CN1473139A - 低温烧成瓷器及其电子部件 - Google Patents

低温烧成瓷器及其电子部件 Download PDF

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Publication number
CN1473139A
CN1473139A CNA028027957A CN02802795A CN1473139A CN 1473139 A CN1473139 A CN 1473139A CN A028027957 A CNA028027957 A CN A028027957A CN 02802795 A CN02802795 A CN 02802795A CN 1473139 A CN1473139 A CN 1473139A
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mentioned
weight
composition
converted
fired porcelain
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CN100396644C (zh
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大m武志
大渕武志
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NGK Insulators Ltd
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NGK Insulators Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/018—Dielectrics
    • H01G4/06—Solid dielectrics
    • H01G4/08—Inorganic dielectrics
    • H01G4/12—Ceramic dielectrics
    • H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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    • B32B2311/02—Noble metals
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/40—Metallic
    • C04B2237/407—Copper
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/40—Metallic
    • C04B2237/408—Noble metals, e.g. palladium, platina or silver

Abstract

本发明的低温烧成瓷器，用强力X射线衍射装置测定时作为主结晶相含有硅钡石相、钡长石相及β－方晶石相，α－方晶石相的(101)面的最大强度与硅钡石相的(101)面的最大强度的比率在5％以下。这种瓷器可在析出方晶石相的硅酸铝－氧化钡系的低温烧成瓷器中降低瓷器内的裂纹发生率。

Description

低温烧成瓷器及其电子部件
技术领域
本发明涉及低温烧成瓷器及用该瓷器的电子部件。
背景技术
在移动电话等高频电路无线设备中，作为高频电路滤波器，例如作为高端滤波器、发送用级间滤波器、局部滤波器、接收用级间滤波器等，使用叠层式电介质滤波器。这样的电介质叠层滤波器的例子如特开平5-243810号公报所揭示。
为制造电介质叠层式滤波器，要多次制作构成电介质的陶瓷粉末的成形体，对于各成形体，要涂敷规定的导电膏剂，从而将规定的电极图形制成各成形体。然后将各成形体层叠起来得到叠层体。通过将此叠层体进行烧成，同时烧成导电膏剂层和各成形体，使之致密化。
这种情况下，电极一般使用银系导体、铜系导体、镍系导体这样的低熔点金属导体，它们的熔点在例如1100℃以下，甚至有的低至930℃以下。因此，就必须用比构成电极的低熔点金属还低的烧成温度使电介体烧结。
