先驱体转化法制备氮化硼纤维研究
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摘要
随着新型高马赫数导弹天线罩对材料防热、承载和透波性能的要求不断提高,现有的透波纤维增强陶瓷基复合材料已经成为天线罩技术发展的瓶颈。氮化硼(BN)纤维具有工作温度高、高温烧蚀率低、工作性能稳定、介电常数和节电损耗小等优点,是新型陶瓷基透波复合材料增强体的理想候选材料。在此背景下,本文开展了聚合物先驱体转化法制备BN纤维的基础研究。
在温和条件下分别以共取代和分步取代法合成了三种不同结构、可溶可熔的聚硼氮烷先驱体,合成过程均不需极低温度,简化了操作,降低了成本。分别采用NMR、FTIR、XPS、TGA和元素分析等手段对三种先驱体进行了表征。
由三氯化硼和甲胺合成了PTMB,PTMB的分子中含有B3N3六元环、C-H、B-N、N-H和C-N等化学键;PTMB可溶于甲苯和二甲苯等溶剂,典型的PTMB的元素组成为(wt%):B(24.5), C(32.8), N(29.9)和H(10.2),其化学式可表示为BC1.20N0.94H4.5。在NH3中的处理可以提高PTMB的陶瓷产率,在NH3中的无机化可以除去碳元素;失重主要发生在600℃以下,900℃基本完成无机化;PTMB的分子结构和较低的陶瓷产率不适宜用于制备BN纤维,但可能用作制备其它BN材料;经1600℃处理的产物为t-BN,该BN在空气中900℃时的失重小于3.0wt%,表现出了较好的抗氧化性能。
由三氯环硼氮烷和异丙胺合成的PTPiAB具有一定的熔融加工性能,PTPiAB的分子中含有B3N3六元环、C-H键、B-N键、N-H键和C-N键等特征结构;PTPiAB可溶于甲苯、二甲苯等常见有机溶剂;典型的PTPiAB的化学组成为(wt%):B (12.4)、N(35.8)、C(37.2)、H(9.3),其化学式可表示为BC2.7N2.2H8.1。1000℃时,PTPiAB在NH3中的陶瓷产率低于在Ar中的陶瓷产率;在NH3中的失重主要发生在800℃以下,800℃先驱体中的有机基团基本消失,接近无机化;NH3的除碳效果明显,600℃时已有94.0wt%的碳被除去;1400℃以上为晶粒长大的主要区间,1800℃热解产物的(002)晶面间距为0.334nm,密度为2.03g·cm-3,在空气中900℃以下的增重小于0.3wt%,抗氧化性能随结晶程度的增加而增强。
由正丙胺/甲胺和三氯环硼氮烷合成了PPAB。通过调控原料的比例,控制合成温度和时间等参数,能得到可以熔融的PPAB先驱体,软化点随聚合反应温度的增加和保温时间的延长而升高;优化的合成工艺参数为n-PA?MA?TCB=2?1?1(摩尔比),聚合温度为150~170℃,保温时间为5~7h,所合成PPAB的软化点为90~100℃;典型的PPAB含有B、N、C和H元素,元素组成为(wt%):B(22.28)、C(23.24)、N(44.75)、H(7.78),其化学式可近似表示为BC0.94N1.55H3.75;PPAB分子中含有N-H、C-H、B-N和C-N等化学键,B3N3六元环通过-B-(NCH3)-B-连接;典型PPAB的数均分子量为1002(相对于聚苯乙烯标样),重均分子量为1359,分散系数为1.50,可溶于甲苯和二甲苯等溶剂,在Ar中1000℃的陶瓷产率约为50wt%。
对三种先驱体进行的熔融挑丝实验表明,PPAB具有更好的成丝性,更适合用于制备BN纤维。PTMB和PTPiAB可用于制备其它形式的BN材料。
对PPAB在空气中的稳定性研究表明,PPAB在空气中极易水解,水解程度随温度、湿度和时间的增加而增大;PPAB对少量的O2不敏感,水解主要是由于H2O引起的;PPAB的水解引入了大量氧元素,生成B-O键,形成不溶不熔的三维网状结构,不能熔融加工;水解的PPAB在Ar中的主要热解产物为BN和B2O3。比较了以PTPiAB和PPAB两种不同分子结构先驱体所制备BN的异同,结果表明:得到的BN均具有近化学计量比,不含碳杂质,具有类似的组成和结构;两种BN的结晶程度不同,具有对称结构的分子单体TPiAB得到的BN结晶程度更高,氧化性能优于由非对称结构单体PAB得到的BN。
考察了PPAB的软化点、纺丝温度和纺丝压力等工艺参数对熔融纺丝的影响,当软化点在93~112℃,纺丝温度高于软化点20~70℃,纺丝压力为0.4~0.6MPa,可以得到连续长度大于200m的PPAB纤维。
PPAB纤维在NH3中的不熔化过程伴随着凝胶含量变化、失重和碳含量下降,碳含量的下降主要由烷基基团的脱去引起,C-N键未参与反应;合适的不熔化工艺为,以0.5℃/min的升温速率升温至70~80℃并保温80min,由此得到的PPAB不熔化纤维的凝胶含量大于90wt%。
PPAB在N2中热解得到含碳的BN,而在NH3中热解会脱除碳元素,得到近化学计量比的BN;在N2中的陶瓷产率高于NH3中陶瓷产率,NH3中的热解产物具有更好的结晶性能、抗氧化性能和介电性能。
采用NH3作为热解气氛,考察了温度、NH3浓度、保温时间和升温速率等参数对PPAB不熔化纤维无机化过程的影响和无机化纤维组成、结构的影响,结果表明:在800℃基本完成无机化,在NH3/N2=1:1(vol)的混合气氛中即可实现脱碳。较优的无机化工艺为:在NH3浓度为50vol%的NH3/N2热解气氛中,以4℃/min的升温速率升至800℃并保温2h,由此得到的无机纤维碳含量小于0.5wt%。
对无机化纤维进行高温处理有利于获得性能更优异的BN纤维,研究了处理温度对纤维结晶性能、密度、力学性能以及抗氧化性能的影响规律。结果表明:1200℃以下是纤维密实性增加的主要阶段, 1800℃得到BN纤维具有较好的抗氧化性,密度为1.92g·cm-3,(002)晶面间距和晶粒尺寸分别为0.337nm和6.50nm,拉伸强度为850MPa,在频率为10GHz处的介电常数为3左右、损耗角正切为10-3量级。
