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CN107226690B - 含有多铝红柱石的烧结体、其制法及复合基板 - Google Patents

含有多铝红柱石的烧结体、其制法及复合基板 Download PDF

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Publication number
CN107226690B
CN107226690B CN201710156213.7A CN201710156213A CN107226690B CN 107226690 B CN107226690 B CN 107226690B CN 201710156213 A CN201710156213 A CN 201710156213A CN 107226690 B CN107226690 B CN 107226690B
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mullite
sintered body
less
substrate
powder
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CN107226690A (zh
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矶田佳范
铃木能大
井上胜弘
胜田祐司
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NGK Insulators Ltd
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NGK Insulators Ltd
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Abstract

本发明涉及一种含有多铝红柱石的烧结体、其制法及复合基板。本发明的含有多铝红柱石的烧结体除了含有多铝红柱石以外，还含有从由氮化硅、氮氧化硅及硅铝氧氮陶瓷构成的组中选择的至少1种。该含有多铝红柱石的烧结体优选40～400℃下的热膨胀系数低于4.3ppm/℃，开口气孔率为0.5％以下，平均结晶粒径为1.5μm以下。

Description

含有多铝红柱石的烧结体、其制法及复合基板
技术领域
本发明涉及含有多铝红柱石的烧结体、其制法及复合基板。
背景技术
多铝红柱石烧结体通常是将氧化铝(Al2O3)和氧化硅(SiO2)以3比2的比例烧结而得到的耐热冲击性优异的材料，用3Al2O3·2SiO2表示。作为该多铝红柱石烧结体，例如专利文献1中所公开那样，已知将在多铝红柱石粉末中混合30质量％的三氧化二钇稳定氧化锆(YSZ)粉末而得到的粉末成型，使该成型体烧结而得到的多铝红柱石烧结体。专利文献1中，从多铝红柱石烧结体上切出多铝红柱石基板，对该多铝红柱石基板的主表面进行研磨，由此，制成用于与GaN基板贴合的基底基板。GaN的热膨胀系数在室温至1000℃的范围内为6.0ppm/K，多铝红柱石的热膨胀系数为5.2ppm/K。因此，如果考虑将两者贴合使用，则希望提高多铝红柱石的热膨胀系数而使其接近于GaN基板的热膨胀系数，因此，在多铝红柱石粉末中混合YSZ粉末并使其烧结。
另一方面，专利文献2中记载有如下例子：将包含钽酸锂、铌酸锂等的功能性基板和多铝红柱石烧结体制支撑基板通过直接接合进行接合，得到复合基板，将该复合基板利用于弹性表面波元件等弹性波器件。该弹性波器件中，作为支撑基板的多铝红柱石基板的热膨胀系数低至4.4ppm/℃(40～400℃)左右，杨氏模量高达220GPa以上，因此，能够减小弹性波器件自身因温度变化而出现的膨胀、收缩，从而，使频率的温度依赖性得到大幅改善。为了将功能性基板和支撑基板直接接合，要求各接合面具有高的平坦性。例如专利文献2中记载：中心线平均粗糙度Ra优选为3nm以下。
现有技术文献
专利文献
专利文献1：日本特许第5585570号公报
专利文献2：日本特许第5861016号公报
发明内容