为了降低杂散电容，减少滞后时间，降低内装谐振器及电容器的高频损失，最好降低低温烧成瓷器的介电常数εr，且使质量系数Q增加。本申请人在特开2000-211969号公报中揭示了有1000℃以下的最适合烧成温度，介电常数εr在10以下，质量系数Q在2500以上的低温烧成瓷器。此瓷器是硅酸铝—氧化钡系，使强度高的钡长石相析出。
发明内容
将低温烧成瓷器应用于内装谐振器和电容器时，就必须使瓷器和内层电极、外装电极之间的热膨胀系数一致，为此一般必须控制瓷器或电极的线膨胀率。为控制硅酸铝—氧化钡系低温烧成瓷器的线膨胀率，控制SiO2单相(例：方晶石、石英、鳞石英)的含有率是有效的。但是，判明了在使瓷器中析出方晶石相和进行电镀工序及无铅电镀的时候瓷器上发生裂纹，有增加不良品的倾向。
本发明的课题是，对析出方晶石相的硅酸铝—氧化钡系的低温烧成瓷器，要能降低瓷器内的裂纹发生率。
本发明的低温烧成瓷器的特征是：用强X射线衍射装置测定时作为结晶相含有硅钡石相、钡长石相及β-方晶石相，α-方晶石相的(101)面的最大强度与硅钡石相的(101)面的最大强度的比率在5％以下。
而且，本发明的低温烧成瓷器的特征是：含有钡成分和锌成分的至少一种、硅成分及铝成分，将钡成分和锌成分的合计量换算成BaO和ZnO为46.0～56.0重量％，将硅成分含量换算成SiO2为39.0～47.0重量％，将铝成分含量换算成Al2O3为0.5～10.0重量％。
还有，本发明的电子部件的特征是：至少一部分由上述低温烧成瓷器构成。
本发明者对于上述瓷器内的裂纹发生状况探讨的结果，得出以下观点。即，在瓷器上例如涂布了金属膏剂的状态下在850～1000℃的温度下烧结。此时，由于在烧结后的瓷器内析出方晶石相，故降低瓷器的线膨胀率。此后，在金属电极上进行镀层和无铅焊锡。此时的温度远远低于低温烧成瓷器的一般的烧结温度(850～1000℃)，故不易考虑到给瓷器内的裂纹产生带来影响。但是，实际上，在烧结生成瓷器后的比较低的温度下的工艺过程对裂纹的发生影响很大。
本发明者对裂纹的原因探讨的结果，发现方晶石相的相变态的影响。方晶石相一般在300℃以上的高温下是稳定的β-方晶石相，在低温下是稳定的α-方晶石相。β-方晶石相一般为高温相，但可以认为在低温烧成瓷器内受其它的结晶粒子的约束，因此向α-方晶石相的相转变受到阻碍。
在处理此瓷器时，可以认为在200～300℃的温度范围内，比较少量的α-方晶石相向β-方晶石相转变，此时，结果引起了线膨胀率的变化。一般，可以认为伴随相转变的线膨胀率的变化依赖于相转变速度。相转变速度大的场合(相转变速度快的场合)，即使相转变产生的结晶相是少量的，在其相转变前后也会引起急剧的线膨胀率的增减。但是，定量地测定相转变的速度显然是很困难的，也没有明确的理论。况且，预测特定的瓷器系特定的结晶相的相转变速度的事例至今未报导。因此，在本发明的瓷器系中，预测比较少量的α-方晶石相向β-方晶石相相转变的速度乃至瓷器的线膨胀率的增减是困难的。
对于本发明的作为结晶相含有硅钡石相、钡长石相及β-方晶石相的低温烧成瓷器，由于α-方晶石相的(101)面的最大强度与硅钡石相的(101)面的最大强度的比率在5％以下，故可防止上述瓷器内产生裂纹。
本发明瓷器的各结晶相如下：
硅钡石相(BaSi2O5)具有JCPDS卡的第26-0176号X射线衍射的最大值。
钡长石相(BaAl2Si2O8)具有JCPDS卡的第38-1450号X射线衍射的最大值。
β-方晶石相(SiO2)具有JCPDS卡的第27-0605号X射线衍射的最大值。
α-方晶石相(SiO2)具有JCPDS卡的第39-1425号X射线衍射的最大值。
本发明的X射线衍射图表及最大强度按以下条件测定。
X射线衍射装置名称：RIGAKU制“PINT2500”
管球：Cu
管电压：50KV
管电流：300mA
单色光仪：入射侧Ge
发散狭缝：1/2deg
散射狭缝：1/2deg
受光狭缝：0.15mm
步长：0.02deg
记数时间：7.00sec
具体实施方式
α-方晶石相的(101)面的最大强度与硅钡石相的(101)面的最大强度的比率最好在4％以下，2％以下则更好。还有，α-方晶石相的表面最大强度低于检测界限尤其好。
钡长石相的(-220)面的最大强度与硅钡石相的(101)面的最大强度的比率最好为1％以上，或者为20％以下。
硅钡石相、钡长石相、β-方晶石相的合计最好占全部结晶相的90重量％以上，占95重量％以上则更好。
