硫铁矿烧渣制备软磁用α-Fe_2O_3和磁记录材料γ-Fe_2O_3工艺及基础理论研究
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摘要
硫铁矿烧渣是用硫铁矿生产硫酸的过程中产生的工业废渣。一般每生产1t硫酸会产生0.8t烧渣,我国每年排放约1200万t硫铁矿烧渣,大量的烧渣排放和堆积,不仅浪费资源,占用土地,还造成了一系列的环境问题。硫铁矿烧渣处理已经成为我国固废处理的重大难题之一,如果能综合利用烧渣中的有效成分,不仅可以使废弃物资源化,提高企业效益,而且能够解决环境问题,因此具有重要的现实意义。本文利用硫铁矿烧渣制备铁氧体用高纯α-Fe203、透明氧化铁黄和磁记录材料γ-Fe203。
采用硫酸直接酸浸硫铁矿烧渣,铁屑还原酸浸液,利用空气氧化产生的新生相氢氧化铁胶体吸附沉降除硅和氟化铵沉淀除钙得到硫酸亚铁溶液,经碳酸盐转化为碳酸亚铁,煅烧后得到高纯的铁氧体用α-Fe203。在硫酸直接酸浸的过程中,反应温度118℃、硫酸浓度50%、硫酸用量系数1.1、反应时间4h,硫铁矿烧渣中铁的浸出率达到92.0%；用铁屑作还原剂,酸浸液中Fe3+浓度在1.6 mol·L-1左右可以得较快的反应速度和高的还原率；空气氧化絮凝法除硅和氟化铵沉淀除钙的过程中,控制反应温度60℃,氟化铵用量4g,pH值5.0～5.4,通入空气量0.2NM3/h,絮凝剂的用量为20-30ppm,静置陈化6-12h,过滤后获得纯净硫酸亚铁溶液,经浓缩、冷却结晶得到符合GB664-93化学试剂标准的硫酸亚铁；α-Fe203制备工艺为,将净化后的硫酸亚铁溶液调整FeS04浓度为lmol/L,初始pH为2-3,反应温度为室温(<40℃),在中强度的搅拌下,按理论值的1.1倍缓慢加入碳酸铵,反应时间为1小时后,经过滤、洗涤、干燥,在870℃温度下煅烧得到Fe203含量>99.4%,视比重0.95,紫棕红色,钙、硅含量均<0.01%,符合HG/T2574-94标准的铁氧体用α-Fe203。
采用空气氧化氨水滴加法,表面活性剂改性获得纳米晶形a-FeOOH。实验结果表明,a-FeOOH晶种制备条件为,硫酸亚铁浓度为40%、碱比为0.25、通气量为0.16-0.2m3/h、搅拌速度为500-600r/min及反应温度为30℃。二次氧化制备α-FeOOH的条件为晶种含量1.0%、初始亚铁浓度0.40-0.50mol/L、空气通气量0.6m3/h、搅拌速度800-900r/min及反应温度80℃。将得到的铁黄粒子经分散剂酒石酸及表面活性剂SDBS改性处理后,所得产品的晶型为a-FeOOH,粒子呈针状,长轴为95nm-125nm,短轴为18-25nm；无团聚现象,单分散性好,产品质量符合中华人民共和国化工行业标准HG/T2249-91。
在碱法制备磁记录材料Y-Fe203的研究中,研究了在强碱条件下空气氧化法制备针形α-FeOOH的反应过程,结果表明反应速率对Fe(Ⅱ)是动力学零级反应,反应表观活化能为6.84kJ/mol,其速率方程为：
反应机理是属于一固相Fe(OH)2转变为另一固相α-FeOOH的过程。反应条件对生成物的晶体形状有明显的影响,反应时的温度高、空气流量大、搅拌速率高、浓度、碱比适中时,产物结晶粗大完整、长度长,长宽比大。当反应条件在亚铁浓度0.3mol/L、反应温度40℃、空气流量0.2 m3/h、搅拌速率420rpm、碱比0.7时,获得产物粒子的长度为0.322μm、宽度为0.028μm、轴比为11.5的针形α-FeOOH.
