CN105948746B - 一种压电陶瓷材料及其制备方法 - Google Patents
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- 239000000463 material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000000919 ceramic Substances 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract 2
- 238000000498 ball milling Methods 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(II,IV) oxide Inorganic materials O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 claims description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical group [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 7
- 229910052709 silver Inorganic materials 0.000 claims description 7
- 239000004332 silver Substances 0.000 claims description 7
- 235000015895 biscuits Nutrition 0.000 claims description 6
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 2
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims 2
- 238000003483 aging Methods 0.000 claims 1
- 239000011812 mixed powder Substances 0.000 claims 1
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims 1
- 229910052697 platinum Inorganic materials 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- 239000010955 niobium Substances 0.000 abstract description 13
- 230000006641 stabilisation Effects 0.000 abstract description 6
- 238000011105 stabilization Methods 0.000 abstract description 6
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 3
- 229910052451 lead zirconate titanate Inorganic materials 0.000 abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract 2
- HWHWBMBTCNLBGY-UHFFFAOYSA-N [Pb].[Ni].[Nb] Chemical compound [Pb].[Ni].[Nb] HWHWBMBTCNLBGY-UHFFFAOYSA-N 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 239000002002 slurry Substances 0.000 description 12
- 239000010936 titanium Substances 0.000 description 10
- 238000001816 cooling Methods 0.000 description 9
- 229910001220 stainless steel Inorganic materials 0.000 description 9
- 239000010935 stainless steel Substances 0.000 description 9
- 238000005303 weighing Methods 0.000 description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 6
- 239000004615 ingredient Substances 0.000 description 6
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- 229910052726 zirconium Inorganic materials 0.000 description 6
- 229910052758 niobium Inorganic materials 0.000 description 4
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- 239000004677 Nylon Substances 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 3
- 229960000935 dehydrated alcohol Drugs 0.000 description 3
- 238000002242 deionisation method Methods 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 3
