KNN和BT高性能无铅压电陶瓷的制备技术及机理研究
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摘要
本文研究了(K,Na)NbO3基无铅压电陶瓷材料烧结温度区间窄的机理,通过两段式烧结和采用纳米粉体低温烧结成功解决这一难题。以纳米粉体为原料,成功制备出(K,Na)NbO3基细晶无铅压电陶瓷,解决了该类陶瓷的细晶化难题。此外,本文还探讨了BaTiO3陶瓷压电性能大幅提高的机理,成功制备出高性能BaTiO3无铅压电陶瓷。
KNbO3-NaNbO3相图的分析表明,(K, Na)NbO3基陶瓷在烧结过程中易发生分凝现象,从而产生液相并出现成分的分凝。液相的出现会导致(K,Na)NbO3基陶瓷显微结构的不均匀,而成分分凝的发生使烧结后的(K,Na)NbO3基陶瓷的成分与原始配方偏离,从而导致性能劣化。不同温度烧结的(K, Na)NbO3基陶瓷的结构与性能变化以及相应典型陶瓷的TEM结构和能谱分析验证了上述机理。
实验表明,两段式烧结既能有效抑制碱金属元素的挥发,又能有效抑制分凝现象的发生,从而能在较宽的温度区间内获得高性能的(K, Na)NbO3基无铅压电陶瓷。纳米粉体的低温烧结也能达到两段式烧结的效果。(K,Na)Nb03基纳米粉体既能在较低温度烧结高致密度陶瓷,又能通过抑制碱金属元素的挥发及避免分凝现象的发生来保持相结构稳定性,并且没有引入任何杂相,因而能在较宽的低温区间内获得高性能的(K, Na)NbO3基无铅压电陶瓷。
以水基溶胶-凝胶法制备的K0.5Na0.5NbO3(?)内米粉体为原料,利用普通烧结法成功制备出晶粒为200-600nm的K0.5Na0.5NbO3细晶陶瓷,压电常数d33和机电耦合系数kp分别达148pC/N和38.9%。以水基溶胶-凝胶法制备的(Na0.52K0.44Li0.04)(Nb0.86Ta0.06Sb0.08)O3纳米粉体为原料,利用SPS成功制备出晶粒为200-400nm的(Na0.52K0.44Li0.04)(Nb0.86Ta0.06Sb0.08)O3细晶陶瓷,d33和kp分别达296pC/N和49.7%。
BaTiO3陶瓷的压电性能存在晶粒尺寸效应。在0.6-12.8μm的晶粒尺寸范围内,2.4μm BaTiO3陶瓷具有最优性能,室温d33高达519pC/N。
In this thesis, thesegregation phenomenonas an important factor causing the narrowsintering temperature window for (K, Na)NbO_3-based ceramics was reported. It wasfound that two-step sintering and low temperature sintering could successfullyovercame the problem. Moreover, ultrafine-grained (K, Na)NbO_3-based ceramicswereprepared by using of nano-powders from water-based sol-gel method. In addition, thepiezoelectric properties ofBaTiO_3ceramics were grain size effect. Based on themechanism, high performance BaTiO_3ceramics could be obtained by controlling thegrain size properly.
According to the analysis of KNbO_3-NaNbO_3phase diagram, the segregationphenomenon was easy to occur in the sintering process of (K, Na)NbO_3-based ceramics.It leaded to the appearance of liquid phase and compositionalinhomogeneity, resultingin nonuniform microstructuresand degraded electrical properties accordingly.Thecorresponding experimental results verified the above mechanism.
Mechanism analysis and experimental results showed thattwo-stepsintering could effectively suppress the volatilization of alkali metal elements,and couldalso effectively inhibit the occurrence of segregation phenomenon. As aresult, two-step sintering was aneffective way to broaden the sinteringtemperature range of (K, Na)NbO_3-based ceramic, and high-performance (K,Na)NbO_3-based ceramicscould be prepared over a wide sinteringtemperaturerange. Low temperature sintering by using of nano-powder couldalso achieve the effect oftwo-step sintering. By using nano-powder, dense (K,Na)NbO_3-based ceramics could be obtained over a low and wide temperature range.Besides, low temperature sintering using nano-powder could also effectivelysuppress the volatilization of alkali metal elements, inhibit the occurrence ofsegregation phenomenon and hardly bring any impurity phases. Therefore,high-performance (K, Na)NbO_3-based ceramicscould be prepared over a wide andlow sintering temperaturerange.
By using the nano-powder prepared from a water-based sol-gel method, theK_(0.5)Na_(0.5)NbO_3ultrafine-grained ceramic with the grain size of200-600nmweresuccessfully prepared by the conventional sintering. Its d33was148pC/N and k_pwas38.9%. Furthermore, by using the nano-powder prepared from awater-based sol-gel method, the(Na_(0.52)K_(0.44)Li_(0.04))(Nb_(0.86)Ta_(0.06)Sb_(0.08))O_3ultrafine-grained ceramic with the grainsize of200-400nmwere successfully prepared by the spark plasma sintering.Itsd33was296pC/N and kpwas49.7%.