With increasing of the ultra-high speed missle radomes’demand for materials with high heat resistance, load bearing and wave transparence, the existing wave transparent fibers reinforced ceramic matrix composites have been a major bottleneck regarding the development of technology for radome. Nitride ceramic fibers, possessing high temperature resistance, good ablation performance and excellent stability, are one of novel intensifiers for wave transparent ceramic matrix composites. Hence, the major objective of the present work is dealt with the basic research on the preparation and characterization of boron nitride (BN) fibers via the polymer-derived ceramics (PDCs) method.
According to the requirement of polymeric precursor’s structure for BN fibers, three soluble and fusible polyborazines were synthesized. These low cost synthetic routes were under mild conditions without extremely low temperature, facilitating the manipulation. These preceramic polymers were characterized by NMR、FTIR、XPS、TGA and elemental analysis.
PTMB synthesized from boron trichloride and methylamine (MA) was composed of B3N3 hexagons, C-H, B-N, N-H and C-N bonds. PTMB was soluble in toluene and oxylene. The typical composition of PTMB was (wt%):B(24.5), C(32.8), N(29.9) and H(10.2) with a chemical formula of BC1.20N0.94H4.5。
The ceramic yield of PTMB was improved by treating under NH3. The carbon in PTMB was removed by pyrolysis in NH3. The major weight loss occurred below 600℃and the transition from organics to mineral basically happened at 900℃. The molecular structure and low ceramic yield of PTMB were not suitable for the preparation of BN fibers, while hopefully, for other forms of BN. Turbostratic BN (t-BN) was obtained by pyrolysis PTMB in NH3 and then in Ar. The t-BN showed a weight loss of less than 3.0wt% at 900℃in air, exhibiting its good oxidation resistance.
PTPiAB synthesized from 2,4,6-trichloroborazine (TCB) and iso-propylamine showed a higher ceramic yield in Ar than that in NH3. PTPiAB was composed of B3N3 hexagons, C-H, B-N, N-H and C-N bonds. PTPiAB was soluble in toluene and oxylene. The typical composition of PTPiAB was (wt%): B(12.4), N(35.8), C(37.2), H(9.3) with a chemical formula of BC2.7N2.2H8.1。
The weight loss in NH3 mainly occurred under 800℃and the organic groups in PTPiAB almost disappeared at 800℃. The removal of carbon in NH3 was evident and 94.0 weight percent of carbon was removed at 600℃. The range for the crystallization was mainly below 1400℃. The sample acquired by pyrolysis of PTPiAB in NH3 at 1000 ℃and then in Ar at 1800℃showed the (002) interlayer spacing of 0.334nm, with a density of 2.03g·cm-3. At 900℃, the weight loss of the sample obtained at 1800℃was less than 0.3wt% in air and the oxidation resistance was improved with the increase of crystallization.
