CN106348748B - 一种高温x8r型陶瓷电容器介质材料及其制备方法 - Google Patents
一种高温x8r型陶瓷电容器介质材料及其制备方法 Download PDFInfo
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- CN106348748B CN106348748B CN201610738044.3A CN201610738044A CN106348748B CN 106348748 B CN106348748 B CN 106348748B CN 201610738044 A CN201610738044 A CN 201610738044A CN 106348748 B CN106348748 B CN 106348748B
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- barium
- fused matter
- titanate
- ceramic capacitor
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- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 29
- 239000003989 dielectric material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- KOJWXHDDSAMYEG-UHFFFAOYSA-N [Na].[Ba].[Bi] Chemical compound [Na].[Ba].[Bi] KOJWXHDDSAMYEG-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910002115 bismuth titanate Inorganic materials 0.000 claims abstract description 54
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 43
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract description 40
- ADQUQHZAQKMUDV-UHFFFAOYSA-N barium boron Chemical compound [B].[Ba] ADQUQHZAQKMUDV-UHFFFAOYSA-N 0.000 claims abstract description 28
- ZVLDJSZFKQJMKD-UHFFFAOYSA-N [Li].[Si] Chemical compound [Li].[Si] ZVLDJSZFKQJMKD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000005245 sintering Methods 0.000 claims abstract description 19
- WLJDBAQOCCWKQY-UHFFFAOYSA-N [Mn].[Nb] Chemical compound [Mn].[Nb] WLJDBAQOCCWKQY-UHFFFAOYSA-N 0.000 claims abstract description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 12
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 8
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 7
- 239000010941 cobalt Substances 0.000 claims abstract description 7
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 5
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 5
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 4
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 4
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 4