The results showed that thepiezoelectric properties of BaTiO_3ceramicswere highly grain sizedependent. In the grain size range of0.6-12.8μm, the2.4μmBaTiO_3ceramic exhibited the best performancewithd33of519pC/N.
KNbO3-NaNbO3相图的分析表明,(K, Na)NbO3基陶瓷在烧结过程中易发生分凝现象,从而产生液相并出现成分的分凝。液相的出现会导致(K,Na)NbO3基陶瓷显微结构的不均匀,而成分分凝的发生使烧结后的(K,Na)NbO3基陶瓷的成分与原始配方偏离,从而导致性能劣化。不同温度烧结的(K, Na)NbO3基陶瓷的结构与性能变化以及相应典型陶瓷的TEM结构和能谱分析验证了上述机理。
实验表明,两段式烧结既能有效抑制碱金属元素的挥发,又能有效抑制分凝现象的发生,从而能在较宽的温度区间内获得高性能的(K, Na)NbO3基无铅压电陶瓷。纳米粉体的低温烧结也能达到两段式烧结的效果。(K,Na)Nb03基纳米粉体既能在较低温度烧结高致密度陶瓷,又能通过抑制碱金属元素的挥发及避免分凝现象的发生来保持相结构稳定性,并且没有引入任何杂相,因而能在较宽的低温区间内获得高性能的(K, Na)NbO3基无铅压电陶瓷。
以水基溶胶-凝胶法制备的K0.5Na0.5NbO3(?)内米粉体为原料,利用普通烧结法成功制备出晶粒为200-600nm的K0.5Na0.5NbO3细晶陶瓷,压电常数d33和机电耦合系数kp分别达148pC/N和38.9%。以水基溶胶-凝胶法制备的(Na0.52K0.44Li0.04)(Nb0.86Ta0.06Sb0.08)O3纳米粉体为原料,利用SPS成功制备出晶粒为200-400nm的(Na0.52K0.44Li0.04)(Nb0.86Ta0.06Sb0.08)O3细晶陶瓷,d33和kp分别达296pC/N和49.7%。
BaTiO3陶瓷的压电性能存在晶粒尺寸效应。在0.6-12.8μm的晶粒尺寸范围内,2.4μm BaTiO3陶瓷具有最优性能,室温d33高达519pC/N。
In this thesis, thesegregation phenomenonas an important factor causing the narrowsintering temperature window for (K, Na)NbO_3-based ceramics was reported. It wasfound that two-step sintering and low temperature sintering could successfullyovercame the problem. Moreover, ultrafine-grained (K, Na)NbO_3-based ceramicswereprepared by using of nano-powders from water-based sol-gel method. In addition, thepiezoelectric properties ofBaTiO_3ceramics were grain size effect. Based on themechanism, high performance BaTiO_3ceramics could be obtained by controlling thegrain size properly.
According to the analysis of KNbO_3-NaNbO_3phase diagram, the segregationphenomenon was easy to occur in the sintering process of (K, Na)NbO_3-based ceramics.It leaded to the appearance of liquid phase and compositionalinhomogeneity, resultingin nonuniform microstructuresand degraded electrical properties accordingly.Thecorresponding experimental results verified the above mechanism.
Mechanism analysis and experimental results showed thattwo-stepsintering could effectively suppress the volatilization of alkali metal elements,and couldalso effectively inhibit the occurrence of segregation phenomenon. As aresult, two-step sintering was aneffective way to broaden the sinteringtemperature range of (K, Na)NbO_3-based ceramic, and high-performance (K,Na)NbO_3-based ceramicscould be prepared over a wide sinteringtemperaturerange. Low temperature sintering by using of nano-powder couldalso achieve the effect oftwo-step sintering. By using nano-powder, dense (K,Na)NbO_3-based ceramics could be obtained over a low and wide temperature range.Besides, low temperature sintering using nano-powder could also effectivelysuppress the volatilization of alkali metal elements, inhibit the occurrence ofsegregation phenomenon and hardly bring any impurity phases. Therefore,high-performance (K, Na)NbO_3-based ceramicscould be prepared over a wide andlow sintering temperaturerange.
By using the nano-powder prepared from a water-based sol-gel method, theK_(0.5)Na_(0.5)NbO_3ultrafine-grained ceramic with the grain size of200-600nmweresuccessfully prepared by the conventional sintering. Its d33was148pC/N and k_pwas38.9%. Furthermore, by using the nano-powder prepared from awater-based sol-gel method, the(Na_(0.52)K_(0.44)Li_(0.04))(Nb_(0.86)Ta_(0.06)Sb_(0.08))O_3ultrafine-grained ceramic with the grainsize of200-400nmwere successfully prepared by the spark plasma sintering.Itsd33was296pC/N and kpwas49.7%.
The results showed that thepiezoelectric properties of BaTiO_3ceramicswere highly grain sizedependent. In the grain size range of0.6-12.8μm, the2.4μmBaTiO_3ceramic exhibited the best performancewithd33of519pC/N.
引文
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