经差热-热重分析得出α-FeOOH转化为α-Fe203的反应活化能为147.65kJ/mol,反应级数是0.81,反应机理为Valens二维扩散；脱水热处理在380℃的温度下,反应60min获得晶形完整的针形α-Fe203。
在α-Fe2O3氢气还原热处理制备Fe304的过程中,经热力学分析、XRD分析得出α-Fe203转化为Fe304时,存在多个相变,还原温度、氢气流量、还原时间对反应的产物产生明显影响,当在还原温度为360℃、还原时间为60min、氢气流量Q H2为150ml/min左右的条件下,获得了晶形完好的针形Fe3O4。
在Fe304空气氧化热处理制备γ-Fe203的过程中,经差热-热重分析、XRD分析和工艺试验得出Fe304转化为γ-Fe203时,存在两个相变过程,Fe304先被氧化转变成γ-Fe203,温度升到500℃后,Fe304转变成a-Fe203。当氧化温度在240℃下氧化45min,获得晶形完整的针形γ-Fe2O3。
溶胶-凝胶法制备γ-Fe2O3的研究表明,在柠檬酸铁溶液的浓度为0.8mo1/L,pH值为7,温度为40℃的反应条件下浓缩五分之四后形成了稳定络合型柠檬酸合铁,经真空减压干燥4h、再常压下,80℃干燥4h、110℃干燥8h后,获得柠檬酸合铁凝胶粉,在450℃下煅烧2.5h得到γ-Fe203。经TG-DTA、XRD、FT-IR表征得出柠檬酸合铁溶胶-凝胶粉转化成γ-Fe2O3的最佳温度是450℃, Scherrer公式计算和TEM表征得出,柠檬酸合铁溶胶-凝胶制备得到的γ-Fe203的粒子大小为32nm。
Pyrite cinder is the industry waste residue which is produced in the process of pyrite sulfuric acid manufacture. Every time along with production of 1 ton sulfuric acid is 0.8 ton of pyrite cinder,12,000,000 ton of pyrite cinder approximately have been discharged every year in China. As waste resources, such plentiful pyrite cinder emissions and stack, not only take land, but also work a series of environment problems. So, disposal of pyrite cinder has already become an important part of solid wastes in China. If we could use comprehensively beneficial ingredients in pyrite cinders, we not only might recycle national resources, enhancing the enterprises' benefits, but also could solve the environment problem, therefore it has vital practical significance. This thesis discusses how to use high-purityα-Fe2O3 for soft magnetic ferrite use, transparent iron oxide yellow, magnetic recording materialsγ-Fe2O3 have been prepared from pyrite cinder.
Using sulfuric acid to leach pyrite cinder, scrap iron was used to reduce acid leaching solution. A purifying ferrous sulfate solution was obtained after when the new Fe(OH)3 sol was created by passing it through air, furthermore adsorbed the impurities such as colloidal silicic acid and by using NH4F to remove Ca. The ferrous carbonate was obtained when the ferrous sulfate solution was reacted with carbonate. The high-purityα-Fe2O3 for ferrite use is up to the standard of HG/T2574-94 after dried the ferrous carbonate product is calcined at 870℃for 1h. In the process of leaching pyrite cinder with sulfuric acid, reaction temperature has the greatest influence on the rate of iron recovery. Under the controlled conditions that sulfuric acid concentration is 50%, coefficient of the sulfuric acid dosage is 1.1, reaction at 118℃for 4h, the rate of iron recovery is up to 92.0%. In the process of reducing acid leaching solution with scrap iron, there are the faster reactive velocity and the high percent of reduction when Fe3+ is reduced to Fe2+ under the conditions of Fe3+ concentration of 1.6mol/L in acid leaching solution. In the process of removing Si with oxidation-flocculation by passing it through air and removing Ca by sedimentation with NH4F, under the controlled conditions that reaction temperature is 60℃, NH4F dosage is 4g, the ferrous sulfate solution pH adjustment 6.0 by ammonia, air flow rate is 0.2NM3/h, when solution pH is up to 5.0 for atmosphere oxidation, the dosage of flocculant polyacrylamide is 20～30ppm, settled and ageing 6～12h, the purified ferrous sulfate solution is obtained by filtrating. FeSO4-7H2O was crystallized from the ferrous sulfate solution by concentrating and cooling that is up to the chemical reagent standard of GB664-93. In the process of preparativeα-Fe2O3, under the controlled conditions that the concentration of the ferrous sulfate solution is 1.Omol/L, beginning pH of the solution is 2-3, reaction temperature is room temperature (less than 40℃), under moderate strength stirred, slowing addition ammonium carbonate proportioning by academic cost 1.1 double, after reacting 1h, the quality of a-Fe2O3 for soft magnetic ferrite use product is up to the standard of HG/T2574-94 after dried ferrous carbonate product by filtrating and sluicing is calcined at 870℃for 1 h. The content of Fe2O3 in the a-Fe2O3 product attains 99.4%, the apparent gravity is 0.95 g/cm3, the appearance color is purple-brown-red, the content of silicon dioxide and calcium oxide in the a-Fe2O3 product can be reduced to less than 0.01%.