PPAB was synthesized from n-propylamine (n-PA), MA and TCB. Through controlling the ratio of raw materials, temperature and holding time, the soluble and fusible PPAB can be synthesized. The softening point of PPAB was heightened by the increase of temperature and holding time. The appropriate condition for the synthesis of PPAB was: n-PA?MA?TCB=2?1?1 (molar ratio), 150~170℃(polymerization temperature), 5~7h (holding time). The softening point of the as-synthesized PPAB was 90~100℃. PPAB was composed of N-H、C-H、B-N and C-N bonds, accompanied by the B3N3 hexagons linked with -B-(NCH3)-B- groups. The typical composition of PPAB was (wt%): B (22.28), C(23.24), N(44.75) and H(7.78) with a chemical formula of BC0.94N1.55H3.75.
The number average molecular weight of typical PPAB was 1002 (relative to PS standards) and the weight number average molecular weight was 1359 with a polydispersity index of 1.50. The PPAB was soluble in toluene and oxylene with a ceramic yield of 50wt% at 1000℃in Ar.
The melt spinning test for three polymeric precursors showed that PPAB possessed best spinnability, adapting to the preparation of BN fibers. Besides, PTMB and PTPiAB could be used to fabricate porous BN and BN coatings.
The research on the PPAB’s stability in air showed: PPAB hydrolyzed in air easily and the hydrolyzation occurred badly with the increase of humidity, temperature and holding time. PPAB was insensitive to O2 in air and the hydrolyzation of PPAB in air was mainly due to H2O. Oxygen came into PPAB during the hydrolyzation process to engender B-O bonds, helping to the formation of insoluble and infusible structure of three-dimensional reticulation. The hydrolyzed PPAB could not be melt processed and the pyrolyzed sample in Ar was mainly BN and B2O3.
The composition, structure and properties of BN derived from PTPiAB and PPAB were compared and the results showed that the two BN samples without carbon impurity both possessed nearly stoichiometric composition. BN derived from PTPiAB had a higher crystallinity and exhibited better oxidation resistance. This is due to that the structure of symmetric molecular derived polymeric precursor is close to that of hexagonal BN.
The influence of softening point, spinning temperature and spinning pressure in the melt spinning process was studied. The optimum spinning condition was found to be the softening point of 93~112℃, the spinning temperature of 20~70℃higher than softening point and the spinning pressure of 0.4~0.6MPa. The corresponding PPAB fibers with a length of longer than 200m could be obtained.
The curing process of PPAB fibers in NH3 was accompanied by the increase of gel content, weight loss and decrease of carbon content. The drop of carbon content in cured fibers was mainly due to removal of alkyl-units during curing, whereas independent of C-N bonds. The optimum curing condition was found to be the heating rate of 0.5℃/min, the temperature of 70~80℃and the holding time of 80min. The gel content of corresponding cured fibers was more than 90wt%.
Pyrolysis of PPAB in N2 resulted in BN with carbon contaminant, whereas in NH3 led to the removal of carbon and obtainment of BN with nearly stoichiometric composition. The ceramic yield of PPAB in N2 was higher than that in NH3. The products acquired in NH3 possessed better crystallization, oxidation resistance and dielectric property than those in N2.
The influence of temperature, NH3 concentration, holding time and heating rate during inorganic transition of cured PPAB fibers was researched. The result showed the inorganic transition of cured fibers was almost completed at 800℃. The removal of carbon could be accomplished in the mixed atmosphere of NH3/N2=1:1(vol). The optimum inorganic condition was found to be the NH3 concentration of 50vol%, the heating rate of 4℃/min, the temperature of 800℃and the holding time of 2h. The carbon content in the corresponding fibers was less than 0.5wt%.
The high temperature treatment of inorganic fibers favored BN fibers’better properties. The influence of temperature in the crystallinity, density, tensile strength and oxidation resistance was studied. The results showed the density of BN fibers increased mainly from 600℃to 1200℃and that of BN fibers prepared by pyrolysis of cured PPAB fibers in NH3 at 800℃and then in Ar at 1800℃was 1.92g·cm-3. For the BN fibers obtained at 1800℃, the (002) interlayer spacing and the crystalline size were 0.337nm and 6.50nm, respectively. The BN fibers with a tensile strength of 850MPa showed a good oxidation resistance. Besides, the BN fibers possessed a dielectric constant of 3 and a dielectric loss of 10-3 at 10GHz.