硅钡石相、钡长石相、β-方晶石相及α-方晶石相以外的结晶相最好在后述的测定条件中低于检测界限。
本发明的低温烧成瓷器中，将硅成分换算成SiO2最好含有20重量％以上，由此可以将介电常数控制在10以下。从进一步降低介电常数的观点出发，将硅成分换算成SiO2最好含有30重量％以上。而且，将硅成分换算成SiO2最好含有80重量％以下，由此能够降低瓷器的最适宜烧成温度。从此观点出发，含有65重量％以下则更好。
本发明的低温烧成瓷器中，将铝成分换算成Al2O3最好含有0.1重量％以上，由此不仅可以在瓷器中增加强度高的钡长石相，而且还可以将由瓷器构成的基板的强度提高到2000Kg/cm2以上。从此观点出发，将铝成分换算成Al2O3最好含有2.0重量％以上。而且，从降低瓷器烧成温度的观点出发，将铝成分换算成Al2O3最好含有20重量％以下，含15重量％以下则更好。
本发明的低温烧成瓷器中，将钡成分换算成BaO最好含有10重量％以上，由此可进一步提高瓷器的质量系数Q。从此观点出发，将钡成分换算成BaO最好含有30重量％以上。而且，将钡成分换算成BaO最好含有64重量％以下，据此可以确保10以下的介电常数εr。从进一步降低介电常数εr的观点出发，将钡成分换算成BaO含有60重量％以下则更好。
通过将锌成分换算成ZnO含有0.5重量％以上(最好是2.0重量％以上)，使低温烧成瓷器的线膨胀率减小，易于烧结，故可以低温烧成。将锌成分换算成ZnO含有20重量％以下(最好是15重量％以下)，可以使瓷器的质量系数Q进一步提高。
本发明特别理想的组成如下，据此特别容易抑制α-方晶石相的析出。
(钡成分和上述锌成分的合计量)
换算成BaO及ZnO为46.0～56.0重量％(最好是48.0重量％以上，49.5重量％以上更好。或者，最好是54.0重量％以下，52.5重量％以下更好)。
(钡成分的量)
最好是BaO为40重量％以上(更好的是42重量％以上)。最好是BaO为51重量％以下(更好的是49重量％以下)。
(锌成分的量)
最好是ZnO为1.0重量％以上，或10.0重量％以下。
(硅成分的量)
将硅成分的含量换算成SiO2为39.0～47.0重量％(最好是39.5重量％以上。而且，最好是41.0重量％以下，40.5重量％以下则更好)。
(铝成分的量)
将铝成分的含量换算成Al2O3为0.5～10.0重量％(最好是1.0重量％以上，2.0重量％以上更好，或者最好是5.0重量％以下，4.0重量％以下则更好)。
在优选实施形式中，将Bi2O3(瓷器成分)和含B2O3的低熔点玻璃一起使用，这样，可以使瓷器的质量系数Q提高，并进一步抑制瓷器的裂纹。
将硼成分换算成B2O3为含有1.5重量％以下，由此可以使瓷器的质量系数Q达到2500以上。从使瓷器的质量系数Q增大的观点出发，将硼成分换算成B2O3最好含有1.0重量％以下，含有0.9重量％以下则更好。而且，将硼成分换算成B2O3为含有0.3重量％以上，则可以在低温下烧成瓷器。将硼成分换算成B2O3最好含有0.5重量％以上，含0.6重量％以上更好。
含有铋成分则减少瓷器裂纹的发生率。此作用效果对于本发明的瓷器在使金属电极层叠的场合，或在使金属电极与瓷器成形体接触的状态下烧成瓷器成形体的场合，或将金属电极埋设于瓷器成形体中的状态下烧成瓷器成形体的场合是显著的。在含有铋成分的情况下，铋成分的量能够用荧光X射线分析法检出即可。但最好是将铋成分的含量换算成Bi2O3为0.1重量％以上，为0.5重量％以上则更好，为1.0重量％以上(尤其是1.5重量％以上，特别是2.0重量％以上)则特别理想。
将铋成分换算成Bi2O3含有20重量％，则可以更进一步增大质量系数Q。由此观点出发，为15重量％以下最好，为10重量％以下则更好。将铋成分换算成Bi2O3含有7.0重量％以下很理想，含有6.0重量％以下则更加理想。
本发明的瓷器不仅实质上可以由钡成分、硅成分、铝成分等构成，而且实质上也可以由钡成分、硅成分、铝成分、硼成分、锌成分及铋成分构成。但是，在这些场合，也允许含有含在各金属原料中的不可避免的杂质。而且，也允许含有上述成分以外的氧化物或金属成分。这种氧化物或金属成分有，例如：MgO、CaO、SrO、Y2O3、V2O5、MnO、Mn2O3、CoO、NiO、Nd2O3、Sm2O3、La2O3、CuO、Ag、Cu、Ni、Pd。