The nanometer crystalline forms a-FeOOH is obtained by air oxidizing, dropping ammonia and surfactant-modified method. The test results show that the eligible a-FeOOH crystal seed is obtained under the controlled conditions that ferrous sulfate concentration is 40%, alkaline ratio is 0.25, air flow rate 0.16-0.2m3/h, stirred rate 500-600r/min and reaction temperature at 30℃for 5h. In the process of secondary oxidation of a-FeOOH growth, the eligible a-FeOOH crystal is obtained under the controlled conditions that the content a-FeOOH crystal seed is 1.0%, beginning ferrous sulfate concentration is 0.40-0.50mol/L, air flow rate 0.6m3/h, stirred rate 800-900r/min and reaction temperature at 80℃for 50h. Finally, the goethite particle would be modification by dispersant tartaric acid and surfactant SDBS. The quality of a-FeOOH product is up to the standard of HG/T2574-94. The nanoparticles were characterized by X ray diffractometry (XRD), and transmission electron microscopy (TEM). The results showed that the homogenous acicular particles with good gloss and dispersion were a FeOOH. The average major axial diameter of the particles was 95-125 nm, and average minor axial diameter was 18-25 nm.
Preparation process of magnetic recording materials y-Fe2O3 was investigated in detailed. Reaction process of preparation of the acicular a-FeOOH by air oxidation in the alkali condition was researched. The results show that the reaction order is zero for Fe(II), apparent activation energy is 6.84kJ/mol, and its rate equation is:
The reaction mechanism is belong to the process of one solid ferrous hydroxide change from another solid goethite. The crystal shape of resultant have evident infection. The effect of process parameters such as reaction temperature, pH value, air rate, stirring rate, ferrous sulfate solution concentration and alkaline ratio on the crassitude and integrity of FeOOH particles was studied. The results showed that the ferrous sulfate solution concentration 0.3mol/L, reaction temperature 40℃, air rate 0.2 m3/h, stirring rate 420rpm, alkaline ratio 0.7 can be obtained acicular a-FeOOH of the average major axial diameter of the particles was 0.322μm, and average minor axial diameter was 0.028μm, and the aspect ratio was 11.5.
In the process that the a-FeOOH is changed toα-Fe2O3 by dehydrating heat treatment, TG-DAT test shows that the reaction order is 0.81 forα-FeOOH, apparent activation energy is 147.65kJ/mol, The reaction mechanism is belong to Valens planar diffusing. The crystal type integrity acicularα-Fe2O3 is obtained when the a-FeOOH was heat treatment at 380℃for 60min.
In the process that theα-Fe2O3 is changed to Fe3O4 by deoxidizing heat treatment with H2, thermodynamics analysis and XRD test shows that the deoxidizing process exists various phase change. The effect of process parameters such as deoxidizing reaction temperature, H2 flow, deoxidizing time on Fe304 particles was studied. The results showed that the deoxidizing reaction temperature 380℃, H2 flow 150ml/min, deoxidizing time 60min can be obtained the crystal type integrity acicular Fe3O4.
In the process that the Fe3O4 is changed toγ-Fe2O3by oxidizing heat treatment with air, TG-DAT, XRD and technics test shows that the oxidizing process exists two phase change. The effect of process parameters such as oxidizing reaction temperature, oxidizing time onγ-Fe2O3 particles was studied. The crystal type integrity acicular Y-Fe2O3 is obtained when the Fe3O4 was heat treatment at 240℃for 45min.
