鋁硼硅系低介電常數(shù)玻璃纖維結(jié)構(gòu)及失透行為研究
發(fā)布時間：2018-08-27 13:52
【摘要】：當前我國電子信息產(chǎn)業(yè)的高速發(fā)展,對于通信設備提出了高速化、高頻化和小型化的需求。印制電路板和雷達天線罩等是信號傳輸工具關(guān)鍵部分,低介電常數(shù)玻璃纖維又是這些部分不可缺少的增強材料,有著十分重要地位。本文主要研究對象為鋁硼硅系低介電常數(shù)玻璃,其應用背景是低介電常數(shù)玻璃纖維拉絲生產(chǎn)中可能遇到的分相或析晶問題。固定玻璃中其他組分,分別改變各種二價氧化物和CaO的摩爾比,外摻不同量的TiO2,設kn(n=1、2、3、4)=(MO/(MO+CaO))(MO為MgO、SrO、BaO、ZnO)。使用(MAS)NMR、FTIR、DSC、梯溫析晶爐、XRD和SEM等測試手段,對鋁硼硅系低介電常數(shù)玻璃纖維結(jié)構(gòu)和失透行為做出了系統(tǒng)的研究,得出以下結(jié)論:隨著k1的增大,玻璃網(wǎng)絡結(jié)構(gòu)逐漸解聚,玻璃結(jié)構(gòu)中[BO4]、[AlO4]和含四個橋氧的[Si O4](Q4)相對含量減少,[BO3]逐漸增多;玻璃熱穩(wěn)定性隨之降低,失透溫度范圍和失透上線溫度都逐漸增大,其失透主要是由于分相引起的;k1較小時,玻璃分相形貌為蜂窩狀的連通相,其機理為為亞穩(wěn)分相,隨著成分和熱處理變化,富堿土金屬和富硼相集聚析出,形成直徑約為1μm的液滴相,穩(wěn)定分相。隨著k2的增大,玻璃結(jié)構(gòu)中[BO4]、[AlO4]和Q4含量略有增多,SrO對玻璃網(wǎng)絡結(jié)構(gòu)有一定的增強作用,但并不明顯。失透溫度范圍和失透上線溫度都隨之減小,甚至不失透,其失透主要是由于分相引起的。隨著k3增大,玻璃結(jié)構(gòu)更加穩(wěn)定,玻璃結(jié)構(gòu)中出現(xiàn)“硼反�！爆F(xiàn)象[BO4]含量先增多后減少,[AlO4]和Q4含量和橋氧數(shù)逐漸增多。BaO對玻璃網(wǎng)絡結(jié)構(gòu)有一定的增強作用,并且相對于SrO增強作用更大。失透溫度范圍和失透上線溫度都隨之減小,其失透主要是由于分相引起的。隨著k4增大,ZnO對玻璃網(wǎng)絡結(jié)構(gòu)破壞和解聚作用增大,玻璃結(jié)構(gòu)中[BO4]、[AlO4]和Q4相對含量減少,玻璃網(wǎng)絡中非橋氧增多,并且各結(jié)構(gòu)的變化相對于Mg組變化更大;其密度逐漸增大,失透溫度范圍和失透上線溫度都隨之增大。當ZnO含量較低和熱處理溫度較小時,失透主要是由于分相引起的。但隨著k4值的增大和熱處理溫度升高和保溫時間的延長,失透是由析晶引起的,主晶相為鋁氧化鋅(Al2ZnO4),次晶相為硼酸鋁(Al8B4O33)。TiO2有減弱玻璃結(jié)構(gòu),促進玻璃分相和析晶的作用。隨著外摻TiO2量增加,玻璃中各四面體結(jié)構(gòu)單元四配位硼[BO4]、四配位鋁[AlO4]和含有四個橋氧的[SiO4](Q4)逐漸減少,三配位硼[BO3]增多,玻璃結(jié)構(gòu)穩(wěn)定性減弱。其玻璃密度增大,其失透溫度范圍大大增加,其更加容易分相和析晶。析出主晶相是長約1μm的板條狀的金紅石型氧化鈦晶體,次晶相是呈顆粒狀的硼酸鋁(Al18B4O33)晶體。
[Abstract]:With the rapid development of electronic information industry in China, the demand of high speed, high frequency and miniaturization for communication equipment is put forward. Printed circuit board (PCB) and radar radome are the key parts of signal transmission tools. Low dielectric constant fiberglass is an indispensable reinforcement material in these parts, and has a very important position. The main research object of this paper is the low dielectric constant glass of aluminum-boron-silicon system. Its application background is the problem of phase separation or crystallization that may be encountered in the production of glass fiber with low dielectric constant. The molar ratios of various divalent oxides and CaO were changed respectively for the other components in the fixed glass. The TiO2, with different admixtures of kn (NX _ (1) O _ (2) O _ (3) O _ (4) = (MO/ (MO CaO) (MO = (MgO,SrO,BaO,ZnO) was used. The structure and devitrification behavior of glass fiber with low permittivity of Al-BB-Si system were systematically studied by means of (MAS) NMR,FTIR,DSC, and SEM. The following conclusions were drawn: with the increase of K1, the network structure of glass was gradually depolymerized. The relative contents of [BO4], [AlO4] and [Si O _ 4] (Q _ 4) in glass structure decrease, and [BO3] increase gradually. The morphology of glass phase is honeycomb, and its mechanism is metastable phase. With the change of composition and heat treatment, alkali rich earth metal and boron rich phase are precipitated, and liquid droplet phase with diameter about 1 渭 m is formed, and the phase separation is stabilized. With the increase of K2, the contents of [BO4], [AlO4] and Q4 in glass structure increase slightly. Both the range of the temperature and the temperature on the line of the loss decrease and even do not lose their transmittance, which is mainly caused by the separation of phases. With the increase of K3, the glass structure becomes more stable. The "boron anomaly" [BO4] content in the glass structure increases first and then decreases. The content of [AlO4] and Q4 and the number of bridge oxygen increase gradually. Bao has a certain enhancement effect on the glass network structure. And it is more effective than SrO. Both the range of the temperature and the temperature of the line are decreased, which is mainly caused by the phase separation. With the increase of k4, the destruction and depolymerization of glass network structure increases, the relative contents of [BO4], [AlO4] and Q4 in glass structure decrease, and the unbridged oxygen in glass network increases, and the change of each structure is larger than that of Mg group, and its density increases gradually. Both the temperature range and the line temperature increase. When the content of ZnO is low and the heat treatment temperature is small, the breakdown is mainly caused by phase separation. However, with the increase of K _ 4 value, heat treatment temperature and holding time, the breakdown is caused by crystallization. The main crystalline phase is Al2ZnO4, and the secondary phase is aluminum borate (Al8B4O33) .TiO _ 2 has the function of weakening glass structure and promoting glass phase separation and crystallization. With the increase of TiO2 content, tetrahedral boron [BO4], tetrahedral aluminum [AlO4] and [SiO4] (Q4) containing four bridged oxygen in glass gradually decrease, while tri-coordinated boron [BO3] increases, and the structural stability of glass decreases. With the increase of glass density, the temperature range of the glass is greatly increased, and it is easier to separate and crystallize. The main precipitated phase is a plate-shaped rutile titanium oxide crystal with a length of about 1 渭 m, while the secondary phase is a granular aluminum borate (Al18B4O33) crystal.