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 4
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 4
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims abstract description 4
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims abstract description 4
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims abstract description 4
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims abstract description 4
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims description 37
- 238000000498 ball milling Methods 0.000 claims description 35
- 238000003786 synthesis reaction Methods 0.000 claims description 28
- 230000015572 biosynthetic process Effects 0.000 claims description 25
- 229910010252 TiO3 Inorganic materials 0.000 claims description 18
- 239000010955 niobium Substances 0.000 claims description 16
- 238000005469 granulation Methods 0.000 claims description 15
- 230000003179 granulation Effects 0.000 claims description 15
- 239000004615 ingredient Substances 0.000 claims description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 11
- 239000011734 sodium Substances 0.000 claims description 11
- 229910052758 niobium Inorganic materials 0.000 claims description 10
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 8
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 8
- 239000012188 paraffin wax Substances 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 229910052788 barium Inorganic materials 0.000 claims description 6
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 claims description 4
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 claims description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 3
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 239000011572 manganese Substances 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 239000003990 capacitor Substances 0.000 abstract description 9
- 238000009766 low-temperature sintering Methods 0.000 abstract description 6
- 229910052573 porcelain Inorganic materials 0.000 abstract description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract 1
- 229910052725 zinc Inorganic materials 0.000 abstract 1
- 239000011701 zinc Substances 0.000 abstract 1
- 238000001354 calcination Methods 0.000 description 21
- 238000002156 mixing Methods 0.000 description 20
- 230000002194 synthesizing effect Effects 0.000 description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 11
- -1 rare earth compound Chemical class 0.000 description 8
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 6
- 229910052681 coesite Inorganic materials 0.000 description 6
- 229910052906 cristobalite Inorganic materials 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 229910052682 stishovite Inorganic materials 0.000 description 6
- 229910052905 tridymite Inorganic materials 0.000 description 6
- 229910052726 zirconium Inorganic materials 0.000 description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 5
- 229910010293 ceramic material Inorganic materials 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 4
- 238000005457 optimization Methods 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- PILOURHZNVHRME-UHFFFAOYSA-N [Na].[Ba] Chemical compound [Na].[Ba] PILOURHZNVHRME-UHFFFAOYSA-N 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 238000003181 co-melting Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- ZYCFPSLHSPMWDE-UHFFFAOYSA-N [Mn].[Nb].[Co] Chemical compound [Mn].[Nb].[Co] ZYCFPSLHSPMWDE-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000011656 manganese carbonate Substances 0.000 description 2
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- LFUSWQZWBZPZCV-UHFFFAOYSA-N [Bi].[Na].[Ti] Chemical compound [Bi].[Na].[Ti] LFUSWQZWBZPZCV-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- XDFCIPNJCBUZJN-UHFFFAOYSA-N barium(2+) Chemical compound [Ba+2] XDFCIPNJCBUZJN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 description 1