In the process of preparativeγ-Fe2O3 by sol-gel, the experimentation results showed that the complexing ferrite citrate sol was synthesized under the controlled conditions that ferrite citrate concentration is 0.8mol/L, the solution pH value was adjusted 7 by ammonia, reaction temperature at 40℃for concentrating 4/5. The Fe(III)-citrate complex gel powde was obtained that the Fe(III)-citrate complex was decompression dried in vacuum for 4h, dried in 80℃for 4h, dried in 110℃for 8h. The dry gel powder were analyzed by TG-DTA、XRD、FT-IR, The results show that theγ-Fe2O3 is obtained when dry gel powder was calcined at 450℃for 2.5h. The structure and crystal phase of the powders were characterized by XRDand TEM. Its primary crystal size calculated accurately by Deby-Scherrer equation was 32nm.
采用硫酸直接酸浸硫铁矿烧渣,铁屑还原酸浸液,利用空气氧化产生的新生相氢氧化铁胶体吸附沉降除硅和氟化铵沉淀除钙得到硫酸亚铁溶液,经碳酸盐转化为碳酸亚铁,煅烧后得到高纯的铁氧体用α-Fe203。在硫酸直接酸浸的过程中,反应温度118℃、硫酸浓度50%、硫酸用量系数1.1、反应时间4h,硫铁矿烧渣中铁的浸出率达到92.0%；用铁屑作还原剂,酸浸液中Fe3+浓度在1.6 mol·L-1左右可以得较快的反应速度和高的还原率；空气氧化絮凝法除硅和氟化铵沉淀除钙的过程中,控制反应温度60℃,氟化铵用量4g,pH值5.0～5.4,通入空气量0.2NM3/h,絮凝剂的用量为20-30ppm,静置陈化6-12h,过滤后获得纯净硫酸亚铁溶液,经浓缩、冷却结晶得到符合GB664-93化学试剂标准的硫酸亚铁；α-Fe203制备工艺为,将净化后的硫酸亚铁溶液调整FeS04浓度为lmol/L,初始pH为2-3,反应温度为室温(<40℃),在中强度的搅拌下,按理论值的1.1倍缓慢加入碳酸铵,反应时间为1小时后,经过滤、洗涤、干燥,在870℃温度下煅烧得到Fe203含量>99.4%,视比重0.95,紫棕红色,钙、硅含量均<0.01%,符合HG/T2574-94标准的铁氧体用α-Fe203。
采用空气氧化氨水滴加法,表面活性剂改性获得纳米晶形a-FeOOH。实验结果表明,a-FeOOH晶种制备条件为,硫酸亚铁浓度为40%、碱比为0.25、通气量为0.16-0.2m3/h、搅拌速度为500-600r/min及反应温度为30℃。二次氧化制备α-FeOOH的条件为晶种含量1.0%、初始亚铁浓度0.40-0.50mol/L、空气通气量0.6m3/h、搅拌速度800-900r/min及反应温度80℃。将得到的铁黄粒子经分散剂酒石酸及表面活性剂SDBS改性处理后,所得产品的晶型为a-FeOOH,粒子呈针状,长轴为95nm-125nm,短轴为18-25nm；无团聚现象,单分散性好,产品质量符合中华人民共和国化工行业标准HG/T2249-91。
在碱法制备磁记录材料Y-Fe203的研究中,研究了在强碱条件下空气氧化法制备针形α-FeOOH的反应过程,结果表明反应速率对Fe(Ⅱ)是动力学零级反应,反应表观活化能为6.84kJ/mol,其速率方程为：
反应机理是属于一固相Fe(OH)2转变为另一固相α-FeOOH的过程。反应条件对生成物的晶体形状有明显的影响,反应时的温度高、空气流量大、搅拌速率高、浓度、碱比适中时,产物结晶粗大完整、长度长,长宽比大。当反应条件在亚铁浓度0.3mol/L、反应温度40℃、空气流量0.2 m3/h、搅拌速率420rpm、碱比0.7时,获得产物粒子的长度为0.322μm、宽度为0.028μm、轴比为11.5的针形α-FeOOH.
