硫酸鋇為內(nèi)核的金紅石型復(fù)合二氧化鈦制備研究
發(fā)布時(shí)間：2019-02-16 08:18
【摘要】：金紅石型Ti O2具有較高的介電常數(shù),常作為介電常數(shù)調(diào)節(jié)劑用于高頻微波基板材料的制備中,若直接使用微米級(jí)Ti O2將造成鈦資源的浪費(fèi)。本文以Ti Cl4為鈦源,以合成Ba SO4為內(nèi)核,采用加熱水解工藝在較低煅燒溫度下制備出Ba SO4/金紅石型Ti O2復(fù)合材料,實(shí)現(xiàn)了資源利用的最大化。該工藝具有原料價(jià)格便宜、流程簡單可控、生產(chǎn)能耗低等優(yōu)點(diǎn),為金紅石型復(fù)合Ti O2的工業(yè)化生產(chǎn)提供了理論與實(shí)踐依據(jù)。本文的主要內(nèi)容如下:(1)粒度分布窄的微米級(jí)近球形Ba SO4內(nèi)核的制備首先,以Ba Cl2為鋇源,選擇不同沉淀劑,分別采用直接沉淀法、均勻沉淀法和EDTA絡(luò)合沉淀法制備Ba SO4內(nèi)核,系統(tǒng)考察了反應(yīng)溫度、反應(yīng)物濃度、體系p H、加料速度、陳化時(shí)間對沉淀粒度、粒度分布以及形貌的影響,并對不同方法進(jìn)行優(yōu)化。SEM與粒度分析結(jié)果表明,只有直接沉淀法中的H2SO4路線與EDTA絡(luò)合沉淀法制得的Ba SO4顆�；痉匣逵脧�(fù)合Ti O2對內(nèi)核的要求,但前者所得Ba SO4存在粒度分布寬、較大顆粒形貌不規(guī)則等不足。相比之下,EDTA絡(luò)合沉淀法能同時(shí)實(shí)現(xiàn)對沉淀粒度以及形貌的有效控制,最優(yōu)工藝條件為:室溫(25 oC)下,絡(luò)合體系p H為8,Ba Cl度為0.20 mol/L,絡(luò)合比為1,Na2SO4濃度為0.25 mol/L,Na2SO4加料速度為5 m L/min,反應(yīng)時(shí)間1 h。在該反應(yīng)條件下,無需陳化,即可得到粒度分布均勻的球形Ba SO4,平均粒度為1.2μm。然后,比較了直接沉淀法與EDTA絡(luò)合沉淀法所得Ba SO4內(nèi)核在相同包覆工藝下的Ti O2包覆效果,結(jié)果表明,EDTA絡(luò)合沉淀法制得的Ba SO4更利于Ti O2包覆,是復(fù)合Ti O2內(nèi)核的最佳選擇。(2)金紅石型復(fù)合Ti O2的制備首先探究水解體系初始p H、水解溫度、硫酸根離子和煅燒溫度對單一Ti O2顆粒晶型的影響,確定出Ti Cl4加熱水解法制備金紅石型Ti O2的工藝;然后在上述工藝的基礎(chǔ)上,以最優(yōu)條件下EDTA絡(luò)合沉淀法制得的Ba SO4為內(nèi)核,進(jìn)一步考察水解時(shí)間、水解溫度、Ti Cl4用量、水解混合液中鈦濃度對包覆效果的影響。最終,確定了加熱水解法制備Ba SO4/金紅石型Ti O2復(fù)合粉體的最優(yōu)工藝條件:水解體系初始p H為0.1,水解混合液中鈦濃度為0.20 mol/L,Ti Cl4用量n(Ti Cl4):n(Ba SO4)為2,水解溫度80 oC,水解時(shí)間1.5 h,煅燒溫度500 oC,煅燒時(shí)間2 h。在該工藝條件下,復(fù)合Ti O有金紅石型包覆層,且包覆率高,包覆層均勻致密,此外還具有球形形貌良好、分散性佳等優(yōu)點(diǎn)。
[Abstract]:Rutile Ti O2 has a high dielectric constant. It is often used as a dielectric constant regulator in the preparation of high frequency microwave substrate materials. The direct use of micron Ti O2 will lead to a waste of titanium resources. In this paper, Ba SO4/ rutile Ti O 2 composites were prepared by using Ti Cl4 as titanium source and Ba SO4 as core. Ba SO4/ rutile type Ti O 2 composites were prepared under low calcination temperature by means of heating hydrolysis process, thus maximizing the utilization of resources. The process has the advantages of cheap raw material price, simple and controllable process and low energy consumption. It provides a theoretical and practical basis for the industrial production of rutile composite Ti O2. The main contents of this paper are as follows: (1) the preparation of micrometer near-spherical Ba SO4 core with narrow particle size distribution. Firstly, the direct precipitation method was used to select different precipitators with Ba Cl2 as the source of barium. The Ba SO4 core was prepared by homogeneous precipitation method and EDTA complex precipitation method. The effects of reaction temperature, reactant concentration, system pH, feeding rate, aging time on the particle size, particle size distribution and morphology of Ba SO4 were investigated. The results of SEM and particle size analysis show that only the Ba SO4 particles prepared by H2SO4 route and EDTA complexation precipitation method basically meet the requirements of the core of composite Ti O2 for substrate. However, the Ba SO4 obtained from the former has some shortcomings, such as wide particle size distribution and irregular morphology of larger particles. In contrast, the EDTA complex precipitation method can effectively control the particle size and morphology of the precipitate at the same time. The optimum conditions are as follows: at room temperature (25 oC), the complex system p H = 8o Ba Cl degree is 0.20 mol/L, complex ratio, and the optimum process conditions are as follows: at room temperature (25 oC), the complexation ratio of pH to Ba is 0.20 mol/L,. The concentration of Na2SO4 is 0.25 mol/L,Na2SO4, the feeding rate is 5 mL / min, the reaction time is 1 h. Under this reaction condition, the average particle size of spherical Ba SO4, with uniform particle size distribution is 1.2 渭 m without aging. Then, the Ti O 2 coating effect of Ba SO4 core obtained by direct precipitation method and EDTA complexation precipitation method was compared. The results showed that the Ba SO4 prepared by EDTA complex precipitation method was more favorable to Ti O 2 coating. (2) the preparation of rutile composite Ti O _ 2 first investigated the effects of initial pH, hydrolysis temperature, sulfate ion and calcination temperature on the crystal morphology of single Ti O _ 2 particles. The process of preparing rutile Ti O 2 by Ti Cl4 heating hydrolysis was determined. On the basis of the above technology, the effects of hydrolysis time, hydrolysis temperature, amount of Ti Cl4 and concentration of titanium in hydrolysis mixture on the coating effect of Ba SO4 prepared by EDTA complexation precipitation under the optimum conditions were further investigated. Finally, the optimum conditions of preparing Ba SO4/ rutile Ti O 2 composite powder by heating hydrolysis method were determined: the initial pH of hydrolysis system was 0.1, and the concentration of titanium in hydrolysis mixture was 0.20 mol/L,. The amount of Ti Cl4 was 2, the hydrolysis temperature was 80 oC, the hydrolysis time was 1.5 h, the calcination temperature was 500 oC, the calcination time was 2 h. Under this condition, the composite Ti O has rutile coating with high coating efficiency, uniform and dense coating layer, good spherical morphology and good dispersion.