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- 150000002910 rare earth metals Chemical group 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- LGERWORIZMAZTA-UHFFFAOYSA-N silicon zinc Chemical compound [Si].[Zn] LGERWORIZMAZTA-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
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Abstract
本发明属于多层陶瓷电容器材料技术领域，特别涉及高温X8R型陶瓷电容器介质材料及其制备方法。该种高温X8R型陶瓷电容器介质材料，以钛酸钡和钛酸铋钠钡的共融物为主基料，添加铌锰和A的氧化物的共融物、硅锂共融物、硼钡共融物、Re2O3，其中，元素A为钴、镍、锌、铋等的一种或几种，元素Re为稀土元素镨、钐、钆、钕、镝等的一种或几种。使用本发明高温X8R型陶瓷电容器介质材料制得的电容器具有高介电常数、高耐压强度、高温度稳定性，并且能够在制备多层瓷介固定电容器时与中低温烧结的30Pd‑70Ag内电极相匹配而实现中温烧结，并实现在高温环境的应用，具有较高的产业化前景和工业应用价值。
Description
技术领域
本发明属于多层陶瓷电容器材料技术领域，特别涉及高温X8R型陶瓷电容器介质材料及其制备方法。
背景技术
多层瓷介固定电容器(下称MLCC)是各种电子设备不可缺少的重要元件，具有容量范围大、介质损耗低、体积小、适合表面贴装等特点，广泛应用于航天、航空、武器装备、电子对抗、汽车控制、能源勘探、工业控制、移动通信、轨道交通等军事和工业领域。
随着现代信息技术和MLCC应用领域产业的高速发展，MLCC不断向高耐压强度、高温度稳定、高容量、微型化、高可靠方向发展,尤其是在一些特殊环境下的应用，对MLCC的工作温度范围和介电容温变化率提出更高的要求，如各种军事装备的大推力发动机、大功率相控雷达，石油钻井设备以及汽车领域的防抱死系统、电子控制单元等对MLCC工作温度要求延伸到150℃，甚至更高。
根据美国EIA标准，X7R的工作温度范围为-55℃～125℃，X8R的工作温度范围为-55℃～150℃，两者的容温变化率均为±15％以内；显然X7R在某些特殊环境的应用，特别是在高温环境的应用不及X8R。钛酸钡的居里温度为125℃左右，其介电常数高，但介质损耗过高、容温变化率恶劣以及老化率严重，近年来国内外研究人员以钛酸钡为基材对X8R材料展开研究，并取得一定程度的进展，如专利200480015816.6，使用稀土氧化物、Nb2O5、Ta2O5、Co3O4、玻璃粉等物质对钛酸钡进行改性，但其发明只能满足X7R要求，不能满足更高工作温度要求；又如专利201210146787.3，使用钛铋钠化合物BNT提高钛酸钡居里温度、并添加锆钛化合物、稀土化合物、玻璃粉等物质对钛酸钡进行改性，其满足X8R特性，介电常数可达2700以上，但是介电损耗最低仍达1.55％，并且其烧结温度在1270℃以上，制成MLCC时不能与中低温烧结用的30Pd-70Ag内电极匹配，只能选用纯Pd,制造成本昂贵，不利于产业化；再如专利201310413203.9，使用(Sr、Ca、Ba)Bi4Ti4O15提高钛酸钡居里温度,并通过微量稀土氧化物、ZnNb2O6、ZrO2、硅锌化合物、MnCO3、玻璃粉等物质对钛酸钡进行改性，其满足X8R特性的介电常数最高仅达1900，并且不涉及耐压强度。
因此，制备一种具有高介电常数(K值)、高耐压强度、高温度稳定性(150℃以上)，并且能够在制备多层瓷介固定电容器时与中低温烧结的30Pd-70Ag内电极相匹配而实现中温烧结(1100℃～1190℃)，并实现在高温环境的应用，具有较高的产业化前景和工业应用价值。
发明内容
为了克服现有技术的不足，本发明提供一种解决工作温度范围低、耐压强度低、介电常数低、介质损耗高、烧结温度高等问题，具有高介电常数(K值)、高耐压强度、高温度稳定性(150℃以上)，并且能够在制备多层瓷介固定电容器时与中低温烧结的30Pd-70Ag内电极相匹配而实现中温烧结(1100℃～1190℃)的高温X8R型陶瓷电容器介质材料及其制备方法。
为实现上述目的，本发明提供了一种高温X8R型陶瓷电容器介质材料，其特征在于：其以100重量份的钛酸钡和钛酸铋钠钡的共融物为主基料，添加0.8～3.0份的铌锰和A的氧化物的共融物、0.2～1.0份的硅锂共融物、0.6～2.5份的硼钡共融物、0.5～2.0份的Re2O3；
其中，元素A为钴(Co)、镍(Ni)、锌(Zn)、铋(Bi)等的一种或几种，元素Re为稀土元素镨(Pr)、钐(Sm)、钆(Gd)、钕(Nd)、镝(Dy)等的一种或几种。