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- 229920001778 nylon Polymers 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 102220055684 rs727504015 Human genes 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 238000011160 research Methods 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- 238000000034 method Methods 0.000 description 1
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Abstract
本发明涉及一种容量温度稳定性明显的铌镍锆钛酸铅基压电陶瓷材料及其制备方法，所述压电陶瓷材料的组成通式为：PbxBa1‑x(Ni1/ 3Nb2/3)y[Zr0.53/Ti0.47]zO3+aNb2O5。其中x、y、z均为摩尔比，0.92≤X≤0.94，0.026≤y≤0.028，0.972≤z≤0.974)，a为重量比，以PbxBa1‑x(Ni1/ 3Nb2/3)y[Zr0.53/Ti0.47]zO3重量为1计，0.2%≤a≤0.35%。该类陶瓷具备高容量温度稳定性。可满足压电驱动器压电扬声器等的应用需要，极具应用前景。
Description
技术领域
本发明涉及一种压电陶瓷材料及其制备方法，属于功能陶瓷材料技术领域。
背景技术
压电陶瓷在电子功能材料领域中占据相当大的比重，近年来，为了满足不同的使用要求，材料研究工作者一方面从老材料中发掘新效应，开拓新应用；另一方面积极地开发新型的压电功能陶瓷。大量研究表明，各种弛豫铁电体固溶物与PZT陶瓷结合而形成的三元系、四元系压电陶瓷系统，以及对这些系统进行离子置换和掺杂改性，可获得高介电、高压电性能的陶瓷材料，并且多元系压电陶瓷的性能也可以在很大范围内调节，故而现在成了人们的研究重点，也使压电陶瓷的研究前景更为广阔。
随着技术的进步，压电微位移驱动器的应用范围逐步扩大，如在纳米工程，高精度定位及加工系统中，压电微位移驱动器有着非常重要的应用。这些系统对压电微位移器也有着非常高的要求，如大压电位移，低的驱动电压，高的温度稳定性等。压电陶瓷在不同温度下介电性能、谐振频率等会发生偏移，超过居里温度点还会出现压电性能消失的情况。因此，此类高性能微位移驱动器用压电陶瓷材料容量温度稳定性不得超过5000ppm，频率稳定稳定性在-40℃到85℃范围内变化不得超过0.4%。
为了达到较高的温度稳定性，提高微位移驱动器的精度，本发明采用PbxBa1-x(Ni1/3Nb2/3)y[Zr0.53/Ti0.47]zO3+aNb2O5，0.026≤y≤0.028，0.972≤z≤0.974的铌镍酸铅和锆钛酸铅比例、钡0.92≤X≤0.94的A位取代量以及铌0.3%≤a≤0.35%的掺杂有效改善了陶瓷具备高容量温度稳定性。可满足压电驱动器压电扬声器等的应用需要，极具应用前景。
实施例一：
在配料前准备好球磨罐及氧化锆球并清洗干净，按照1L尼龙罐1.5kgφ3锆球500g粉料比例配备待用。
步骤1）按照PbxBa1-x(Ni1/3Nb2/3)y[Zr0.53/Ti0.47]zO3+aNb2O5，其中x、y、z均为摩尔比，X=0.935，y=0.0275，z=0.9725，a为重量比，以PbxBa1-x(Ni1/3Nb2/3)y[Zr0.53/Ti0.47]zO3重量为1计，a=0.34%。
准备物料，并进行水分测试，测试数据用以修正称量重量。根据修正好的重量数据称重配料，配料时按照四氧化三铅（约1/2）、及锆、钛、铌、碳酸钡、另一半的四氧化三铅的顺序加入到球磨罐中。按照料：去离子水：无工业酒精=1:0.8:0.08（重量比）加相应的去离子水及无水乙醇到球磨桶中。用行星球磨机球磨2～3小时，倒出混合好的料于不锈钢盘中，开启箱电源，设定上下温度为120～150℃，前期每10～15分钟进行搅拌一次直至料浆烘至粘稠状，当料浆烘干至块状不黏手时即为烘干，关电源，自然冷却待烘干（料浆粒度达到：D50＜0.55μm,D90＜1.55μm）。将冷却后的不锈钢盘取出，在盘中初步捣碎料块后，刮下盘壁上粘料混均，加入打粉机粉碎。再将粉料装入匣钵中，每加入半勺，铺平，振实，即将加满时称重，料重控制在620±3g.压实后的料面距匣钵上沿1.5cm左右。装好的匣钵送入预烧炉中预烧。
步骤2）将装好的匣钵放入高温炉预烧，在800～900℃合成2～3小时，将合成好的粉体捣碎按照料：去离子水：无工业酒精=1:0.8:0.08（重量比）加相应的去离子水及无水乙醇到球磨桶中。用行星球磨机球磨2.5小时，倒出混合好的料于不锈钢盘中，开启箱电源，设定上下温度为135℃烘干，关电源，自然冷却待烘干（料浆粒度达到：D50＜0.55μm,D90＜1.55μm）。
步骤3）将烘干好的预烧粉加入8%（重量比）的PVA水溶液（PVA含量5%）。在10Mpa下压制成素坯，放入高温烧结炉中1300℃烧结2小时。取出后两面磨平，涂敷银电极并用120℃烘干后，放入高温炉设置温度为500℃保温十分钟。
步骤4）将上完银电极的压电陶瓷片在130℃温度下采用1100V/mm电压极化。
将极化好的陶瓷片在100℃老化10h，并测试数据得：Kp=0.75,C33=1800 tgθ=1.6%Qm=45 d33=500容量温度稳定性<2000ppm，-40℃到85℃，频率变化为0.3%。
实施例二：
在配料前准备好球磨罐及氧化锆球并清洗干净，按照1L尼龙罐1.5kgφ3锆球500g粉料比例配备待用。
步骤1）按照PbxBa1-x(Ni1/3Nb2/3)y[Zr0.53/Ti0.47]zO3+aNb2O5，其中x、y、z均为摩尔比，X=0.93，y=0.027，z=0.973，a为重量比，以PbxBa1-x(Ni1/3Nb2/3)y[Zr0.53/Ti0.47]zO3重量为1计，a=0.345%。