【學位授予單位】：重慶理工大學
【學位級別】：碩士
【學位授予年份】：2015
【分類號】：TQ171.771
本文編號：2207486
[Abstract]:With the rapid development of electronic information industry in China, the demand of high speed, high frequency and miniaturization for communication equipment is put forward. Printed circuit board (PCB) and radar radome are the key parts of signal transmission tools. Low dielectric constant fiberglass is an indispensable reinforcement material in these parts, and has a very important position. The main research object of this paper is the low dielectric constant glass of aluminum-boron-silicon system. Its application background is the problem of phase separation or crystallization that may be encountered in the production of glass fiber with low dielectric constant. The molar ratios of various divalent oxides and CaO were changed respectively for the other components in the fixed glass. The TiO2, with different admixtures of kn (NX _ (1) O _ (2) O _ (3) O _ (4) = (MO/ (MO CaO) (MO = (MgO,SrO,BaO,ZnO) was used. The structure and devitrification behavior of glass fiber with low permittivity of Al-BB-Si system were systematically studied by means of (MAS) NMR,FTIR,DSC, and SEM. The following conclusions were drawn: with the increase of K1, the network structure of glass was gradually depolymerized. The relative contents of [BO4], [AlO4] and [Si O _ 4] (Q _ 4) in glass structure decrease, and [BO3] increase gradually. The morphology of glass phase is honeycomb, and its mechanism is metastable phase. With the change of composition and heat treatment, alkali rich earth metal and boron rich phase are precipitated, and liquid droplet phase with diameter about 1 渭 m is formed, and the phase separation is stabilized. With the increase of K2, the contents of [BO4], [AlO4] and Q4 in glass structure increase slightly. Both the range of the temperature and the temperature on the line of the loss decrease and even do not lose their transmittance, which is mainly caused by the separation of phases. With the increase of K3, the glass structure becomes more stable. The "boron anomaly" [BO4] content in the glass structure increases first and then decreases. The content of [AlO4] and Q4 and the number of bridge oxygen increase gradually. Bao has a certain enhancement effect on the glass network structure. And it is more effective than SrO. Both the range of the temperature and the temperature of the line are decreased, which is mainly caused by the phase separation. With the increase of k4, the destruction and depolymerization of glass network structure increases, the relative contents of [BO4], [AlO4] and Q4 in glass structure decrease, and the unbridged oxygen in glass network increases, and the change of each structure is larger than that of Mg group, and its density increases gradually. Both the temperature range and the line temperature increase. When the content of ZnO is low and the heat treatment temperature is small, the breakdown is mainly caused by phase separation. However, with the increase of K _ 4 value, heat treatment temperature and holding time, the breakdown is caused by crystallization. The main crystalline phase is Al2ZnO4, and the secondary phase is aluminum borate (Al8B4O33) .TiO _ 2 has the function of weakening glass structure and promoting glass phase separation and crystallization. With the increase of TiO2 content, tetrahedral boron [BO4], tetrahedral aluminum [AlO4] and [SiO4] (Q4) containing four bridged oxygen in glass gradually decrease, while tri-coordinated boron [BO3] increases, and the structural stability of glass decreases. With the increase of glass density, the temperature range of the glass is greatly increased, and it is easier to separate and crystallize. The main precipitated phase is a plate-shaped rutile titanium oxide crystal with a length of about 1 渭 m, while the secondary phase is a granular aluminum borate (Al18B4O33) crystal.
【學位授予單位】：重慶理工大學
【學位級別】：碩士
【學位授予年份】：2015
【分類號】：TQ171.771
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，本文編號：2207486
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