lanthanum phosphate nanorods prepared in Example 2 of the present invention.
具体实施方式 Detailed ways
为更好理解本发明，下面结合实施例对本发明做进一步地详细说明，但是本发明要求保护的范围并不局限于实施例表示的范围。In order to better understand the present invention, the present invention will be further described in detail below in conjunction with the examples, but the protection scope of the present invention is not limited to the range indicated by the examples.
实施例1Example 1
将10ml1.0mol/L氯化镧水溶液和10ml1.0mol/L磷酸钠水溶液，加入到30ml正丁醇中，氯化镧在混合溶液中的摩尔浓度为0.2mol/L，搅拌至混合均匀后，用磷酸调节溶液pH＝4，转移到带有聚四氟乙烯内衬的高压釜中，恒温箱内220℃条件下溶剂热反应4h，制得磷酸镧纳米棒。如图1中曲线1所示，所有衍射峰都能与底部的单斜晶系磷酸镧的标准峰相对应，由此可知所得磷酸镧纳米棒为纯相的独居石结构，属于单斜晶系，独居石结构。根据谢乐公式D＝κ·λ/βcosθ，κ为谢乐常数，一般取值0.89；λ为X射线波长，本实施例中取值0.154056nm；β为衍射峰半高宽，即峰顶到峰底的高度一半的地方的宽度，测量出来后再转化为弧度；θ为衍射角。可以估算晶粒尺寸D约为8nm。由于一般情况下材料的粒径越小，比表面积越大，可使其物理化学性能优化，因此本专利中所合成的磷酸镧纳米棒可应用于光学或催化性能加强方面。Add 10ml of 1.0mol/L lanthanum chloride aqueous solution and 10ml of 1.0mol/L sodium phosphate aqueous solution into 30ml of n-butanol, the molar concentration of lanthanum chloride in the mixed solution is 0.2mol/L, stir until evenly mixed, Phosphoric acid was used to adjust the pH of the solution to 4, transferred to a polytetrafluoroethylene-lined autoclave, and solvothermally reacted for 4 hours at 220° C. in a constant temperature box to prepare lanthanum phosphate nanorods. As shown in
实施例2Example 2
将1.0mol/L氯化镧水溶液和1.0mol/L磷酸钠水溶液，加入到30ml正丙醇中，其它实验操作和试剂用量与实施1相同，制得磷酸镧纳米棒。如图1中曲线2所示，所有衍射峰都能与底部的单斜晶系磷酸镧的标准峰相对应，由此可知所得磷酸镧纳米棒为纯相的独居石结构，由展宽的半高宽，用谢乐公式可以估算晶粒尺寸约为7nm。Add 1.0 mol/L lanthanum chloride aqueous solution and 1.0 mol/L sodium phosphate aqueous solution into 30 ml of n-propanol, and other experimental operations and reagent consumption are the same as those in
实施例3Example 3
将10ml1.5mol/L氯化镧水溶液和15ml1.0mol/L磷酸钠水溶液，加入到25ml正丁醇中，氯化镧在混合溶液中的摩尔浓度为0.3mol/L，搅拌至混合均匀后，用磷酸调节溶液pH＝5，转移到带有聚四氟乙烯内衬的高压釜中，恒温箱内180℃条件下溶剂热反应24h，制得磷酸镧纳米棒。如图1中曲线3所示，所有衍射峰都能与底部的单斜晶系磷酸镧的标准峰相对应，由此可知所得磷酸镧纳米棒为纯相的独居石结构，由展宽的半高宽，用谢乐公式可以估算晶粒尺寸约为9nm。Add 10ml of 1.5mol/L lanthanum chloride aqueous solution and 15ml of 1.0mol/L sodium phosphate aqueous solution into 25ml of n-butanol, the molar concentration of lanthanum chloride in the mixed solution is 0.3mol/L, stir until it is evenly mixed, Phosphoric acid was used to adjust the pH of the solution to 5, transferred to an autoclave lined with polytetrafluoroethylene, and subjected to solvothermal reaction at 180° C. for 24 hours in an incubator to prepare lanthanum phosphate nanorods. As shown in
实施例4Example 4
将10ml1.5mol/L氯化镧水溶液和15ml1.0mol/L磷酸钠水溶液，加入到25ml正丙醇中，其它实验操作和试剂用量与实施1相同，制得磷酸镧纳米棒。如图1中曲线4所示，所有衍射峰都能与底部的单斜晶系磷酸镧的标准峰相对应，由此可知所得磷酸镧纳米棒为纯相的独居石结构，由展宽的半高宽，用谢乐公式可以估算晶粒尺寸约为8nm。图2为制备的磷酸镧纳米棒的透射电镜照片。如图2所示，本实施例所得磷酸镧纳米棒形貌单一，粗细均匀，棒的直径基本都在10nm以下，分散性好。Add 10ml of 1.5mol/L lanthanum chloride aqueous solution and 15ml of 1.0mol/L sodium phosphate aqueous solution into 25ml of n-propanol, and other experimental operations and reagent dosages are the same as those in
