机械化学法制备氧化物陶瓷过程及动力学研究
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摘要
在机械化学反应动力学中引入结构转变分析,并借鉴燃烧合成领域的结构宏观动力学理论,本文提出了机械化学反应结构宏观动力学及其研究方法,从化学反应和物质结构转变两方面共同对材料的机械化学合成过程进行考察并成功应用于锐钛矿型TiO2、CaO+TiO2以及Fe2O3+ZnO体系的研究。
主要结论如下：
1、剪切力促进了锐钛矿相的晶型转变,通过改变机械力作用方式,可望实现锐钛矿型Ti02沿着不同的相变途径转化,这对合成有晶型组成要求的Ti02陶瓷材料具有实际参考价值。本实验条件下的研究表明,锐钛矿型Ti02在行星球磨机和搅拌球磨机中的相变历程表现为锐钛矿相→TiO2-Ⅱ相→金红石相的分步相变；在振动磨样机中除了分步相变外,还发生了锐钛矿相→金红石相的直接相变。
2、在相同研磨条件下,碱土金属氧化物MgO、CaO、BaO与锐钛矿型Ti02的机械化学反应速率依次增大。实验表明,机械化学合成中存在同系递变现象。锐钛矿型Ti02与碱土金属氧化物的机械化学反应过程中可发生锐钛矿相的相变,导致反应过程存在差异。
(1)在MgO+TiO2体系中,锐钛矿型TiO2难以直接与MgO发生反应得到MgTiO3,而是首先发生锐钛矿型Ti02向TiO2-Ⅱ相的转变,新生相TiO2-Ⅱ较锐钛矿相有更好的反应活性,可以与MgO发生反应得到MgTiO3。
体系存在如下的化学反应：TiO2(Anatase)→TiO2-Ⅱ AO+TiO2-Ⅱ→ATiO3
(2)对于CaO+TiO2及BaO+TiO2体系,未检测到TiO2-Ⅱ相,锐钛矿型TiO2易与CaO和BaO直接发生反应得到CaTiO3和BaTiO3。
体系存在如下的化学反应：AO+TiO2(Anatase)→ATiO3
3、在相同研磨条件下,CuO、NiO、ZnO三种金属氧化物与Fe2O3的机械化学反应速率依次增大。研究表明,反应物和生成物的结构相似,则反应容易进行；反之,则反应相对困难。
4、锐钛矿型Ti02体系生成金红石相的机械化学相变动力学、CaO+TiO2体系和Fe2O3+ZnO体系的机械化学反应动力学均满足Avrami-Erofe'ev模型,属于形核生长机制,表明产物晶核随机产生并随后长大。
(1)锐钛矿型Ti02体系的相变动力学方程为：[-ln(1-α)1/1.9147＝0.2484t(振动磨样机,710rpm)
(2)CaO+TiO2体系的反应动力学方程为：[-ln(1-α)]1/0.8685=0.3658t(行星球磨机,500rpm,球料比20：1)
(3)Fe2O3+ZnO体系的反应动力学方程为：[-ln(1-α)]1/133262=0.0859t(行星球磨机,500rpm,球料比20：1)
5、以Fe2O3+ZnO体系合成ZnFe2O4的机械化学过程为例,进行了动力学的能量方法研究。研究表明,Fe2O3+ZnO体系的机械化学反应按Avrami-Erofe'ev动力学模型拟合可以得到很好的拟合效果。在本实验条件下,对于确定的球料比,反应转化率只与能量输入直接相关。用能量代替研磨时间来度量机械化学反应动力学可有较少的研磨参数限制。动力学方程在不同球料比条件下的具体形式为：[-ln(1-α)]1/1.3179=0.0254EKum(球料比40：1)[-ln(1-α)]1/1.3706=0.0151EKum(球料比20：1)
By introducing the structural transformation analysis into the kinetics of mechanochemical reaction and borrowing the structural macrokinetics research theory from the combustion synthesis, the structural macrokinetics of mechanochemical reaction and its research methods are put forward in this thesis. Based on the chemical reaction and material structure transformation, the mechanochemical processes were investigated and the research methods were applied successfully to the anatase TiO2, CaO+TiO2and Fe2O3+ZnO systems.
The main conclusions are as follows:
1. The shear force can promote the crystal transfer of anatase phase. By changing the action mode of mechanical force, the phase transformation of anatase can be expected to proceed along different courses, which is of practical reference value to synthesize TiO2ceramic material with the demands of crystal form. Results show that under our experimental conditions the anatase TiO2powder is demonstrated to induce different phase transformation phenomena with mechanical processing:a step-by-step transformation from anatase to TiO2-Ⅱ and then to rutile in all three mills:a planetary ball mill, an attritor and a ring-roller mill; besides a direct transformation from anatase to rutile in the ring-roller mill.
2. Under the same milling conditions, the mechanochemical reaction rates increased in turn when the alkaline-earth metal oxides MgO, CaO and BaO were milled with anatase, respectively, which indicates the existence of an alternation phenomenon along main group elements. Phase transformation might occur in anatase when it was milled with alkaline-earth metal oxides, which results in the different courses of reaction.