进一步的，钛酸钡和钛酸铋钠钡的共融物的化学式为:
[(1-x)BaTiO3-xBay(NaO.5Bi0.5)(1-y)TiO3]，其中，x＝0.005～0.03；y＝0.02～0.1。
进一步的，铌锰和A的氧化物的共融物中，铌与锰的原子比为6-11，铌与元素A的原子比为4.5-8.5。
进一步的，硅锂共融物中,Li/Si原子比＝2-4。
进一步的，硼钡共融物中,Ba/B原子比＝0.25-0.5。
一种高温X8R型陶瓷电容器介质材料的制备方法，其特征在于，包括以下步骤：
步骤1，先合成钛酸铋钠钡后再合成钛酸钡和钛酸铋钠钡的共融物；
步骤2，合成铌锰和A的氧化物的共融物；
步骤3，合成硅锂共融物；
步骤4，合成硼钡共融物；
步骤5，根据原料配比分别称量步骤1-4制备的共融物，以水为分散介质，依次进行球磨、干燥、破碎并造粒，造粒后的粉料在2～10Mpa条件下压制成圆片生坯，然后在空气气氛中升温至1100～1190℃，并保温烧结1～4h，即制得高温X8R型陶瓷电容器介质材料。
优化的，步骤1中：
合成钛酸铋钠钡[Bay(NaO.5Bi0.5)(1-y)TiO3]，按化学式[Bay(Na0.5Bi0.5)(1-y)TiO3],以Ba(OH)2·8H2O、Na2CO3、Bi2O3、TiO2原料，进行配料、球磨、干燥、破碎、过40目标准筛网，然后在850～950℃条件下煅烧1～4h合成钛酸铋钠钡。
优化的，步骤1中：
合成钛酸钡和钛酸铋钠钡的共融物[(1-x)BaTiO3-xBay(NaO.5Bi0.5)(1-y)TiO3]，按化学式[(1-x)BaTiO3-xBay(Na0.5Bi0.5)(1-y)TiO3]，把合成的钛酸铋钠钡Bay(NaO.5Bi0.5)(1-y)TiO3添加到BaTiO3中进行配料、球磨、干燥、破碎、过40目标准筛网，然后在1020～1150℃条件下煅烧2～6h合成钛酸钡和钛酸铋钠钡的共融物。
优化的，步骤5中，球磨工艺采用2～5mm的氧化锆球作磨介，研磨2～10h，然后烘干、过筛，再加入5～10重量份的石蜡做粘结剂共同烘焙造粒，并再次过筛。
由上述对本发明描述可知，本发明具有如下有益效果：
第一，本发明的高温X8R型陶瓷电容器介质材料通过合成钛酸钡和钛酸铋钠钡的共融物提高钛酸钡体系的居里温度，使其具有更高的工作温度范围。
第二，本发明通过铌锰和A的氧化物的共融物以及稀土氧化物的共同作用，使得钛酸钡基介电陶瓷材料实现双峰结构，有效降低介电容温变化率，实现X8R特性；并且Nb5+、Gd3 +、Nd3+、Pr3+、Dy3+、Sm3+等离子的存在有利于维持电中性，提高体系绝缘电阻，并在烧结过程中抑制晶粒长大提高烧结致密性，从而降低介质损耗，提高体系的耐压强度。
第三，本发明通过添加硅锂共融物、硼钡共融物等助熔剂，一方面起到降低烧结温度作用；更重要的一方面是Li+能有效改善高温稳定性，Ba2+的存在也可以有效拟补陶瓷材料在烧结过程中产生的Ba空位，从而减少本发明中陶瓷材料的缺陷，提高绝缘电阻，降低介电损耗，实现高耐压强度，并保持钛酸钡晶体结构稳定，从而使本发明的陶瓷材料具有更好的高温稳定性。
第四，本发明的介电陶瓷材料能够中温烧结，其在制备多层瓷介固定电容器时能与中低温烧结的30Pd-70Ag内电极相匹配，从而降低生产成本，有利于产业化发展。
第五，本发明的介电陶瓷材料采用传统固相法工艺即可制备，工艺要求不高。
综上所述，本发明所制得的陶瓷电容器介质材料具有高介电常数(K值)、高耐压强度、高温度稳定性(150℃以上)，并且能够在制备多层瓷介固定电容器时与中低温烧结的30Pd-70Ag内电极相匹配而实现中温烧结(1100℃～1190℃)，并实现在高温环境的应用，具有较高的产业化前景和工业应用价值。
附图说明
图1为本发明制得的陶瓷电容器介质材料的电容温变化曲线示意图。
具体实施方式
参照图1所示，以下通过具体实施方式对本发明作进一步的描述。
一种高温X8R型陶瓷电容器介质材料，其以100重量份的钛酸钡和钛酸铋钠钡的共融物为主基料，添加0.8～3.0份的铌锰和A的氧化物的共融物、0.2～1.0份的硅锂共融物、0.6～2.5份的硼钡共融物、0.5～2.0份的Re2O3；
其中，钛酸钡和钛酸铋钠钡的共融物的化学式为:[(1-x)BaTiO3-xBay(NaO.5Bi0.5)(1-y)TiO3]，其中，x＝0.005～0.03；y＝0.02～0.1；
铌锰和A的氧化物的共融物中，元素A为钴(Co)、镍(Ni)、锌(Zn)、铋(Bi)等的一种或几种，铌与锰的原子比为6-11，铌与元素A的原子比为4.5-8.5；
硅锂共融物中，Li/Si原子比＝2-4；