经差热-热重分析得出α-FeOOH转化为α-Fe203的反应活化能为147.65kJ/mol,反应级数是0.81,反应机理为Valens二维扩散；脱水热处理在380℃的温度下,反应60min获得晶形完整的针形α-Fe203。
在α-Fe2O3氢气还原热处理制备Fe304的过程中,经热力学分析、XRD分析得出α-Fe203转化为Fe304时,存在多个相变,还原温度、氢气流量、还原时间对反应的产物产生明显影响,当在还原温度为360℃、还原时间为60min、氢气流量Q H2为150ml/min左右的条件下,获得了晶形完好的针形Fe3O4。
在Fe304空气氧化热处理制备γ-Fe203的过程中,经差热-热重分析、XRD分析和工艺试验得出Fe304转化为γ-Fe203时,存在两个相变过程,Fe304先被氧化转变成γ-Fe203,温度升到500℃后,Fe304转变成a-Fe203。当氧化温度在240℃下氧化45min,获得晶形完整的针形γ-Fe2O3。
溶胶-凝胶法制备γ-Fe2O3的研究表明,在柠檬酸铁溶液的浓度为0.8mo1/L,pH值为7,温度为40℃的反应条件下浓缩五分之四后形成了稳定络合型柠檬酸合铁,经真空减压干燥4h、再常压下,80℃干燥4h、110℃干燥8h后,获得柠檬酸合铁凝胶粉,在450℃下煅烧2.5h得到γ-Fe203。经TG-DTA、XRD、FT-IR表征得出柠檬酸合铁溶胶-凝胶粉转化成γ-Fe2O3的最佳温度是450℃, Scherrer公式计算和TEM表征得出,柠檬酸合铁溶胶-凝胶制备得到的γ-Fe203的粒子大小为32nm。
Pyrite cinder is the industry waste residue which is produced in the process of pyrite sulfuric acid manufacture. Every time along with production of 1 ton sulfuric acid is 0.8 ton of pyrite cinder,12,000,000 ton of pyrite cinder approximately have been discharged every year in China. As waste resources, such plentiful pyrite cinder emissions and stack, not only take land, but also work a series of environment problems. So, disposal of pyrite cinder has already become an important part of solid wastes in China. If we could use comprehensively beneficial ingredients in pyrite cinders, we not only might recycle national resources, enhancing the enterprises' benefits, but also could solve the environment problem, therefore it has vital practical significance. This thesis discusses how to use high-purityα-Fe2O3 for soft magnetic ferrite use, transparent iron oxide yellow, magnetic recording materialsγ-Fe2O3 have been prepared from pyrite cinder.
Using sulfuric acid to leach pyrite cinder, scrap iron was used to reduce acid leaching solution. A purifying ferrous sulfate solution was obtained after when the new Fe(OH)3 sol was created by passing it through air, furthermore adsorbed the impurities such as colloidal silicic acid and by using NH4F to remove Ca. The ferrous carbonate was obtained when the ferrous sulfate solution was reacted with carbonate. The high-purityα-Fe2O3 for ferrite use is up to the standard of HG/T2574-94 after dried the ferrous carbonate product is calcined at 870℃for 1h. In the process of leaching pyrite cinder with sulfuric acid, reaction temperature has the greatest influence on the rate of iron recovery. Under the controlled conditions that sulfuric acid concentration is 50%, coefficient of the sulfuric acid dosage is 1.1, reaction at 118℃for 4h, the rate of iron recovery is up to 92.0%. In the process of reducing acid leaching solution with scrap iron, there are the faster reactive velocity and the high percent of reduction when Fe3+ is reduced to Fe2+ under the conditions of Fe3+ concentration of 1.6mol/L in acid leaching solution. In the process of removing Si with oxidation-flocculation by passing it through air and removing Ca by sedimentation with NH4F, under the controlled conditions that reaction temperature is 60℃, NH4F dosage is 4g, the ferrous sulfate solution pH adjustment 6.0 by ammonia, air flow rate is 0.2NM3/h, when solution pH is up to 5.0 for atmosphere oxidation, the dosage of flocculant polyacrylamide is 20～30ppm, settled and ageing 6～12h, the purified ferrous sulfate solution is obtained by filtrating. FeSO4-7H2O was crystallized from the ferrous sulfate solution by concentrating and cooling that is up to the chemical reagent standard of GB664-93. In the process of preparativeα-Fe2O3, under the controlled conditions that the concentration of the ferrous sulfate solution is 1.Omol/L, beginning pH of the solution is 2-3, reaction temperature is room temperature (less than 40℃), under moderate strength stirred, slowing addition ammonium carbonate proportioning by academic cost 1.1 double, after reacting 1h, the quality of a-Fe2O3 for soft magnetic ferrite use product is up to the standard of HG/T2574-94 after dried ferrous carbonate product by filtrating and sluicing is calcined at 870℃for 1 h. The content of Fe2O3 in the a-Fe2O3 product attains 99.4%, the apparent gravity is 0.95 g/cm3, the appearance color is purple-brown-red, the content of silicon dioxide and calcium oxide in the a-Fe2O3 product can be reduced to less than 0.01%.
