不同粒径纳米碱土氟化物粉体的制备及热稳定性研究
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摘要
本论文采用微乳液,水溶液直接沉淀,双注小区反应和醇/水混合溶剂沉淀四种湿化学方法研究了碱土金属氟化物BaF_2,CaF_2和SrF_2纳米粉体的制备科学和技术,目的在于获得粒径可控的碱土金属氟化物纳米粉体,并研究其晶粒尺寸热稳定性,为碱土金属氟化物纳米粉体和块材的性能和应用研究打好基础。
首先,采用CTAB/丁醇/庚烷/水四组分体系微乳液制备BaF_2纳米粉体,研究了体系组分的含量和配比对微乳液稳定性和对BaF_2粒径形貌的影响。结果表明,采用丁醇和CTAB质量比1:1有利于形成稳定的微乳液,BaF_2粒径大小和分布随微乳液体系中CTAB和水质量比升高而增大,获得了粒径为10nm的BaF_2纳米粉体。
微乳液法虽然容易控制粒径,但产量低,成本高,本文研究了具有高产量和低成本优势的水溶液直接沉淀法制备BaF_2纳米粉体。根据过饱和度对沉淀粒径和分布影响的理论,用不同反应物浓度和混合方式制备BaF_2沉淀,还研究了临界过饱和附近的沉淀情况。结果表明,缓慢滴加混合,过饱和度低,非均相形核比重大,利于沉淀颗粒长大,反应物浓度对粒径的影响大,获得了亚微米级沉淀;快速混合沉淀,有利于形成高过饱和,利于均相形核,利于生成粒径小的沉淀,反应物浓度对粒径影响小,获得了80nm沉淀。在临界过饱和度值1.2附近获得粒径为10nm的BaF_2沉淀。
为了进一步提高反应的过饱和度和均匀性,研究了极高过饱和度对沉淀粒径和分布的影响,设计了双注小区反应装置,同时还研究NH_4F溶液浓度和表面活性剂的影响。结果表明,双注小区反应形成极高的过饱和度,沉淀初期形成大量极小的粒子,但极不稳定,小粒子长大后,粒径和分布没有较大改观。长大后的沉淀似乎没有受到反应高过饱和度和初期沉淀小粒子的影响,推测这是水溶液中的一种本征的稳定状态。改变NH_4F溶液浓度和使用表面活性剂对沉淀粒径和分布也没有发生明显影响。可以认为,当过饱和度高于一定值后,继续提高过饱和度和过饱和度均匀性对沉淀粒径和分布减小没有明显效果。
为了研究溶解度对沉淀物粒径的影响,使用低介电常数的醇/水混合溶剂沉淀制备了BaF_2纳米粉体。用纯水溶剂,水和乙醇体积比分别为3:1,1:1,3:5和1:4的不同混合溶剂沉淀得到了粒径分别为70nm,61nm,52nm,43nm和33nm的BaF_2纳米粉体。粒径随混合溶剂乙醇含量升高而减小,分散性和形貌规则性随之改善。乙醇/水混合溶剂制备的BaF_2沉淀粒径的倒数和溶剂介电常数倒数呈线性关系。通过混合溶剂成功控制了沉淀粒径。
The wet chemical methods of microemulsion, aqueous precipitation, double jet and water/ethanol mixed solvents were applied to synthesize nanocrystalline of alkaline fluorides including BaF_2, CaF_2 and SrF_2. The object of this dissertation is to obtain nanocrystalline of alkaline fluorides with controllable particle size, study the thermo-stability, and provide fundamental data for the research of properties and application of nanocrystalline alkaline fluorides powders and bulk materials.Firstly, Cetyltrimethylammonium bromide(CTAB)/butanol/heptane/water microemulsion system was applied to synthesize BaF_2 nanoparticles. The influences of the mass ratio of butanol to CTAB, the content of heptane and water, and the species of solute in water phase on the stability of microemulsion system and resultant BaF_2 particle size and size distribution were investigated. It was found that, the mass ratio 1 : 1 of butanol to CTAB favor to form stable microemulsion, and about 10nm BaF_2 particles with well monodispersed and ball-shaped were synthesized by reaction of stable Ba(NO_3)_2 microemulsion and NH_4F microemulsion, the BaF_2 particle size and distribution decreases with the mass ratio of CTAB to water increasing.Although it is easy to control the particle size of fluorides while synthesized with the method of microemulsion, the productivity of the method is quite low and cost is relatively high. A high productive and low cost method — aqueous precipitation was applied to syntheses nanocrystalline BaF_2. Based on the dependence of precipitate particle size and size distribution on the supersaturation, different reactant concentration and mixed manner were utilized to change supersaturation, and the precipitation in the vicinity of the critical supersaturation was also investigated. The results indicated that particles were easy to grow into submicro-crystalline, as the supersaturation was quite low while the reactants were added in droplet mode. In rapidly mixing mode, the particle size of resultants was much smaller as the supersaturation was relatively high. The nano-BaF_2 powders with the size of about 10nm were produced when the reactions happened in the vicinity of the critical supersaturation.A device for double jet reaction was designed and the influence of ultrahigh supersaturation on the particle size and size distribution was study so as to increase the supersaturation and uniformity of precipitation. The influences of surfactants and the concentration of NH4F solution were also studied. The results indicated that the method of double jet could provide very high supersaturation and large numbers of ultrafine particles