硼钡共融物中,Ba/B原子比＝0.25-0.5。
Re2O3中，元素Re为稀土元素镨(Pr)、钐(Sm)、钆(Gd)、钕(Nd)、镝(Dy)等的一种或几种。
一种高温X8R型陶瓷电容器介质材料的制备方法，其特征在于，包括以下步骤：
步骤1，先合成钛酸铋钠钡后再合成钛酸钡和钛酸铋钠钡的共融物；
步骤2，合成铌锰和A的氧化物的共融物，按铌与锰的原子比为6ˉ11，铌与A元素的原子比为4.5ˉ8.5，以Nb2O5、MnCO3、A的氧化物为原料，其中A元素为钴(Co)、镍(Ni)、锌(Zn)、铋(Bi)等的一种或几种，进行配料、球磨、干燥、破碎、过40目标准筛网，然后在900～1150℃条件下煅烧2～6h合成铌锰和A的氧化物的共融物；
步骤3，合成硅锂共融物，按Li/Si原子比＝2ˉ4，以Li2CO3、SiO2为原料，进行配料、球磨、干燥、破碎、过40目标准筛网，然后在550～750℃条件下煅烧1～4h合成硅锂共融物；
步骤4，合成硼钡共融物，按Ba/B原子比＝0.25ˉ0.5，以Ba(OH)2·8H2O、H3BO3为原料，进行配料、球磨、干燥、破碎、过40目标准筛网，然后在500～700℃条件下煅烧2～6h合成硼钡共融物；
步骤5，以100重量份的钛酸钡和钛酸铋钠钡的共融物为主基料，添加0.8～3.0重量份的铌锰和A的氧化物的共融物、0.2～1.0重量份的硅锂共融物、0.6～2.5重量份的硼钡共融物及0.5～2.0重量份的Re2O3，以水为分散介质，依次进行球磨、干燥、破碎并造粒，造粒后的粉料在2～10Mpa条件下压制成圆片生坯，然后在空气气氛中升温至1100～1190℃，并保温烧结1～4h，即制得高温X8R型陶瓷电容器介质材料，球磨工艺采用2～5mm的氧化锆球作磨介，研磨2～10h，然后烘干、过筛，再加入5～10重量份的石蜡做粘结剂共同烘焙造粒，并再次过筛。
优化的，步骤1中：
合成钛酸铋钠钡[Bay(NaO.5Bi0.5)(1-y)TiO3]，按化学式[Bay(Na0.5Bi0.5)(1-y)TiO3],以Ba(OH)2·8H2O、Na2CO3、Bi2O3、TiO2原料，进行配料、球磨、干燥、破碎、过40目标准筛网，然后在850～950℃条件下煅烧1～4h合成钛酸铋钠钡；
合成钛酸钡和钛酸铋钠钡的共融物[(1-x)BaTiO3-xBay(NaO.5Bi0.5)(1-y)TiO3]，按化学式[(1-x)BaTiO3-xBay(Na0.5Bi0.5)(1-y)TiO3]，把合成的钛酸铋钠钡Bay(NaO.5Bi0.5)(1-y)TiO3添加到BaTiO3中进行配料、球磨、干燥、破碎、过40目标准筛网，然后在1020～1150℃条件下煅烧2～6h合成钛酸钡和钛酸铋钠钡的共融物。
具体实施例一：
步骤1，先合成钛酸铋钠钡后再合成钛酸钡和钛酸铋钠钡的共融物，分别称取8.11g Ba(OH)2·8H2O、10.68g Na2CO3、46.96g Bi2O3、34.25g TiO2，混合球磨、干燥、破碎、过40目标准筛网，于850℃煅烧2h合成钛酸铋钠钡；分别称取98g BaTiO3和2g步骤①合成的钛酸铋钠钡,混合球磨、干燥、破碎、过40目标准筛网，于1100℃煅烧3h合成钛酸钡和钛酸铋钠钡的共融物；
步骤2，合成铌锰和A的氧化物的共融物，分别称取78g Nb2O5、10g MnCO3、3gZnO、9gCo2O3，混合球磨、干燥、破碎、过40目标准筛网，于900℃条件下煅烧2.5h合成铌锰锌钴共融物；
步骤3，合成硅锂共融物，分别称取71.09g Li2CO3、28.91g SiO2，混合球磨、干燥、破碎、过40目标准筛网，于600℃煅烧2h合成硅锂共融物；
步骤4，合成硼钡共融物，分别称取71.83g Ba(OH)2·8H2O、28.17g H3BO3，混合球磨、干燥、破碎、过40目标准筛网，于600℃煅烧2h合成硼钡共融物；
步骤5，准确称取100g钛酸钡和钛酸铋钠钡的共融物，1.5g铌锰锌钴共融物、0.3g硅锂共融物、0.9g硼钡共融物及0.8g Gd2O3进行配料,以水为分散介质，采用2mm的锆球研磨6h，烘干、过80目标准筛网，再加入8％的石蜡做粘结剂共同烘焙造粒，并再次过80目标准筛网，将造粒后的粉料在8Mpa条件下压制成圆片生坯，然后在空气气氛中升温至1170℃，并保温烧结3h，即制得高温X8R型陶瓷电容器介质材料。
具体实施例二：
步骤1，先合成钛酸铋钠钡后再合成钛酸钡和钛酸铋钠钡的共融物，分别称取8.11g Ba(OH)2·8H2O、10.68g Na2CO3、46.96g Bi2O3、34.25g TiO2，混合球磨、干燥、破碎、过40目标准筛网，于900℃煅烧2h合成钛酸铋钠钡,分别称取97.5g BaTiO3和2.5g步骤①合成的钛酸铋钠钡,混合球磨、干燥、破碎、过40目标准筛网，于1090℃煅烧3h合成钛酸钡和钛酸铋钠钡的共融物；