(1) In the system MgO+TiO2, it is hard to synthesize MgTiO3directly from the reaction of MgO with anatase TiO2. Experimental results show that the TiO2-Ⅱ, as a newborn phase with better reactivity than anatase TiO2, is firstly transformed from anatase TiO2with mechanical force, and MgTiO3can be formed through the reaction of MgO with the TiO2-Ⅱ.
There exist the chemical reactions in the system as follows: TiO2(Anatase)→TiO2-Ⅱ AO+TiO2-Ⅱ→ATiO3
(2) For the system CaO+TiO2and BaO+TiO2, TiO2-Ⅱ was not detected during the course of milling. And experimental results show that it is easy for anatase TiO2to directly react with CaO and BaO to form CaTiO3and BaTiO3, respectively. There exists the chemical reaction in the two systems as follows: AO+TiO2(Anatase)→ATiO3
3. Under the same milling conditions, the mechanochemical reaction rates increased in turn when the metallic oxides CuO, NiO and ZnO were milled with Fe2O3, respectively. Results show that with a similar structure between the reactant and the resultant, the reaction runs smoothly; otherwise, it runs relatively hard.
4. The mechanochemical kinetics of phase transformation to rutile in anatase system and reactions in both CaO+TiO2and Fe2O3+ZnO systems, are best expressed by Avrami-Erofe'ev model, which indicates the random nucleation of products phase followed by a growth of nuclei.
(1) The kinetic equation of anatase system is as:[-1n(1-α)]1/1.9147=0.2484t (Ring-roller mill,710rpm)
(2) The kinetic equation of CaO+TiO2system is as:[-ln(1-α)]1/08685=0.36581(Planetary ball mill,500rpm, BPR=20:1)
(3) The kinetic equation of Fe2O3+ZnO system is as:[-ln(1-α)]1/13262=0.0859/(Planetary ball mill,500rpm, BPR=20:1)
5. Taking the mechanochemical synthesis of ZnFe2O4by milling Fe2O3+ZnO mixed powders for example, the reaction kinetics was studied by energetic approach in this thesis. Results show that a fine effect could be obtained when Avrami-Erofe'ev kinetics model is used to fit the mechanochemical reaction. When it is under a certain BPR, the reaction conversion degree only directly relates to the energy dose. Energy-scaled knetics of mechanochemical reaction has less restriction on milling parameters than time-scaled kinetics.The kinetic equations under different BPR are as follows:
[-ln(1-α)]1/1.3179=0.0254Ekum(BPR=40:1)
[-ln(1-α)]1/13706=0.0151Ekum(BPR=20:1)
主要结论如下：
1、剪切力促进了锐钛矿相的晶型转变,通过改变机械力作用方式,可望实现锐钛矿型Ti02沿着不同的相变途径转化,这对合成有晶型组成要求的Ti02陶瓷材料具有实际参考价值。本实验条件下的研究表明,锐钛矿型Ti02在行星球磨机和搅拌球磨机中的相变历程表现为锐钛矿相→TiO2-Ⅱ相→金红石相的分步相变；在振动磨样机中除了分步相变外,还发生了锐钛矿相→金红石相的直接相变。
2、在相同研磨条件下,碱土金属氧化物MgO、CaO、BaO与锐钛矿型Ti02的机械化学反应速率依次增大。实验表明,机械化学合成中存在同系递变现象。锐钛矿型Ti02与碱土金属氧化物的机械化学反应过程中可发生锐钛矿相的相变,导致反应过程存在差异。
(1)在MgO+TiO2体系中,锐钛矿型TiO2难以直接与MgO发生反应得到MgTiO3,而是首先发生锐钛矿型Ti02向TiO2-Ⅱ相的转变,新生相TiO2-Ⅱ较锐钛矿相有更好的反应活性,可以与MgO发生反应得到MgTiO3。
体系存在如下的化学反应：TiO2(Anatase)→TiO2-Ⅱ AO+TiO2-Ⅱ→ATiO3
(2)对于CaO+TiO2及BaO+TiO2体系,未检测到TiO2-Ⅱ相,锐钛矿型TiO2易与CaO和BaO直接发生反应得到CaTiO3和BaTiO3。
体系存在如下的化学反应：AO+TiO2(Anatase)→ATiO3
3、在相同研磨条件下,CuO、NiO、ZnO三种金属氧化物与Fe2O3的机械化学反应速率依次增大。研究表明,反应物和生成物的结构相似,则反应容易进行；反之,则反应相对困难。
4、锐钛矿型Ti02体系生成金红石相的机械化学相变动力学、CaO+TiO2体系和Fe2O3+ZnO体系的机械化学反应动力学均满足Avrami-Erofe'ev模型,属于形核生长机制,表明产物晶核随机产生并随后长大。
(1)锐钛矿型Ti02体系的相变动力学方程为：[-ln(1-α)1/1.9147＝0.2484t(振动磨样机,710rpm)
(2)CaO+TiO2体系的反应动力学方程为：[-ln(1-α)]1/0.8685=0.3658t(行星球磨机,500rpm,球料比20：1)
(3)Fe2O3+ZnO体系的反应动力学方程为：[-ln(1-α)]1/133262=0.0859t(行星球磨机,500rpm,球料比20：1)
5、以Fe2O3+ZnO体系合成ZnFe2O4的机械化学过程为例,进行了动力学的能量方法研究。研究表明,Fe2O3+ZnO体系的机械化学反应按Avrami-Erofe'ev动力学模型拟合可以得到很好的拟合效果。在本实验条件下,对于确定的球料比,反应转化率只与能量输入直接相关。用能量代替研磨时间来度量机械化学反应动力学可有较少的研磨参数限制。动力学方程在不同球料比条件下的具体形式为：[-ln(1-α)]1/1.3179=0.0254EKum(球料比40：1)[-ln(1-α)]1/1.3706=0.0151EKum(球料比20：1)
By introducing the structural transformation analysis into the kinetics of mechanochemical reaction and borrowing the structural macrokinetics research theory from the combustion synthesis, the structural macrokinetics of mechanochemical reaction and its research methods are put forward in this thesis. Based on the chemical reaction and material structure transformation, the mechanochemical processes were investigated and the research methods were applied successfully to the anatase TiO2, CaO+TiO2and Fe2O3+ZnO systems.