作为本发明的对象的电子部件没有特别的限定，可以是例如：叠层由介体滤波器、多层配线基板、电介体天线、电介体偶合器、电介体复合模块。
本发明的电子部件中，最好是低温烧成瓷器接合在电子部件之外的部件上。对之外的部件没有限定，但最好是电介体层、磁性体层、压电体层或金属电极。
可以用于电子部件的金属电极没有限定，但最好是银电极、铜电极、镍电极，或者是由它们的合金或它们的混合物构成的电极，由银、银合金、银和其它金属的混合物构成的电极更好，银电极则特别理想。
而且，在金属电极上，可以设镀层及/或焊锡层。作为镀层的成分，可以是例如Ni、Sn。作为焊锡层的成分，可以是例如：Sn-Pb、Sn-Pb-Ag、Sn-Pb-Sb、Sn-Pb-In-Sb-Ag、Sn-Pb-Ag-Cu、Sn-Zn-In、Sn-Ag、Sn-Ag-Bi-Cu、Sn-Ag-Cu、Sn-Cu、Sn-Sb-Ag-Cu、Sn。
本发明的电子部件中，可以将本发明的低温烧成瓷器和介电常数εr为10～150的其它的低温烧成瓷器形成一体。
这样的瓷器的组成体系没有限定，但最好是以下的组成系。BaO-TiO2-ZnO-SiO2-B2O3BaO-TiO2-Bi2O3-Nd2O3-ZnO-SiO2-B2O3BaO-TiO2-Bi2O3-La2O3-Sm2O3-ZnO-SiO2-B2O3MgO-CaO-TiO2-ZnO-Al2O3-SiO2-B2O3
构成磁性体层的磁性体可以例示以下组成。MnO-ZnO-Fe2O3-CuO；MnO-ZnO-Fe2O3-CuO-SiO2；MnO-ZnO-Fe2O3-CuO-Ta2O5；MnO-ZnO-Fe2O3-CuO-SiO2-Ta2O5；NiO-ZnO-Fe2O3；MnO-ZnO-Fe2O3；MnO-ZnO-Fe2O3-Bi2O3-MoO3；NiO-CuO-ZnO。
构成压电体层的压电体可以例示以下组成。PbO-ZrO2-TiO2；PbO-ZrO2-TiO2-Sb2O3；K2O-Na2O-Li2O-Nb2O5-Ta2O5-Bi2O3；PbO-CoO-Nb2O3-ZrO2-TiO2；PbO-MgO-Nb2O3-Yb2O3-TiO2-ZrO2；BaO-TiO2。
在制造本发明的低温烧成瓷器的时候，最好是将各金属成分的原料按规定比率混合而得到混合粉末，将混合粉末在850～1200℃下煅烧，粉碎煅烧体，得到陶瓷粉末。而且，最好是用陶瓷粉末和由SiO2、B2O3及ZnO构成的玻璃粉末制作生片，再将生片在850～930℃下烧成。作为各金属成分的原料，可以使用各金属的氧化物、硝酸盐、碳酸盐、硫酸盐等。
实施例
(陶瓷粉末的制造)
将碳酸钡、氧化铝、氧化硅、氧化锌、氧化铋的各粉末按规定的组成称量，并进行湿法混合。将此混合粉末在900～1000℃下煅烧，得到煅烧体。为了调查煅烧物的结晶相和其结晶性，对粉末进行X射线衍射测定。之后，将煅烧的粉末在球磨机中粉碎至规定的粒度，将粉末干燥，得到陶瓷粉末。
(玻璃粉末的制造)
将氧化锌、氧化硼及氧化硅各粉末称量，进行干法混合，使混合粉末在白金坩埚中熔融，将熔融物投入水中迅速冷却，得到块状玻璃。将此玻璃进行湿法粉碎，得到低熔点的玻璃粉末。
(介电特性评价用试样的制造)
将得到的陶瓷粉末和玻璃粉末与离子交换水、有机粘合剂一起，用氧化铝钵、氧化铝球进行混合，得到生料，将生料干燥，得到粉体。将得到的粉体在金属模压力机中成形出规定的形状，在900～930℃下烧成，测定按3GHz换算的介电常数εr。
(裂纹评价用试样的制造)
将得到的陶瓷粉末和玻璃粉末与有机粘合剂、可塑剂、分散剂及有机溶剂一起，用氧化铝钵、氧化铝球进行湿法混合，得到生片成形用生料。将此生料用刮刀片装置制成厚0.03～2mm的各生片。
(裂纹的评价)
用Ag-Pt(Pt1重量％)膏剂将电容器电极图形和谐振器电极图形用丝网印刷方法印在各生片上，将各生片层叠规定片数，得到叠层体，用切块机切成11mm×8mm×3mm的形状，在850～930℃下烧成2小时得到烧结体。然后，将烧结体洗净，进行电解电镀，接着在锡中性液中进行电解电镀。将得到的试料洗净。对此试料，评价裂纹的有无。有无裂纹的确认用超声波探伤装置(日立建机股份有限公制的“マイスコ-プ”)，根据从裂纹部分传来的超声波回波反射的图象数据判断。分别对100个试料测定，不良品的发生个数表示在表中。
(X射线衍射峰值的测定)