然而，虽然专利文献1中记载有在多铝红柱石中加入相当量的其它成分来提高热膨胀系数的多铝红柱石烧结体，专利文献2中记载有多铝红柱石的纯度较高的多铝红柱石烧结体，但是，没有涉及到降低了热膨胀系数的多铝红柱石烧结体，甚至不知道其是这种低热膨胀的多铝红柱石烧结体且抛光面的表面平坦性高。另外，在将低热膨胀、但低刚性的多铝红柱石烧结体用作复合基板的支撑基板的情况下，复合基板有时也会因少许的温度差而翘曲。
本发明是为了解决该课题而完成的，其主要目的是使含有多铝红柱石的烧结体与多铝红柱石单体相比，热膨胀系数降低并且刚性提高，并且，提高研磨面的平坦性。
本发明的含有多铝红柱石的烧结体除了含有多铝红柱石以外，还含有从由氮化硅、氮氧化硅及硅铝氧氮陶瓷构成的组中选择的至少1种，其中，40～400℃下的热膨胀系数低于4.3ppm/℃，开口气孔率为0.5％以下，平均结晶粒径(烧结粒子的平均粒径)为1.5μm以下。该含有多铝红柱石的烧结体与多铝红柱石单体相比，热膨胀系数低且刚性高。另外，能够提高研磨面的平坦性。
本发明的含有多铝红柱石的烧结体的制法包括以下工序：(a)将平均粒径1.5μm以下的多铝红柱石粉末50～90体积％和平均粒径1μm以下的氮化硅粉末10～50体积％按合计为100体积％进行混合，得到混合原料粉末；(b)将所述混合原料粉末成型为规定形状的成型体，将所述成型体以压制压力20～300kgf/cm2、烧成温度1525～1700℃进行热压烧成，由此，得到含有多铝红柱石的烧结体。该制法适合于制造上述的本发明的含有多铝红柱石的烧结体。应予说明，粉末的平均粒径是通过激光衍射法测定得到的值(以下相同)。
本发明的复合基板是将功能性基板和支撑基板接合而得到的复合基板，其中，所述支撑基板为上述的含有多铝红柱石的烧结体。该复合基板由于作为支撑基板的含有多铝红柱石的烧结体的研磨面的平坦性高，因此，与功能性基板良好地接合。另外，将该复合基板利用于弹性表面波器件的情况下，频率温度依赖性得到大幅改善。另外，即便在光波导器件、LED器件、开关器件中，支撑基板的热膨胀系数也较小，由此，性能得到提高。
附图说明
图1是含有多铝红柱石的烧结体的制造工序图。
图2是复合基板10的立体图。
图3是使用复合基板10制作得到的电子器件30的立体图。
符号说明
10-复合基板、12-压电基板、14-支撑基板、30-电子器件、32、34-IDT电极、36-反射电极。
具体实施方式
以下，对本发明的实施方式具体地进行说明，但是，本发明并不限定于以下的实施方式，应当理解为：基于本领域技术人员的通常知识，在不脱离本发明的主旨的范围内，可以适当进行变更、改良等。
本实施方式的含有多铝红柱石的烧结体除了含有多铝红柱石以外，还含有从由氮化硅、氮氧化硅及硅铝氧氮陶瓷构成的组中选择的至少1种。多铝红柱石优选为烧结体中包含最多的成分(主成分)，但是从上述组中选择的成分也可以为主成分。该含有多铝红柱石的烧结体优选在40～400℃下的热膨胀系数低于4.3ppm/℃，开口气孔率为0.5％以下，平均结晶粒径为1.5μm以下。该含有多铝红柱石的烧结体与多铝红柱石单体相比，热膨胀系数低且杨氏模量(刚性)高。另外，该含有多铝红柱石的烧结体的开口气孔率为0.5％以下，几乎没有气孔，平均结晶粒径低至1.5μm以下，因此，抛光面(研磨面)的平坦性提高。
本实施方式的含有多铝红柱石的烧结体优选研磨面的每100μm×100μm面积中存在的最大长度1μm以上的气孔的数量为10个以下。如果气孔的数量为10个以下，则抛光面的平坦性进一步提高。该气孔的数量更优选为3个以下，进一步优选为零。
本实施方式的含有多铝红柱石的烧结体的杨氏模量优选为240GPa以上，4点弯曲强度优选为300MPa以上。氮化硅及源自于氮化硅的成分的杨氏模量、强度比多铝红柱石高，因此，通过调整氮化硅相对于多铝红柱石的添加比例，能够使含有多铝红柱石的烧结体的杨氏模量为240GPa以上，并使4点弯曲强度为300MPa以上。应予说明，4点弯曲强度更优选为320MPa以上。
本实施方式的含有多铝红柱石的烧结体优选研磨面的中心线平均粗糙度Ra为1.5nm以下。作为被用于弹性波器件等的复合基板，已知有将功能性基板和支撑基板接合得到的复合基板，但是，通过像这样将研磨面的Ra为1.5nm以下的含有多铝红柱石的烧结体用作支撑基板，支撑基板与功能性基板的接合性变得良好。例如接合界面中实际接合的面积的比例(接合面积比例)为80％以上(优选为90％以上)。研磨面的中心线平均粗糙度Ra更优选为1.1nm以下，进一步优选为1.0nm以下。