步骤2，合成铌锰和A的氧化物的共融物，分别称取80g Nb2O5、10g MnCO3、10gCo2O3，混合球磨、干燥、破碎、过40目标准筛网，于930℃条件下煅烧2.5h合成铌锰钴共融物；
步骤3，合成硅锂共融物，分别称取66.28g Li2CO3、33.72g SiO2，混合球磨、干燥、破碎、过40目标准筛网，于630℃煅烧2h合成硅锂共融物
步骤4，合成硼钡共融物，分别称取71.83g Ba(OH)2·8H2O、28.17g H3BO3，混合球磨、干燥、破碎、过40目标准筛网，于630℃煅烧2h合成硼钡共融物
步骤5，准确称取100g钛酸钡和钛酸铋钠钡的共融物，0.8g铌锰钴共融物、0.4g硅锂共融物、1.5g硼钡共融物及1.0g Dy2O3进行配料,以水为分散介质，采用2mm的锆球研磨6h，烘干、过80目标准筛网，再加入8％的石蜡做粘结剂共同烘焙造粒，并再次过80目标准筛网，将造粒后的粉料在8Mpa条件下压制成圆片生坯，然后在空气气氛中升温至1160℃，并保温烧结3h，即制得高温X8R型陶瓷电容器介质材料。
具体实施例三：
步骤1，先合成钛酸铋钠钡后再合成钛酸钡和钛酸铋钠钡的共融物，分别称取5.49g Ba(OH)2·8H2O、11.07g Na2CO3、48.67g Bi2O3、34.76g TiO2，混合球磨、干燥、破碎、过40目标准筛网，于890℃煅烧2h合成钛酸铋钠钡，分别称取97g BaTiO3和3g步骤①合成的钛酸铋钠钡,混合球磨、干燥、破碎、过40目标准筛网，于1100℃煅烧3h合成钛酸钡和钛酸铋钠钡的共融物；
步骤2，合成铌锰和A的氧化物的共融物，分别称取80g Nb2O5、10g MnCO3、10gBi2O3，混合球磨、干燥、破碎、过40目标准筛网，于930℃条件下煅烧2.5h合成铌锰铋共融物；
步骤3，合成硅锂共融物，分别称取71.09g Li2CO3、28.91g SiO2，混合球磨、干燥、破碎、过40目标准筛网，于650℃煅烧2h合成硅锂共融物；
步骤4，合成硼钡共融物，分别称取60.18g Ba(OH)2·8H2O、39.82g H3BO3，混合球磨、干燥、破碎、过40目标准筛网，于650℃煅烧2h合成硼钡共融物；步骤5，准确称取100g钛酸钡和钛酸铋钠钡的共融物，2.2g铌锰铋共融物、0.2g硅锂共融物、2.0g硼钡共融物及1.3gPr2O3进行配料,以水为分散介质，采用2mm的锆球研磨6h，烘干、过80目标准筛网，再加入8％的石蜡做粘结剂共同烘焙造粒，并再次过80目标准筛网，将造粒后的粉料在8Mpa条件下压制成圆片生坯，然后在空气气氛中升温至1160℃，并保温烧结3h，即制得高温X8R型陶瓷电容器介质材料。
具体实施例四：
步骤1，先合成钛酸铋钠钡后再合成钛酸钡和钛酸铋钠钡的共融物，分别称取5.49g Ba(OH)2·8H2O、11.07g Na2CO3、48.67g Bi2O3、34.76g TiO2，混合球磨、干燥、破碎、过40目标准筛网，于890℃煅烧2h合成钛酸铋钠钡，分别称取99g BaTiO3和1g步骤①合成的钛酸铋钠钡,混合球磨、干燥、破碎、过40目标准筛网，于1100℃煅烧3h合成钛酸钡和钛酸铋钠钡的共融物；
步骤2，合成铌锰和A的氧化物的共融物，分别称取85g Nb2O5、7g MnCO3、4g NiO、4gZnO，混合球磨、干燥、破碎、过40目标准筛网，于950℃条件下煅烧2.5h合成铌锰镍锌共融物；
步骤3，合成硅锂共融物，分别称取66.28g Li2CO3、33.72g SiO2，混合球磨、干燥、破碎、过40目标准筛网，于650℃煅烧2h合成硅锂共融物；
步骤4，合成硼钡共融物，分别称取61.18g Ba(OH)2·8H2O、39.82g H3BO3，混合球磨、干燥、破碎、过40目标准筛网，于650℃煅烧2h合成硼钡共融物；
步骤5，准确称取100g步骤钛酸钡和钛酸铋钠钡的共融物，3.0g铌锰镍锌共融物、1.0g硅锂共融物、1.0g硼钡共融物及1.5g Sm2O3进行配料,以水为分散介质，采用2mm的锆球研磨6h，烘干、过80目标准筛网，再加入8％的石蜡做粘结剂共同烘焙造粒，并再次过80目标准筛网，将造粒后的粉料在8Mpa条件下压制成圆片生坯，然后在空气气氛中升温至1140℃，并保温烧结3h，即制得高温X8R型陶瓷电容器介质材料。
具体实施例五：
步骤1，先合成钛酸铋钠钡后再合成钛酸钡和钛酸铋钠钡的共融物，分别称取5.49g Ba(OH)2·8H2O、11.07g Na2CO3、48.67g Bi2O3、34.76g TiO2，混合球磨、干燥、破碎、过40目标准筛网，于890℃煅烧2h合成钛酸铋钠钡，分别称取98.5g BaTiO3和1.5g步骤①合成的钛酸铋钠钡,混合球磨、干燥、破碎、过40目标准筛网，于1100℃煅烧3h合成钛酸钡和钛酸铋钠钡的共融物；