formed at the beginning of precipitation. But the ultrafine particles were quite unstable and tend to grow into large particles, seem that they had not been affect by early supersaturation. It can be deduced to be an intrinsic stable state of aqueous precipitation. The concentration variety of NH4F solution and the application surfactants had little influence on the particle size and distribution. It can be deduced that further increase of supersaturation is not a effective method to obtain smaller particles and narrower distribution.A low dielectric constant system of water/ethanol mixed solvents was applied to synthesize nano-BaF2 powders so as to investigate the dependence of the particle size of the precipitates on the solubility. The average particle size 70nm, 61nm, 52nm, 43nm and 33nm of nano-BaF2 powders were obtained separately in pure water solvent and mixed solvents with the volume ratio of water to ethanol 3 I 1,1 I 1,3 I 5 and 1 : 4. The results indicated that the particle size of nano-BaF2 powders decreases with increasing the volume ratio of ethanol to water of the mixed solvents, and the dispersion and the morphology are better together. The relationship between the reciprocal of BaF2 particle size and the reciprocal of dielectric constant of mixed solvents is linear. This work showed the particle size can be successfully controlled by the mixed solvents.Ethanol/Water mixed solvents were also used to prepare nano-CaF2 powders with different particle size. CaF2 powders well dispersed , narrow size distribution, with the particle size 242nm, 78.7nm, 51nm, 31nm, 22.7nm and 14nm were obtained by combining the aqueous solvents with low reactant supersaturation and mixed solvents. The results showed that relatively bigger particles can be synthesized in the condition of low reactant supersaturation, small particles can be produced in mixed solvents. Precipitates with average size from micrometer to several nanometer region can be controllably synthesized by combining the low supersaturation manner and mixed solvent manner.Nano-SrF2 powders were synthesized by precipitation in the ethanol/water mixed solvents. Well dispersed Nano-SrF2 powders with the average size 32nm, 18.6nm, 23.2nm, 16nm, and 14.9nm were obtained in pure water solvent and mixed solvents with the volume ratio of water to ethanol 3 : 1, 1 : 1, 3 .' 5 and 1 ! 4, respectively.Finally, the thermal stability of Nano-BaF2 powders with different particle size was investigated by Differential scanning calorimetry (DSC). By Kissinger equation, the activation energy of BaF2 nanopowder with particle size 70nm, 52nm, 43nm and 33nm is 187.8KJ/mol or 1.947eV, 137.1KJ/mol or 1.422eV, 132.2KJ/mol or 1.371eV, 111.167KJ/mol or 1.153eV, respectively. An interesting result was showed that the activation energy
decreased linearly to the particle size of nanocrystalline BaF2 powders decreasing, which can be explained in terms of the larger grains grow at the expense of the smaller ones in the grain growth.