在温和条件下分别以共取代和分步取代法合成了三种不同结构、可溶可熔的聚硼氮烷先驱体,合成过程均不需极低温度,简化了操作,降低了成本。分别采用NMR、FTIR、XPS、TGA和元素分析等手段对三种先驱体进行了表征。
由三氯化硼和甲胺合成了PTMB,PTMB的分子中含有B3N3六元环、C-H、B-N、N-H和C-N等化学键;PTMB可溶于甲苯和二甲苯等溶剂,典型的PTMB的元素组成为(wt%):B(24.5), C(32.8), N(29.9)和H(10.2),其化学式可表示为BC1.20N0.94H4.5。在NH3中的处理可以提高PTMB的陶瓷产率,在NH3中的无机化可以除去碳元素;失重主要发生在600℃以下,900℃基本完成无机化;PTMB的分子结构和较低的陶瓷产率不适宜用于制备BN纤维,但可能用作制备其它BN材料;经1600℃处理的产物为t-BN,该BN在空气中900℃时的失重小于3.0wt%,表现出了较好的抗氧化性能。
由三氯环硼氮烷和异丙胺合成的PTPiAB具有一定的熔融加工性能,PTPiAB的分子中含有B3N3六元环、C-H键、B-N键、N-H键和C-N键等特征结构;PTPiAB可溶于甲苯、二甲苯等常见有机溶剂;典型的PTPiAB的化学组成为(wt%):B (12.4)、N(35.8)、C(37.2)、H(9.3),其化学式可表示为BC2.7N2.2H8.1。1000℃时,PTPiAB在NH3中的陶瓷产率低于在Ar中的陶瓷产率;在NH3中的失重主要发生在800℃以下,800℃先驱体中的有机基团基本消失,接近无机化;NH3的除碳效果明显,600℃时已有94.0wt%的碳被除去;1400℃以上为晶粒长大的主要区间,1800℃热解产物的(002)晶面间距为0.334nm,密度为2.03g·cm-3,在空气中900℃以下的增重小于0.3wt%,抗氧化性能随结晶程度的增加而增强。
由正丙胺/甲胺和三氯环硼氮烷合成了PPAB。通过调控原料的比例,控制合成温度和时间等参数,能得到可以熔融的PPAB先驱体,软化点随聚合反应温度的增加和保温时间的延长而升高;优化的合成工艺参数为n-PA?MA?TCB=2?1?1(摩尔比),聚合温度为150~170℃,保温时间为5~7h,所合成PPAB的软化点为90~100℃;典型的PPAB含有B、N、C和H元素,元素组成为(wt%):B(22.28)、C(23.24)、N(44.75)、H(7.78),其化学式可近似表示为BC0.94N1.55H3.75;PPAB分子中含有N-H、C-H、B-N和C-N等化学键,B3N3六元环通过-B-(NCH3)-B-连接;典型PPAB的数均分子量为1002(相对于聚苯乙烯标样),重均分子量为1359,分散系数为1.50,可溶于甲苯和二甲苯等溶剂,在Ar中1000℃的陶瓷产率约为50wt%。
对三种先驱体进行的熔融挑丝实验表明,PPAB具有更好的成丝性,更适合用于制备BN纤维。PTMB和PTPiAB可用于制备其它形式的BN材料。
对PPAB在空气中的稳定性研究表明,PPAB在空气中极易水解,水解程度随温度、湿度和时间的增加而增大;PPAB对少量的O2不敏感,水解主要是由于H2O引起的;PPAB的水解引入了大量氧元素,生成B-O键,形成不溶不熔的三维网状结构,不能熔融加工;水解的PPAB在Ar中的主要热解产物为BN和B2O3。比较了以PTPiAB和PPAB两种不同分子结构先驱体所制备BN的异同,结果表明:得到的BN均具有近化学计量比,不含碳杂质,具有类似的组成和结构;两种BN的结晶程度不同,具有对称结构的分子单体TPiAB得到的BN结晶程度更高,氧化性能优于由非对称结构单体PAB得到的BN。
考察了PPAB的软化点、纺丝温度和纺丝压力等工艺参数对熔融纺丝的影响,当软化点在93~112℃,纺丝温度高于软化点20~70℃,纺丝压力为0.4~0.6MPa,可以得到连续长度大于200m的PPAB纤维。
PPAB纤维在NH3中的不熔化过程伴随着凝胶含量变化、失重和碳含量下降,碳含量的下降主要由烷基基团的脱去引起,C-N键未参与反应;合适的不熔化工艺为,以0.5℃/min的升温速率升温至70~80℃并保温80min,由此得到的PPAB不熔化纤维的凝胶含量大于90wt%。
PPAB在N2中热解得到含碳的BN,而在NH3中热解会脱除碳元素,得到近化学计量比的BN;在N2中的陶瓷产率高于NH3中陶瓷产率,NH3中的热解产物具有更好的结晶性能、抗氧化性能和介电性能。
采用NH3作为热解气氛,考察了温度、NH3浓度、保温时间和升温速率等参数对PPAB不熔化纤维无机化过程的影响和无机化纤维组成、结构的影响,结果表明:在800℃基本完成无机化,在NH3/N2=1:1(vol)的混合气氛中即可实现脱碳。较优的无机化工艺为:在NH3浓度为50vol%的NH3/N2热解气氛中,以4℃/min的升温速率升至800℃并保温2h,由此得到的无机纤维碳含量小于0.5wt%。
对无机化纤维进行高温处理有利于获得性能更优异的BN纤维,研究了处理温度对纤维结晶性能、密度、力学性能以及抗氧化性能的影响规律。结果表明:1200℃以下是纤维密实性增加的主要阶段, 1800℃得到BN纤维具有较好的抗氧化性,密度为1.92g·cm-3,(002)晶面间距和晶粒尺寸分别为0.337nm和6.50nm,拉伸强度为850MPa,在频率为10GHz处的介电常数为3左右、损耗角正切为10-3量级。