【學(xué)位授予單位】：江南大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TQ134.11
本文編號(hào)：2424241
[Abstract]:Rutile Ti O2 has a high dielectric constant. It is often used as a dielectric constant regulator in the preparation of high frequency microwave substrate materials. The direct use of micron Ti O2 will lead to a waste of titanium resources. In this paper, Ba SO4/ rutile Ti O 2 composites were prepared by using Ti Cl4 as titanium source and Ba SO4 as core. Ba SO4/ rutile type Ti O 2 composites were prepared under low calcination temperature by means of heating hydrolysis process, thus maximizing the utilization of resources. The process has the advantages of cheap raw material price, simple and controllable process and low energy consumption. It provides a theoretical and practical basis for the industrial production of rutile composite Ti O2. The main contents of this paper are as follows: (1) the preparation of micrometer near-spherical Ba SO4 core with narrow particle size distribution. Firstly, the direct precipitation method was used to select different precipitators with Ba Cl2 as the source of barium. The Ba SO4 core was prepared by homogeneous precipitation method and EDTA complex precipitation method. The effects of reaction temperature, reactant concentration, system pH, feeding rate, aging time on the particle size, particle size distribution and morphology of Ba SO4 were investigated. The results of SEM and particle size analysis show that only the Ba SO4 particles prepared by H2SO4 route and EDTA complexation precipitation method basically meet the requirements of the core of composite Ti O2 for substrate. However, the Ba SO4 obtained from the former has some shortcomings, such as wide particle size distribution and irregular morphology of larger particles. In contrast, the EDTA complex precipitation method can effectively control the particle size and morphology of the precipitate at the same time. The optimum conditions are as follows: at room temperature (25 oC), the complex system p H = 8o Ba Cl degree is 0.20 mol/L, complex ratio, and the optimum process conditions are as follows: at room temperature (25 oC), the complexation ratio of pH to Ba is 0.20 mol/L,. The concentration of Na2SO4 is 0.25 mol/L,Na2SO4, the feeding rate is 5 mL / min, the reaction time is 1 h. Under this reaction condition, the average particle size of spherical Ba SO4, with uniform particle size distribution is 1.2 渭 m without aging. Then, the Ti O 2 coating effect of Ba SO4 core obtained by direct precipitation method and EDTA complexation precipitation method was compared. The results showed that the Ba SO4 prepared by EDTA complex precipitation method was more favorable to Ti O 2 coating. (2) the preparation of rutile composite Ti O _ 2 first investigated the effects of initial pH, hydrolysis temperature, sulfate ion and calcination temperature on the crystal morphology of single Ti O _ 2 particles. The process of preparing rutile Ti O 2 by Ti Cl4 heating hydrolysis was determined. On the basis of the above technology, the effects of hydrolysis time, hydrolysis temperature, amount of Ti Cl4 and concentration of titanium in hydrolysis mixture on the coating effect of Ba SO4 prepared by EDTA complexation precipitation under the optimum conditions were further investigated. Finally, the optimum conditions of preparing Ba SO4/ rutile Ti O 2 composite powder by heating hydrolysis method were determined: the initial pH of hydrolysis system was 0.1, and the concentration of titanium in hydrolysis mixture was 0.20 mol/L,. The amount of Ti Cl4 was 2, the hydrolysis temperature was 80 oC, the hydrolysis time was 1.5 h, the calcination temperature was 500 oC, the calcination time was 2 h. Under this condition, the composite Ti O has rutile coating with high coating efficiency, uniform and dense coating layer, good spherical morphology and good dispersion.
【學(xué)位授予單位】：江南大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TQ134.11
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