对各瓷器试料，按上述条件测定X射线衍射峰值。而且，将α-方晶石相的(101)面的最大强度与硅钡石相的(101)面的最大强度的比率表示在表1～4中。将硅钡石相、钡长石相、β-方晶石相、α-方晶石相以外的结晶相的有无表示在表4中。而且，适当的烧成温度为，介电常数εr的变化相对于烧成温度的变化在0.1/℃以内的温度。
(与外装电极的线膨胀率差)
用热膨胀计测定外装电极及实验试料的各线膨胀率(250℃)，得到线膨胀率之差。
(实验结果)
以上的实验中，将各金属的比例按表1～表4所示作了种种变更。并对各实验试料测定了上述各特性，列于表1～表4。
                                                                    表1
  BaO+ZnO   SiO2   Al2O3   Bi2O3   B2O3   α-方晶石相的最大强度与硅钡石相的最大强度的比率(％)   β-方晶石相的最大强度与硅钡石相的最大强度的比率(％)   与外装电极的线膨胀系数差(250℃；ppm/℃)     裂纹发生数    适当烧成温度范围(℃)
    A1   45.5   47.5   3.0   3.4   0.6      12     20      3.2    86/100     880～930
    A2   46.0   47.0   1.0   5.2   0.8      5     13      1.2    2/100     880～930
    A3   48.0   39.0   5.0   7.0   1.0      2     10      0.8    0/100     880～930
    A4   49.5   39.5   4.0   6.5   0.5      小于检测界限值     8      0.5    0/100     880～930
    A5   51.0   40.0   3.0   5.2   0.8      小于检测界限值     6      0.4    0/100     880～930
    A6   52.5   40.5   3.0   3.3   0.7      小于检测界限值     4      0.5    0/100     880～930
    A7   54.0   41.0   1.5   2.6   0.9      小于检测界限值     3      0.6    0/100     880～930
    A8   56.0   39.0   2.0   2.0   1.0      小于检测界限值     2      1.0    1/100     880～930
    A9   56.5   38.0   2.4   2.5   0.6      小于检测界限值     小于检测界限值      1.7    19/100     880～930
                                                                        表2
  BaO+ZnO   SiO2    Al2O3   Bi2O3    B2O3   α-方晶石相的最大强度与硅钡石相的最大强度的比率(％)  β-方晶石相的最大强度与硅钡石相的最大强度的比率(％)   与外装电极的线膨胀系数差(250℃；ppm/℃)     裂纹发生数     适当烧成温度范围(℃)
    B1   52.5   40.5    0.2   6.2    0.6   小于检测界限值     4      0.7     0/100     830～870
    B2   51.3   40.4    0.5   7.0    0.8   小于检测界限值     5      0.5     0/100     850～890
    B3   52.5   41.7    1.0   3.8    1.0   小于检测界限值     6      0.6     0/100     880～930
    B4   50.7   43.5    2.0   3.3    0.5   小于检测界限值     5      0.5     0/100     880～930