With increasing of the ultra-high speed missle radomes’demand for materials with high heat resistance, load bearing and wave transparence, the existing wave transparent fibers reinforced ceramic matrix composites have been a major bottleneck regarding the development of technology for radome. Nitride ceramic fibers, possessing high temperature resistance, good ablation performance and excellent stability, are one of novel intensifiers for wave transparent ceramic matrix composites. Hence, the major objective of the present work is dealt with the basic research on the preparation and characterization of boron nitride (BN) fibers via the polymer-derived ceramics (PDCs) method.
According to the requirement of polymeric precursor’s structure for BN fibers, three soluble and fusible polyborazines were synthesized. These low cost synthetic routes were under mild conditions without extremely low temperature, facilitating the manipulation. These preceramic polymers were characterized by NMR、FTIR、XPS、TGA and elemental analysis.
PTMB synthesized from boron trichloride and methylamine (MA) was composed of B3N3 hexagons, C-H, B-N, N-H and C-N bonds. PTMB was soluble in toluene and oxylene. The typical composition of PTMB was (wt%):B(24.5), C(32.8), N(29.9) and H(10.2) with a chemical formula of BC1.20N0.94H4.5。
The ceramic yield of PTMB was improved by treating under NH3. The carbon in PTMB was removed by pyrolysis in NH3. The major weight loss occurred below 600℃and the transition from organics to mineral basically happened at 900℃. The molecular structure and low ceramic yield of PTMB were not suitable for the preparation of BN fibers, while hopefully, for other forms of BN. Turbostratic BN (t-BN) was obtained by pyrolysis PTMB in NH3 and then in Ar. The t-BN showed a weight loss of less than 3.0wt% at 900℃in air, exhibiting its good oxidation resistance.
PTPiAB synthesized from 2,4,6-trichloroborazine (TCB) and iso-propylamine showed a higher ceramic yield in Ar than that in NH3. PTPiAB was composed of B3N3 hexagons, C-H, B-N, N-H and C-N bonds. PTPiAB was soluble in toluene and oxylene. The typical composition of PTPiAB was (wt%): B(12.4), N(35.8), C(37.2), H(9.3) with a chemical formula of BC2.7N2.2H8.1。
The weight loss in NH3 mainly occurred under 800℃and the organic groups in PTPiAB almost disappeared at 800℃. The removal of carbon in NH3 was evident and 94.0 weight percent of carbon was removed at 600℃. The range for the crystallization was mainly below 1400℃. The sample acquired by pyrolysis of PTPiAB in NH3 at 1000 ℃and then in Ar at 1800℃showed the (002) interlayer spacing of 0.334nm, with a density of 2.03g·cm-3. At 900℃, the weight loss of the sample obtained at 1800℃was less than 0.3wt% in air and the oxidation resistance was improved with the increase of crystallization.