The main conclusions are as follows:
1. The shear force can promote the crystal transfer of anatase phase. By changing the action mode of mechanical force, the phase transformation of anatase can be expected to proceed along different courses, which is of practical reference value to synthesize TiO2ceramic material with the demands of crystal form. Results show that under our experimental conditions the anatase TiO2powder is demonstrated to induce different phase transformation phenomena with mechanical processing:a step-by-step transformation from anatase to TiO2-Ⅱ and then to rutile in all three mills:a planetary ball mill, an attritor and a ring-roller mill; besides a direct transformation from anatase to rutile in the ring-roller mill.
2. Under the same milling conditions, the mechanochemical reaction rates increased in turn when the alkaline-earth metal oxides MgO, CaO and BaO were milled with anatase, respectively, which indicates the existence of an alternation phenomenon along main group elements. Phase transformation might occur in anatase when it was milled with alkaline-earth metal oxides, which results in the different courses of reaction.
(1) In the system MgO+TiO2, it is hard to synthesize MgTiO3directly from the reaction of MgO with anatase TiO2. Experimental results show that the TiO2-Ⅱ, as a newborn phase with better reactivity than anatase TiO2, is firstly transformed from anatase TiO2with mechanical force, and MgTiO3can be formed through the reaction of MgO with the TiO2-Ⅱ.
There exist the chemical reactions in the system as follows: TiO2(Anatase)→TiO2-Ⅱ AO+TiO2-Ⅱ→ATiO3
(2) For the system CaO+TiO2and BaO+TiO2, TiO2-Ⅱ was not detected during the course of milling. And experimental results show that it is easy for anatase TiO2to directly react with CaO and BaO to form CaTiO3and BaTiO3, respectively. There exists the chemical reaction in the two systems as follows: AO+TiO2(Anatase)→ATiO3
3. Under the same milling conditions, the mechanochemical reaction rates increased in turn when the metallic oxides CuO, NiO and ZnO were milled with Fe2O3, respectively. Results show that with a similar structure between the reactant and the resultant, the reaction runs smoothly; otherwise, it runs relatively hard.
4. The mechanochemical kinetics of phase transformation to rutile in anatase system and reactions in both CaO+TiO2and Fe2O3+ZnO systems, are best expressed by Avrami-Erofe'ev model, which indicates the random nucleation of products phase followed by a growth of nuclei.
(1) The kinetic equation of anatase system is as:[-1n(1-α)]1/1.9147=0.2484t (Ring-roller mill,710rpm)
(2) The kinetic equation of CaO+TiO2system is as:[-ln(1-α)]1/08685=0.36581(Planetary ball mill,500rpm, BPR=20:1)
(3) The kinetic equation of Fe2O3+ZnO system is as:[-ln(1-α)]1/13262=0.0859/(Planetary ball mill,500rpm, BPR=20:1)
5. Taking the mechanochemical synthesis of ZnFe2O4by milling Fe2O3+ZnO mixed powders for example, the reaction kinetics was studied by energetic approach in this thesis. Results show that a fine effect could be obtained when Avrami-Erofe'ev kinetics model is used to fit the mechanochemical reaction. When it is under a certain BPR, the reaction conversion degree only directly relates to the energy dose. Energy-scaled knetics of mechanochemical reaction has less restriction on milling parameters than time-scaled kinetics.The kinetic equations under different BPR are as follows:
[-ln(1-α)]1/1.3179=0.0254Ekum(BPR=40:1)
[-ln(1-α)]1/13706=0.0151Ekum(BPR=20:1)
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