准备物料，并进行水分测试，测试数据用以修正称量重量。根据修正好的重量数据称重配料，配料时按照四氧化三铅（约1/2）、及锆、钛、铌、碳酸钡、另一半的四氧化三铅的顺序加入到球磨罐中。按照料：去离子水：无工业酒精=1:0.8:0.08（重量比）加相应的去离子水及无水乙醇到球磨桶中。用行星球磨机球磨3小时，倒出混合好的料于不锈钢盘中，开启箱电源，设定上下温度为120～150℃，前期每10～15分钟进行搅拌一次直至料浆烘至粘稠状，当料浆烘干至块状不黏手时即为烘干，关电源，自然冷却待烘干（料浆粒度达到：D50＜0.55μm,D90＜1.55μm）。将冷却后的不锈钢盘取出，在盘中初步捣碎料块后，刮下盘壁上粘料混均，加入打粉机粉碎。再将粉料装入匣钵中，每加入半勺，铺平，振实，即将加满时称重，料重控制在620±3g.压实后的料面距匣钵上沿1.5cm左右。装好的匣钵送入预烧炉中预烧。
步骤2）将装好的匣钵放入高温炉预烧，在800～900℃合成2～3小时，将合成好的粉体捣碎按照料：去离子水：无工业酒精=1:0.8:0.08（重量比）加相应的去离子水及无水乙醇到球磨桶中。用行星球磨机球磨2.5小时，倒出混合好的料于不锈钢盘中，开启箱电源，设定上下温度为135℃烘干，关电源，自然冷却待烘干（料浆粒度达到：D50＜0.55μm,D90＜1.55μm）。
步骤3）将烘干好的预烧粉加入8%（重量比）的PVA水溶液（PVA含量5%）。在8Mpa下压制成素坯，放入高温烧结炉中1250℃烧结2小时。取出后两面磨平，涂敷银钯电极并用120℃烘干后，放入高温炉设置温度为500℃保温十分钟。
步骤4）将上完银电极的压电陶瓷片在130℃温度下采用1000V/mm电压极化。
将极化好的陶瓷片在100℃老化10h，并测试数据得：Kp=0.73,C33=1900 tgθ=1.7%Qm=48 d33=550容量温度稳定性<2200ppm，-40℃到85℃，频率变化为0.35%。
实施例三：
在配料前准备好球磨罐及氧化锆球并清洗干净，按照1L尼龙罐1.5kgφ3锆球500g粉料比例配备待用。
步骤1）按照PbxBa1-x(Ni1/3Nb2/3)y[Zr0.53/Ti0.47]zO3+aNb2O5，其中x、y、z均为摩尔比，X=0.94，y=0.028，z=0.972，a为重量比，以PbxBa1-x(Ni1/3Nb2/3)y[Zr0.53/Ti0.47]zO3重量为1计，a=0.35%。
准备物料，并进行水分测试，测试数据用以修正称量重量。根据修正好的重量数据称重配料，配料时按照四氧化三铅（约1/2）、及锆、钛、铌、碳酸钡、另一半的四氧化三铅的顺序加入到球磨罐中。按照料：去离子水：无工业酒精=1:0.8:0.08（重量比）加相应的去离子水及无水乙醇到球磨桶中。用行星球磨机球磨2～3小时，倒出混合好的料于不锈钢盘中，开启箱电源，设定上下温度为120～150℃，前期每10～15分钟进行搅拌一次直至料浆烘至粘稠状，当料浆烘干至块状不黏手时即为烘干，关电源，自然冷却待烘干（料浆粒度达到：D50＜0.55μm,D90＜1.55μm）。将冷却后的不锈钢盘取出，在盘中初步捣碎料块后，刮下盘壁上粘料混均，加入打粉机粉碎。再将粉料装入匣钵中，每加入半勺，铺平，振实，即将加满时称重，料重控制在620±3g.压实后的料面距匣钵上沿1.5cm左右。装好的匣钵送入预烧炉中预烧。
步骤2）将装好的匣钵放入高温炉预烧，在800～900℃合成2～3小时，将合成好的粉体捣碎按照料：去离子水：无工业酒精=1:0.8:0.08（重量比）加相应的去离子水及无水乙醇到球磨桶中。用行星球磨机球磨2.5小时，倒出混合好的料于不锈钢盘中，开启箱电源，设定上下温度为135℃烘干，关电源，自然冷却待烘干（料浆粒度达到：D50＜0.55μm,D90＜1.55μm）。
步骤3）将烘干好的预烧粉加入8%（重量比）的PVA水溶液（PVA含量5%）。在15Mpa下压制成素坯，放入高温烧结炉中1350℃烧结2小时。取出后两面磨平，涂敷银电极并用120℃烘干后，放入高温炉设置温度为500℃保温十分钟。
步骤4）将上完银电极的压电陶瓷片在130℃温度下采用1100V/mm电压极化。
将极化好的陶瓷片在100℃老化10h，并测试数据得：Kp=0.76,C33=1800 tgθ=1.6%Qm=42 d33=530容量温度稳定性<2100ppm，-40℃到85℃，频率变化为0.28%。
Claims (4)
1.一种压电陶瓷材料，其特征在于：组成式为Pb0.94Ba0.06(Ni1/3Nb2/3)0.026[Zr0.53/Ti0.47]0.974O3+aNb2O5或者为Pb0.93Ba0.07(Ni1/3Nb2/3)0.027[Zr0.53/Ti0.47]0.973O3+aNb2O5，0.34%≤a≤0.35%。
2.一种权利要求1所述压电陶瓷材料制备方法，其特征在于制备方法包括：
步骤1）将原材料Pb3O4、TiO2、ZrO2、BaCO3、NiO、Nb2O5按照所述化学计量比称量，首先加入一半左右Pb3O4，加完其他材料后再加入剩余Pb3O4，最后加入去离子水，球磨2～3小时倒出烘干；
步骤2）将混合均匀的粉体倒入氧化铝匣钵振实，在800～900℃合成2～4小时，将合成好的粉体捣碎加入去离子水球磨2～3小时倒出烘干；
步骤3）将烘干的粉体中加入PVA压制素坯，压制素坯压力为5～15Mpa，压制成素坯在1200℃～1350℃烧结2～3小时，双面磨平，表面覆盖电极；
步骤4）将覆盖电极的压电陶瓷极化，极化电压为900V/mm～1500V/mm，极化温度为120℃～140℃，获得具备高容量温度稳定性的压电陶瓷。
3.如权利要求2所述的制备方法，其特征在于步骤3）表面覆盖电极为银电极、银钯或银铂电极中的一种。
4.如权利要求2所述的制备方法，其特征在于极化好的压电陶瓷材料需要在100℃老化8～12h。
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