PPAB was synthesized from n-propylamine (n-PA), MA and TCB. Through controlling the ratio of raw materials, temperature and holding time, the soluble and fusible PPAB can be synthesized. The softening point of PPAB was heightened by the increase of temperature and holding time. The appropriate condition for the synthesis of PPAB was: n-PA?MA?TCB=2?1?1 (molar ratio), 150~170℃(polymerization temperature), 5~7h (holding time). The softening point of the as-synthesized PPAB was 90~100℃. PPAB was composed of N-H、C-H、B-N and C-N bonds, accompanied by the B3N3 hexagons linked with -B-(NCH3)-B- groups. The typical composition of PPAB was (wt%): B (22.28), C(23.24), N(44.75) and H(7.78) with a chemical formula of BC0.94N1.55H3.75.
The number average molecular weight of typical PPAB was 1002 (relative to PS standards) and the weight number average molecular weight was 1359 with a polydispersity index of 1.50. The PPAB was soluble in toluene and oxylene with a ceramic yield of 50wt% at 1000℃in Ar.
The melt spinning test for three polymeric precursors showed that PPAB possessed best spinnability, adapting to the preparation of BN fibers. Besides, PTMB and PTPiAB could be used to fabricate porous BN and BN coatings.
The research on the PPAB’s stability in air showed: PPAB hydrolyzed in air easily and the hydrolyzation occurred badly with the increase of humidity, temperature and holding time. PPAB was insensitive to O2 in air and the hydrolyzation of PPAB in air was mainly due to H2O. Oxygen came into PPAB during the hydrolyzation process to engender B-O bonds, helping to the formation of insoluble and infusible structure of three-dimensional reticulation. The hydrolyzed PPAB could not be melt processed and the pyrolyzed sample in Ar was mainly BN and B2O3.
The composition, structure and properties of BN derived from PTPiAB and PPAB were compared and the results showed that the two BN samples without carbon impurity both possessed nearly stoichiometric composition. BN derived from PTPiAB had a higher crystallinity and exhibited better oxidation resistance. This is due to that the structure of symmetric molecular derived polymeric precursor is close to that of hexagonal BN.
The influence of softening point, spinning temperature and spinning pressure in the melt spinning process was studied. The optimum spinning condition was found to be the softening point of 93~112℃, the spinning temperature of 20~70℃higher than softening point and the spinning pressure of 0.4~0.6MPa. The corresponding PPAB fibers with a length of longer than 200m could be obtained.
The curing process of PPAB fibers in NH3 was accompanied by the increase of gel content, weight loss and decrease of carbon content. The drop of carbon content in cured fibers was mainly due to removal of alkyl-units during curing, whereas independent of C-N bonds. The optimum curing condition was found to be the heating rate of 0.5℃/min, the temperature of 70~80℃and the holding time of 80min. The gel content of corresponding cured fibers was more than 90wt%.
Pyrolysis of PPAB in N2 resulted in BN with carbon contaminant, whereas in NH3 led to the removal of carbon and obtainment of BN with nearly stoichiometric composition. The ceramic yield of PPAB in N2 was higher than that in NH3. The products acquired in NH3 possessed better crystallization, oxidation resistance and dielectric property than those in N2.
The influence of temperature, NH3 concentration, holding time and heating rate during inorganic transition of cured PPAB fibers was researched. The result showed the inorganic transition of cured fibers was almost completed at 800℃. The removal of carbon could be accomplished in the mixed atmosphere of NH3/N2=1:1(vol). The optimum inorganic condition was found to be the NH3 concentration of 50vol%, the heating rate of 4℃/min, the temperature of 800℃and the holding time of 2h. The carbon content in the corresponding fibers was less than 0.5wt%.
The high temperature treatment of inorganic fibers favored BN fibers’better properties. The influence of temperature in the crystallinity, density, tensile strength and oxidation resistance was studied. The results showed the density of BN fibers increased mainly from 600℃to 1200℃and that of BN fibers prepared by pyrolysis of cured PPAB fibers in NH3 at 800℃and then in Ar at 1800℃was 1.92g·cm-3. For the BN fibers obtained at 1800℃, the (002) interlayer spacing and the crystalline size were 0.337nm and 6.50nm, respectively. The BN fibers with a tensile strength of 850MPa showed a good oxidation resistance. Besides, the BN fibers possessed a dielectric constant of 3 and a dielectric loss of 10-3 at 10GHz.
引文
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