    B5   51.0   42.2    3.0   3.1    0.7   小于检测界限值     4      0.6     0/100     880～930
    B6   52.5   40.5    4.0   2.1    0.9   小于检测界限值     5      0.5     0/100     880～930
    B7   49.5   39.5    5.0   5.2    0.8   小于检测界限值     4      0.7     0/100     880～930
    B8   46.2   40.0    10.0   3.1    0.7   小于检测界限值     2      1.0     2/100     880～930
    B9   47.2   39.0    11.0   2.0    0.8   小于检测界限值     小于检测界限值      1.8     23/100     880～930
                                                                       表3
   BaO+ZnO    SiO2  Al2O3   Bi2O3   B2O3   α-方晶石相的最大强度与硅钡石相的最大强度的比率(％) β-方晶石相的最大强度与硅钡石相的最大强度的比率(％)   与外装电极的线膨胀系数差(250℃；ppm/℃)     裂纹发生数    适当烧成温度范围(℃)
    C1    53.4    40.5  5.0   0.5   0.6   小于检测界限值     6   0.5    0/100     850～900
    C2    52.8    42.7  3.0   1.0   0.5   小于检测界限值     6   0.4    0/100     860～910
    C3    51.6    41.7  4.0   1.5   0.7   小于检测界限值     6   0.5    0/100     880～930
    C4    50.4    43.7  1.0   2.0   0.9   小于检测界限值     6   0.3    0/100     880～930
    C5    51.2    40.1  3.0   5.0   0.7   小于检测界限值     6   0.4    0/100     880～930
    C6    49.2    40.5  4.0   6.0   0.8   小于检测界限值     5   0.4    0/100     880～930
    C7    49.5    39.5  3.0   7.0   1.0   小于检测界限值     5   0.4    0/100     880～930
    C8    46.3    40.0  3.0   10.0   0.7   小于检测界限值     5   0.5    0/100     890～940
    C9    47.2    39.0  2.0   11.0   0.8   小于检测界限值     6   0.4    0/100     900～950
                                                                                表4
  BaO+ZnO    SiO2   Al2O3   Bi2O3   B2O3   α-方晶石相的最大强度与硅钡石相的最大强度的比率(％) β-方晶石相的最大强度与硅钡石相的最大强度的比率(％)  与外装电极的线膨胀系数差(250℃；ppm/℃)     裂纹发生数  目的以外的结晶相   适当烧成温度范围(℃)
    D1   51.2    40.5   4.0   4.1   0.2   小于检测界限值    7     0.5     0/100     无   850～900
    D2   52.9    42.0   1.0   3.8   0.3   小于检测界限值    7     0.4     0/100     无   860～910