The nanometer crystalline forms a-FeOOH is obtained by air oxidizing, dropping ammonia and surfactant-modified method. The test results show that the eligible a-FeOOH crystal seed is obtained under the controlled conditions that ferrous sulfate concentration is 40%, alkaline ratio is 0.25, air flow rate 0.16-0.2m3/h, stirred rate 500-600r/min and reaction temperature at 30℃for 5h. In the process of secondary oxidation of a-FeOOH growth, the eligible a-FeOOH crystal is obtained under the controlled conditions that the content a-FeOOH crystal seed is 1.0%, beginning ferrous sulfate concentration is 0.40-0.50mol/L, air flow rate 0.6m3/h, stirred rate 800-900r/min and reaction temperature at 80℃for 50h. Finally, the goethite particle would be modification by dispersant tartaric acid and surfactant SDBS. The quality of a-FeOOH product is up to the standard of HG/T2574-94. The nanoparticles were characterized by X ray diffractometry (XRD), and transmission electron microscopy (TEM). The results showed that the homogenous acicular particles with good gloss and dispersion were a FeOOH. The average major axial diameter of the particles was 95-125 nm, and average minor axial diameter was 18-25 nm.
Preparation process of magnetic recording materials y-Fe2O3 was investigated in detailed. Reaction process of preparation of the acicular a-FeOOH by air oxidation in the alkali condition was researched. The results show that the reaction order is zero for Fe(II), apparent activation energy is 6.84kJ/mol, and its rate equation is:
The reaction mechanism is belong to the process of one solid ferrous hydroxide change from another solid goethite. The crystal shape of resultant have evident infection. The effect of process parameters such as reaction temperature, pH value, air rate, stirring rate, ferrous sulfate solution concentration and alkaline ratio on the crassitude and integrity of FeOOH particles was studied. The results showed that the ferrous sulfate solution concentration 0.3mol/L, reaction temperature 40℃, air rate 0.2 m3/h, stirring rate 420rpm, alkaline ratio 0.7 can be obtained acicular a-FeOOH of the average major axial diameter of the particles was 0.322μm, and average minor axial diameter was 0.028μm, and the aspect ratio was 11.5.
In the process that the a-FeOOH is changed toα-Fe2O3 by dehydrating heat treatment, TG-DAT test shows that the reaction order is 0.81 forα-FeOOH, apparent activation energy is 147.65kJ/mol, The reaction mechanism is belong to Valens planar diffusing. The crystal type integrity acicularα-Fe2O3 is obtained when the a-FeOOH was heat treatment at 380℃for 60min.
In the process that theα-Fe2O3 is changed to Fe3O4 by deoxidizing heat treatment with H2, thermodynamics analysis and XRD test shows that the deoxidizing process exists various phase change. The effect of process parameters such as deoxidizing reaction temperature, H2 flow, deoxidizing time on Fe304 particles was studied. The results showed that the deoxidizing reaction temperature 380℃, H2 flow 150ml/min, deoxidizing time 60min can be obtained the crystal type integrity acicular Fe3O4.
In the process that the Fe3O4 is changed toγ-Fe2O3by oxidizing heat treatment with air, TG-DAT, XRD and technics test shows that the oxidizing process exists two phase change. The effect of process parameters such as oxidizing reaction temperature, oxidizing time onγ-Fe2O3 particles was studied. The crystal type integrity acicular Y-Fe2O3 is obtained when the Fe3O4 was heat treatment at 240℃for 45min.
In the process of preparativeγ-Fe2O3 by sol-gel, the experimentation results showed that the complexing ferrite citrate sol was synthesized under the controlled conditions that ferrite citrate concentration is 0.8mol/L, the solution pH value was adjusted 7 by ammonia, reaction temperature at 40℃for concentrating 4/5. The Fe(III)-citrate complex gel powde was obtained that the Fe(III)-citrate complex was decompression dried in vacuum for 4h, dried in 80℃for 4h, dried in 110℃for 8h. The dry gel powder were analyzed by TG-DTA、XRD、FT-IR, The results show that theγ-Fe2O3 is obtained when dry gel powder was calcined at 450℃for 2.5h. The structure and crystal phase of the powders were characterized by XRDand TEM. Its primary crystal size calculated accurately by Deby-Scherrer equation was 32nm.
引文
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