首先,采用CTAB/丁醇/庚烷/水四组分体系微乳液制备BaF_2纳米粉体,研究了体系组分的含量和配比对微乳液稳定性和对BaF_2粒径形貌的影响。结果表明,采用丁醇和CTAB质量比1:1有利于形成稳定的微乳液,BaF_2粒径大小和分布随微乳液体系中CTAB和水质量比升高而增大,获得了粒径为10nm的BaF_2纳米粉体。
微乳液法虽然容易控制粒径,但产量低,成本高,本文研究了具有高产量和低成本优势的水溶液直接沉淀法制备BaF_2纳米粉体。根据过饱和度对沉淀粒径和分布影响的理论,用不同反应物浓度和混合方式制备BaF_2沉淀,还研究了临界过饱和附近的沉淀情况。结果表明,缓慢滴加混合,过饱和度低,非均相形核比重大,利于沉淀颗粒长大,反应物浓度对粒径的影响大,获得了亚微米级沉淀;快速混合沉淀,有利于形成高过饱和,利于均相形核,利于生成粒径小的沉淀,反应物浓度对粒径影响小,获得了80nm沉淀。在临界过饱和度值1.2附近获得粒径为10nm的BaF_2沉淀。
为了进一步提高反应的过饱和度和均匀性,研究了极高过饱和度对沉淀粒径和分布的影响,设计了双注小区反应装置,同时还研究NH_4F溶液浓度和表面活性剂的影响。结果表明,双注小区反应形成极高的过饱和度,沉淀初期形成大量极小的粒子,但极不稳定,小粒子长大后,粒径和分布没有较大改观。长大后的沉淀似乎没有受到反应高过饱和度和初期沉淀小粒子的影响,推测这是水溶液中的一种本征的稳定状态。改变NH_4F溶液浓度和使用表面活性剂对沉淀粒径和分布也没有发生明显影响。可以认为,当过饱和度高于一定值后,继续提高过饱和度和过饱和度均匀性对沉淀粒径和分布减小没有明显效果。
为了研究溶解度对沉淀物粒径的影响,使用低介电常数的醇/水混合溶剂沉淀制备了BaF_2纳米粉体。用纯水溶剂,水和乙醇体积比分别为3:1,1:1,3:5和1:4的不同混合溶剂沉淀得到了粒径分别为70nm,61nm,52nm,43nm和33nm的BaF_2纳米粉体。粒径随混合溶剂乙醇含量升高而减小,分散性和形貌规则性随之改善。乙醇/水混合溶剂制备的BaF_2沉淀粒径的倒数和溶剂介电常数倒数呈线性关系。通过混合溶剂成功控制了沉淀粒径。
The wet chemical methods of microemulsion, aqueous precipitation, double jet and water/ethanol mixed solvents were applied to synthesize nanocrystalline of alkaline fluorides including BaF_2, CaF_2 and SrF_2. The object of this dissertation is to obtain nanocrystalline of alkaline fluorides with controllable particle size, study the thermo-stability, and provide fundamental data for the research of properties and application of nanocrystalline alkaline fluorides powders and bulk materials.Firstly, Cetyltrimethylammonium bromide(CTAB)/butanol/heptane/water microemulsion system was applied to synthesize BaF_2 nanoparticles. The influences of the mass ratio of butanol to CTAB, the content of heptane and water, and the species of solute in water phase on the stability of microemulsion system and resultant BaF_2 particle size and size distribution were investigated. It was found that, the mass ratio 1 : 1 of butanol to CTAB favor to form stable microemulsion, and about 10nm BaF_2 particles with well monodispersed and ball-shaped were synthesized by reaction of stable Ba(NO_3)_2 microemulsion and NH_4F microemulsion, the BaF_2 particle size and distribution decreases with the mass ratio of CTAB to water increasing.Although it is easy to control the particle size of fluorides while synthesized with the method of microemulsion, the productivity of the method is quite low and cost is relatively high. A high productive and low cost method — aqueous precipitation was applied to syntheses nanocrystalline BaF_2. Based on the dependence of precipitate particle size and size distribution on the supersaturation, different reactant concentration and mixed manner were utilized to change supersaturation, and the precipitation in the vicinity of the critical supersaturation was also investigated. The results indicated that particles were easy to grow into submicro-crystalline, as the supersaturation was quite low while the reactants were added in droplet mode. In rapidly mixing mode, the particle size of resultants was much smaller as the supersaturation was relatively high. The nano-BaF_2 powders with the size of about 10nm were produced when the reactions happened in the vicinity of the critical supersaturation.A device for double jet reaction was designed and the influence of ultrahigh supersaturation on the particle size and size distribution was study so as to increase the supersaturation and uniformity of precipitation. The influences of surfactants and the concentration of NH4F solution were also studied. The results indicated that the method of double jet could provide very high supersaturation and large numbers of ultrafine particles