    D3   52.5    41.7   3.0   2.3   0.5   小于检测界限值    6     0.5     0/100     无   880～930
    D4   50.7    43.5   1.0   4.2   0.6   小于检测界限值    6     0.3     0/100     无   880～930
    D5   50.2    41.4   5.0   2.7   0.7   小于检测界限值    6     0.3     0/100     无   880～930
    D6   51.0    39.0   4.0   5.2   0.9   小于检测界限值    5     0.4     0/100     无   880～930
    D7   51.6    39.5   3.0   4.9   1.0   小于检测界限值    5     0.4     0/100     无   890～940
    D8   51.0    43.0   2.0   2.5   1.5   小于检测界限值    5     0.5     0/100     无   900～950
    D9   50.2    39.8   5.0   3.0   2.0   小于检测界限值    6     0.3     0/100     无   930～970
对于表1的各试料，主要使(BaO+ZnO)及(SiO2)的量变化。并且，成功地将α-方晶石相的(101)面的最大强度与硅钡石相的(101)面的最大强度的比率(以下，称上述比率)控制在5％以下。其结果，确认了通过将上述比率控制在5％以下，能够减少与250℃下的外装电极的热膨胀差，可以抑制形成外装电极后的裂纹。
对于表2的各试料，主要使Al2O3的量变化。而且，确认了通过将上述比率控制在5％以下，能够减少与250℃下的外装电极的热膨胀差，可以抑制形成外装电极后的裂纹。在B1中，适当烧成温度范围向低温侧移动。
对于表3的各试料，主要使Bi2O3的量变化。而且，确认了通过将上述比率控制在5％以下，能够减少与250℃下的外装电极的热膨胀差，可以抑制形成外装电极后的裂纹。在C1中，适当烧成温度范围向低温侧移动。在C9中，适当烧成温度范围向高温侧移动。
对于表4的各试料，主要使B2O3的量变化。而且，确认了通过将上述比率控制在5％以下，能够减少与250℃下的外装电极的热膨胀差，可以抑制形成外装电极后的裂纹。在D1中，适当烧成温度范围向低温侧移动。在D9中，适当烧成温度范围向高温侧移动。
总之，由于和由Cu及Ag构成的内层电极同时烧成的温度的适当范围是880℃～930℃，故本实施例的瓷器的适当烧成温度范围最好也在880℃～930℃的范围内。由此观点来看，本实施例的瓷器也适合于电子部件的用途。
如上所述，根据本发明，在析出方晶石相的硅酸铝-氧化钡系的低温烧成瓷器中，能降低瓷器内的裂纹发生率。

Claims (20)

1.一种低温烧成瓷器，其特征在于：用强力X射线衍射装置测定时作为结晶相含有硅钡石相、钡长石相及β-方晶石相，α-方晶石相的(101)面的最大强度与上述硅钡石相的(101)面的最大强度的比率在5％以下。
2.根据权利要求1记载的低温烧成瓷器，其特征在于：上述α-方晶石相的(101)面的最大强度低于检测界限。
3.根据权利要求1或2记载的低温烧成瓷器，其特征在于：上述硅钡石相、上述钡长石相、上述β-方晶石相及上述α-方晶石相以外的结晶相低于检测界限。
4.根据权利要求1～3中任一项记载的低温烧成瓷器，其特征在于：含有
将钡成分换算成BaO为10～64重量％，
将硅成分换算成SiO2为20～80重量％，
将铝成分换算成Al2O3为0.1～20重量％，
将硼成分换算成B2O3为0.3～1.0重量％，
将锌成分换算成ZnO为0.5～20重量％，
将铋成分换算成Bi2O3为20重量％以下。
5.根据权利要求1～3中任一项记载的低温烧成瓷器，其特征在于：
含有钡成分和锌成分中的至少一种、硅成分及铝成分，
将上述钡成分和上述锌成分的合计量换算成BaO和ZnO为46.0～56.0重量％，
将上述硅成分含量换算成SiO2为39.0～47.0重量％，
将上述铝成分含量换算成Al2O3为0.5～10.0重量％。