步骤2，合成铌锰和A的氧化物的共融物，分别称取87g Nb2O5、5g MnCO3、5gNiO、3gCo2O3，混合球磨、干燥、破碎、过40目标准筛网，于950℃条件下煅烧2.5h合成铌锰镍钴共融物；
步骤3，合成硅锂共融物，分别称取69.19g Li2CO3、30.81g SiO2，混合球磨、干燥、破碎、过40目标准筛网，于660℃煅烧2h合成硅锂共融物；
步骤4，合成硼钡共融物，分别称取69.07g Ba(OH)2·8H2O、30.93g H3BO3，混合球磨、干燥、破碎、过40目标准筛网，于650℃煅烧2h合成硼钡共融物；
步骤5，准确称取100g钛酸钡和钛酸铋钠钡的共融物，1.0g铌锰镍钴共融物、0.7g硅锂共融物、1.4g硼钡共融物及2.0g Nd2O3进行配料,以水为分散介质，采用2mm的锆球研磨6h，烘干、过80目标准筛网，再加入8％的石蜡做粘结剂共同烘焙造粒，并再次过80目标准筛网，将造粒后的粉料在8Mpa条件下压制成圆片生坯，然后在空气气氛中升温至1160℃，并保温烧结3h，即制得高温X8R型陶瓷电容器介质材料。
参照图1所示，高温X8R型陶瓷电容器，将具体实施例1-5所制得的高温X8R型陶瓷电容器介质材料两侧烧制银电极，制成圆片电容器，并检测各项电性能，检测结果如下表：
其中，Max|△C/C|(％)值的温度范围为-55℃～150℃
上述仅为本发明的一个具体实施方式，但本发明的设计构思并不局限于此，凡利用此构思对本发明进行非实质性的改动，均应属于侵犯本发明保护范围的行为。
Claims (5)
1.一种高温X8R型陶瓷电容器介质材料，其特征在于：其以100重量份的钛酸钡和钛酸铋钠钡的共融物为主基料，添加0.8～3.0份的铌锰和A的氧化物的共融物、0.2～1.0份的硅锂共融物、0.6～2.5份的硼钡共融物、0.5～2.0份的Re2O3；
其中，元素A为钴(Co)、镍(N i)、锌(Zn)、铋(Bi)的一种或几种，元素Re为稀土元素镨(Pr)、钐(Sm)、钆(Gd)、钕(Nd)、镝(Dy)的一种或几种；
所述的钛酸钡和钛酸铋钠钡的共融物的化学式为:
[(1-x)BaTiO3-xBay(NaO.5Bi0.5)(1-y)TiO3]，其中，x＝0.005～0.03；y＝0.02～0.1；
所述铌锰和A的氧化物的共融物中，铌与锰的原子比为6-11，铌与元素A的原子比为4.5-8.5；
所述硅锂共融物中,Li/Si原子比＝2-4；
所述硼钡共融物中,Ba/B原子比＝0.25-0.5。
2.一种高温X8R型陶瓷电容器介质材料的制备方法，其特征在于，包括以下步骤：
步骤1，先合成钛酸铋钠钡后再合成钛酸钡和钛酸铋钠钡的共融物；
步骤2，合成铌锰和A的氧化物的共融物；
步骤3，合成硅锂共融物；
步骤4，合成硼钡共融物；
步骤5，根据权利要求1的原料配比分别称量步骤1-4制备的共融物，以水为分散介质，依次进行球磨、干燥、破碎并造粒，造粒后的粉料在2～10Mpa条件下压制成圆片生坯，然后在空气气氛中升温至1100～1190℃，并保温烧结1～4h，即制得高温X8R型陶瓷电容器介质材料。
3.根据权利要求2所述的高温X8R型陶瓷电容器介质材料的制备方法，其特征在于：所述步骤1中：
合成钛酸铋钠钡[Bay(NaO.5Bi0.5)(1-y)TiO3]，按化学式[Bay(Na0.5Bi0.5)(1-y)TiO3],以Ba(OH)2·8H2O、Na2CO3、Bi2O3、TiO2原料，进行配料、球磨、干燥、破碎、过40目标准筛网，然后在850～950℃条件下煅烧1～4h合成钛酸铋钠钡。
4.根据权利要求2或3所述的高温X8R型陶瓷电容器介质材料的制备方法，其特征在于：所述步骤1中：
合成钛酸钡和钛酸铋钠钡的共融物[(1-x)BaTiO3-xBay(NaO.5Bi0.5)(1-y)TiO3]，按化学式[(1-x)BaTiO3-xBay(Na0.5Bi0.5)(1-y)TiO3]，把合成的钛酸铋钠钡Bay(NaO.5Bi0.5)(1-y)TiO3添加到BaTiO3中进行配料、球磨、干燥、破碎、过40目标准筛网，然后在1020～1150℃条件下煅烧2～6h合成钛酸钡和钛酸铋钠钡的共融物。
5.根据权利要求2所述的高温X8R型陶瓷电容器介质材料的制备方法，其特征在于：所述步骤5中，球磨工艺采用2～5mm的氧化锆球作磨介，研磨2～10h，然后烘干、过筛，再加入5～10重量份的石蜡做粘结剂共同烘焙造粒，并再次过筛。
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