本实施方式的含有多铝红柱石的烧结体在40～400℃下的热膨胀系数更优选为3.8ppm/℃以下。通过将以该含有多铝红柱石的烧结体为支撑基板的复合基板用于弹性波器件，在弹性波器件的温度上升的情况下，功能性基板的热膨胀比原来的热膨胀小，因此，弹性波器件的频率温度依赖性得到改善。在40～400℃下的热膨胀系数进一步优选为3.5ppm/℃以下。
接下来，对本发明的含有多铝红柱石的烧结体的制造方法的一个实施方式进行说明。如图1所示，含有多铝红柱石的烧结体的制造流程包括以下工序：(a)调制混合原料粉末；(b)制作含有多铝红柱石的烧结体。
·工序(a)：混合原料粉末的调制
通过将多铝红柱石粉末和氮化硅粉末混合来调制混合原料粉末。作为多铝红柱石原料，优选使用纯度高且平均粒径小的粉末。纯度优选为99.0％以上，更优选为99.5％以上，进一步优选为99.8％以上。纯度的单位是质量％。另外，平均粒径(D50)优选为1.5μm以下，更优选为0.1～1.5μm。多铝红柱石原料可以使用市售品，也可以使用采用高纯度的氧化铝、二氧化硅粉末制作得到的物质。作为制作多铝红柱石原料的方法，例如可以举出专利文献2中记载的方法。作为氮化硅原料，优选使用平均粒径小的粉末。平均粒径优选为1μm以下，更优选为0.1～1μm。关于多铝红柱石原料与氮化硅原料的混合比例，例如可以将多铝红柱石原料50～90体积％(优选为70～90体积％)和氮化硅原料10～50体积％(优选为10～30体积％)按合计为100体积％进行称量，用罐式球磨机等混合机进行混合，根据需要用喷雾干燥器进行干燥，得到混合原料粉末。
·工序(b)：含有多铝红柱石的烧结体的制作
将工序(a)中得到的混合原料粉末成型为规定形状的成型体。对于成型方法没有特别限制，可以使用一般的成型法。例如可以将混合原料粉末直接通过模具压制成型。压制成型的情况下，如果将混合原料粉末预先通过喷雾干燥法制成颗粒状，则成型性变得良好。此外，可以加入有机粘合剂，制作生坯而进行挤压成型，或者制作浆料而进行片成型。这些工艺中，必须在烧成工序前或者烧成工序中除去有机粘合剂成分。另外，还可以利用CIP(冷等静压制)进行高压成型。
接下来，将得到的成型体烧成，制作含有多铝红柱石的烧结体。此时，从提高含有多铝红柱石的烧结体的表面平坦性方面考虑，优选维持烧结粒子较为微细，并在烧结中排出气体。作为其方法，热压法非常有效。通过使用该热压法，与常压烧结相比，在低温下以微细粒的状态进行致密化，能够抑制在常压烧结中常见的粗大气孔的残留。该热压时的烧成温度(最高温度)优选为1525～1700℃。另外，热压时的压制压力优选为20～300kgf/cm2。由于特别低的压制压力能够使热压夹具小型化且长寿命化，因此优选。关于在烧成温度下的保持时间，可以考虑成型体的形状、大小、加热炉的特性等，适宜地选择适当的时间。具体的优选保持时间例如为1～12小时，更优选为2～8小时。对于烧成气氛也没有特别限制，热压时的气氛一般为氮、氩等不活泼气氛。升温速度、降温速度只要考虑成型体的形状、大小、加热炉的特性等适当设定即可，只要在例如50～300℃/hr的范围设定即可。
接下来，对本发明的复合基板的一个实施方式进行说明。本实施方式的复合基板是将功能性基板和上述的含有多铝红柱石的烧结体制支撑基板接合得到的。该复合基板的两个基板的接合面积比例增大，表现出良好的接合性。作为功能性基板，没有特别限定，例如可以举出：钽酸锂、铌酸锂、氮化镓、硅等。接合方法优选直接接合。直接接合的情况下，对功能性基板和支撑基板各自的接合面进行研磨后，活化，在使两个接合面相对的状态下按压两个基板。接合面的活化例如除了对接合面照射不活泼气体(氩等)的离子束以外，通过照射等离子、中性原子束等来进行。功能性基板与支撑基板的厚度比(功能性基板的厚度/支撑基板的厚度)优选为0.1以下。图2中示出复合基板之一例。复合基板10是通过直接接合将作为功能性基板的压电基板12和支撑基板14接合得到的。