formed at the beginning of precipitation. But the ultrafine particles were quite unstable and tend to grow into large particles, seem that they had not been affect by early supersaturation. It can be deduced to be an intrinsic stable state of aqueous precipitation. The concentration variety of NH4F solution and the application surfactants had little influence on the particle size and distribution. It can be deduced that further increase of supersaturation is not a effective method to obtain smaller particles and narrower distribution.A low dielectric constant system of water/ethanol mixed solvents was applied to synthesize nano-BaF2 powders so as to investigate the dependence of the particle size of the precipitates on the solubility. The average particle size 70nm, 61nm, 52nm, 43nm and 33nm of nano-BaF2 powders were obtained separately in pure water solvent and mixed solvents with the volume ratio of water to ethanol 3 I 1,1 I 1,3 I 5 and 1 : 4. The results indicated that the particle size of nano-BaF2 powders decreases with increasing the volume ratio of ethanol to water of the mixed solvents, and the dispersion and the morphology are better together. The relationship between the reciprocal of BaF2 particle size and the reciprocal of dielectric constant of mixed solvents is linear. This work showed the particle size can be successfully controlled by the mixed solvents.Ethanol/Water mixed solvents were also used to prepare nano-CaF2 powders with different particle size. CaF2 powders well dispersed , narrow size distribution, with the particle size 242nm, 78.7nm, 51nm, 31nm, 22.7nm and 14nm were obtained by combining the aqueous solvents with low reactant supersaturation and mixed solvents. The results showed that relatively bigger particles can be synthesized in the condition of low reactant supersaturation, small particles can be produced in mixed solvents. Precipitates with average size from micrometer to several nanometer region can be controllably synthesized by combining the low supersaturation manner and mixed solvent manner.Nano-SrF2 powders were synthesized by precipitation in the ethanol/water mixed solvents. Well dispersed Nano-SrF2 powders with the average size 32nm, 18.6nm, 23.2nm, 16nm, and 14.9nm were obtained in pure water solvent and mixed solvents with the volume ratio of water to ethanol 3 : 1, 1 : 1, 3 .' 5 and 1 ! 4, respectively.Finally, the thermal stability of Nano-BaF2 powders with different particle size was investigated by Differential scanning calorimetry (DSC). By Kissinger equation, the activation energy of BaF2 nanopowder with particle size 70nm, 52nm, 43nm and 33nm is 187.8KJ/mol or 1.947eV, 137.1KJ/mol or 1.422eV, 132.2KJ/mol or 1.371eV, 111.167KJ/mol or 1.153eV, respectively. An interesting result was showed that the activation energy
decreased linearly to the particle size of nanocrystalline BaF2 powders decreasing, which can be explained in terms of the larger grains grow at the expense of the smaller ones in the grain growth.
引文
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