6.根据权利要求5记载的低温烧成瓷器，其特征在于：将上述钡成分和上述锌成分的合计量换算成BaO和ZnO为48.0～54.0重量％，
将上述硅成分含量换算成SiO2为39.0～41.0重量％，
将上述铝成分含量换算成Al2O3为1.0～5.0重量％。
7.根据权利要求5或6记载的低温烧成瓷器，其特征在于：含有将硼成分换算成B2O3为0.3～1.5重量％，以及将铋成分换算成Bi2O3为1.0～10.0重量％。
8.根据权利要求7记载的低温烧成瓷器，其特征在于：实质上是由上述钡成分、上述硅成分、上述铝成分、上述硼成分、上述锌成分以及上述铋成分构成。
9.根据权利要求4、7或8记载的低温烧成瓷器，其特征在于：使用含B2O3的玻璃和含Bi2O3的陶瓷作为初始原料制得。
10.根据权利要求9记载的低温烧成瓷器，其特征在于：上述玻璃是含有SiO2、B2O3及ZnO的玻璃。
11.一种低温烧成瓷器，其特征在于：含有钡成分和锌成分的至少一种、硅成分及铝成分，
将上述钡成分和上述锌成分的合计量换算成BaO和ZnO为46.0～56.0重量％，
将上述硅成分含量换算成SiO2为39.0～47.0重量％，
将上述铝成分含量换算成Al2O3为0.5～10.0重量％。
12.根据权利要求11记载的低温烧成瓷器，其特征在于：
将上述钡成分和上述锌成分的合计量换算成BaO和ZnO为48.0～54.0重量％，
将上述硅成分含量换算成SiO2为39.0～41.0重量％，
将上述铝成分含量换算成Al2O3为1.0～5.0重量％。
13.根据权利要求11或12记载的低温烧成瓷器，其特征在于：含有将硼成分换算成B2O3为0.3～1.5重量％，以及将铋成分换算成Bi2O3为1.0～10.0重量％。
14.根据权利要求13记载的低温烧成瓷器，其特征在于：实质上是由上述钡成分、上述硅成分、上述铝成分、上述硼成分、上述锌成分及上述铋成分构成。
15.根据权利要求13或14记载的低温烧成瓷器，其特征在于：使用含B2O3的玻璃和含Bi2O3的陶瓷作为初始原料制得。
16.根据权利要求15记载的低温烧成瓷器，其特征在于：上述玻璃是含有SiO2、B2O3及ZnO的玻璃。
17.根据权利要求11～16中任一项记载的低温烧成瓷器，其特征在于：用强力X射线衍射装置测定时作为主结晶相含有硅钡石相、钡长石相及β-方晶石相，α-方晶石相的(101)面的最大强度与上述硅钡石相的(101)面的最大强度的比率在5％以下。
18.根据权利要求17记载的低温烧成瓷器，其特征在于：上述α-方晶石相的(101)面的最大强度低于检测界限。
19.一种电子部件，其特征在于：由权利要求1～18的任一项权利要求中记载的低温烧成瓷器构成至少一部分。
20.根据权利要求19记载的电子部件，其特征在于：上述低温烧成瓷器与上述电子部件的其它构件接合，上述其它构件是介电体层、磁性体层、压电体层或金属电极。
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JP3741556B2 (ja) 1999-01-22 2006-02-01 日本碍子株式会社 低温焼成磁器およびこれを備えた電子部品
JP3838541B2 (ja) * 2001-03-09 2006-10-25 日本碍子株式会社 低温焼成磁器および電子部品

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CN101679104B (zh) * 2007-02-28 2014-12-17 欧罗克拉公司 含铋玻璃、玻璃-陶瓷、制品和制造方法
TWI594971B (zh) * 2014-07-09 2017-08-11 菲洛公司 介電糊料組成物及形成電子組件之方法
CN110423116A (zh) * 2019-07-24 2019-11-08 桂林理工大学 一种x7r型陶瓷电容器介质材料及其制备方法
CN110423116B (zh) * 2019-07-24 2021-07-02 桂林理工大学 一种x7r型陶瓷电容器介质材料及其制备方法
CN111175324A (zh) * 2020-01-07 2020-05-19 中钢洛耐新材料科技有限公司 一种分析线起止角度在测量α-石英相含量中的应用

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