实施例5Example 5
将10ml2.0mol/L氯化镧水溶液和20ml1.0mol/L磷酸钠水溶液，加入到20ml正丁醇中，再加入氯化镧在混合溶液中的摩尔浓度为0.4mol/L，搅拌至混合均匀后，用磷酸调节溶液pH＝6，转移到带有聚四氟乙烯内衬的高压釜中，恒温箱内140℃条件下溶剂热反应48h，制得磷酸镧纳米棒。如图1中曲线5所示，所有衍射峰都能与底部的单斜晶系磷酸镧的标准峰相对应，由此可知所得磷酸镧纳米棒为纯相的独居石结构，由展宽的半高宽，用谢乐公式可以估算晶粒尺寸约为10nm。Add 10ml of 2.0mol/L lanthanum chloride aqueous solution and 20ml of 1.0mol/L sodium phosphate aqueous solution into 20ml of n-butanol, then add lanthanum chloride to a molar concentration of 0.4mol/L in the mixed solution, and stir until well mixed Finally, the pH of the solution was adjusted to 6 with phosphoric acid, transferred to an autoclave lined with polytetrafluoroethylene, and solvothermally reacted at 140° C. for 48 hours in a constant temperature box to prepare lanthanum phosphate nanorods. As shown in
实施例6Example 6
将10ml2.0mol/L氯化镧水溶液和20ml1.0mol/L磷酸钠水溶液，加入到20ml正丙醇中，其它实验操作和试剂用量与实施5相同，制得磷酸镧纳米棒。如图1中曲线6所示，所有衍射峰都能与底部的单斜晶系磷酸镧的标准峰相对应，由此可知所得磷酸镧纳米棒为纯相的独居石结构，由展宽的半高宽，用谢乐公式可以估算晶粒尺寸约为8nm。Add 10 ml of 2.0 mol/L lanthanum chloride aqueous solution and 20 ml of 1.0 mol/L sodium phosphate aqueous solution into 20 ml of n-propanol, and other experimental operations and reagent dosages are the same as those in
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| CN102071460A (en) * | 2010-11-19 | 2011-05-25 | 长春理工大学 | Method for preparing europium-doped lanthanum phosphate porous nanorods on basis of herring sperm DNA template |
| CN111747392A (en) * | 2020-07-17 | 2020-10-09 | 南昌航空大学 | A kind of method for preparing hemihydrate samarium phosphate rod-shaped nanocrystal |
| CN115340077A (en) * | 2022-07-22 | 2022-11-15 | 承德莹科精细化工股份有限公司 | Preparation method of high-purity lanthanum phosphate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102071460A (en) * | 2010-11-19 | 2011-05-25 | 长春理工大学 | Method for preparing europium-doped lanthanum phosphate porous nanorods on basis of herring sperm DNA template |
| CN102071460B (en) * | 2010-11-19 | 2012-10-31 | 长春理工大学 | A method for preparing europium-doped lanthanum phosphate porous nanorods based on herring sperm DNA template |
| CN111747392A (en) * | 2020-07-17 | 2020-10-09 | 南昌航空大学 | A kind of method for preparing hemihydrate samarium phosphate rod-shaped nanocrystal |
| CN111747392B (en) * | 2020-07-17 | 2023-03-14 | 南昌航空大学 | Method for preparing semi-hydrated samarium phosphate rod-shaped nanocrystalline |
| CN115340077A (en) * | 2022-07-22 | 2022-11-15 | 承德莹科精细化工股份有限公司 | Preparation method of high-purity lanthanum phosphate |
| CN115340077B (en) * | 2022-07-22 | 2024-05-03 | 承德莹科精细化工股份有限公司 | Preparation method of high-purity lanthanum phosphate |
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