本实施方式的复合基板可用于电子器件等。作为该电子器件，除了弹性波器件(弹性表面波器件、兰姆波元件、薄膜谐振器(FBAR)等)以外，还可以举出：LED器件、光波导器件、开关器件等。弹性波器件中利用上述的复合基板的情况下，作为支撑基板的含有多铝红柱石的烧结体的热膨胀系数低至小于4.3ppm/K(40～400℃)，因此，频率温度依赖性得到大幅改善。图3中示出使用复合基板10制作得到的电子器件30之一例。电子器件30是单端口SAW谐振器亦即弹性表面波器件。首先，使用一般的光刻技术，在复合基板10的压电基板12上形成多个电子器件30的图案，然后，通过切割切成一个一个的电子器件30。电子器件30通过光刻技术在压电基板12的表面形成有IDT(Interdigital Transducer)电极32、34和反射电极36。
应予说明，本发明不受上述的实施方式任何限定，只要属于本发明的技术范围，当然可以以各种方式进行实施。
实施例
1.混合原料粉末的制作
作为多铝红柱石原料，使用市场上销售的纯度99.9％以上、平均粒径1.5μm的多铝红柱石粉末，作为氮化硅原料，使用市场上销售的纯度97％以上、平均粒径0.8μm的氮化硅粉末。将多铝红柱石原料和氮化硅原料以表1的实验例1～3中所示的比例进行称量，使用
Figure BDA0001247083860000061
的氧化铝球石以罐式球磨机进行混合，通过喷雾干燥法制作混合原料粉末。
表1
Figure BDA0001247083860000071
2.含有多铝红柱石的烧结体的制作
将实验例1～3的混合原料粉末放入直径约125mm的模具中，以200kgf/cm2的压力成型为厚度10～15mm左右的圆盘状，得到含有多铝红柱石的成型体。接下来，将含有多铝红柱石的成型体收纳于内径约125mm的热压用石墨模具中，利用热压炉制作直径约125mm且厚度5～8mm左右的含有多铝红柱石的烧结体。应予说明，使烧成时的最高温度(烧成温度)为1650℃，使烧成温度下的保持时间为5hr，使升温速度、降温速度均为100℃/hr。在升温过程中达到900℃以上时使压制载荷为200kgf/cm2，炉内气氛是：抽真空直至达到900℃，达到900℃后，导入N2，在N2下进行烧结。在烧成温度下保持规定时间后，降温至1200℃，停止对压制载荷和炉内气氛的控制，自然冷却至室温。另外，实验例4中，仅以多铝红柱石粉末同样地制作成型体、烧结体。
3.特性评价
从实验例1～4的烧结体上切出试验片(4×3×40mm尺寸的抗折棒等)，评价各种特性。另外，烧结体的研磨面是通过研磨将4×3×10mm左右的试验片的一面精加工成镜面状而得到的。以3μm的金刚石磨粒、0.5μm的金刚石磨粒依次进行研磨，最终精加工时，使用0.1μm以下的金刚石磨粒，进行精研。评价的特性如下。
(1)结晶相
将烧结体粉碎，利用X射线衍射装置进行结晶相的鉴定。测定条件为CuKα、50kV、300mA、2θ＝5－70°，使用旋转对阴极型X射线衍射装置(理学电机制RINT)。
(2)结晶相比率
由上述(1)的X射线衍射图谱，计算出各结晶相的峰面积比率。以多铝红柱石(210)晶面(2θ＝26.2°)的峰面积为1，使各结晶相的峰面积相对于多铝红柱石(210)晶面(2θ＝26.2°)的峰面积的比为结晶相比率。此处，作为各结晶相的代表峰，氮化硅使用(101)晶面(2θ＝20.6°)，硅铝氧氮陶瓷使用Si2Al3O7N的(3－20)晶面(2θ＝24.6°)及Si5AlON7的(200)晶面(2θ＝26.9°)。
(3)体积密度、开口气孔率
使用抗折棒，利用采用了纯水的阿基米德法来测定体积密度、开口气孔率。
(4)杨氏模量
以依据JIS R1602的静态挠度法进行测定。试验片形状为3mm×4mm×40mm抗折棒。
(5)弯曲强度
依据JIS R1601，测定4点弯曲强度。试验片形状为3mm×4mm×40mm抗折棒或者其一半大小。
(6)热膨胀系数(40～400℃)
依据JIS R1618，以推杆式示差热膨胀计测定。试验片形状为3mm×4mm×20mm。
(7)气孔的数量
以SEM观察如上所述精加工后的烧结体的研磨面，计量每100μm×100μm中存在的最大长度为1μm以上的气孔的数量。
(8)表面平坦性(Ra)
使用AFM，针对如上所述精加工后的烧结体的研磨面测定中心线平均粗糙度Ra。测定范围为10μm×10μm。
(9)烧结粒子的平均粒径
利用磷酸对如上所述精加工后的烧结体的研磨面进行化学蚀刻，以SEM测定200个以上烧结粒子的大小，使用线段法计算出平均粒径。线段法的系数为1.5，将以SEM实测的长度乘以1.5得到的值作为平均粒径。
(10)接合性
从实验例1～4的烧结体上切出直径100mm、厚度600μm左右的圆板。如上所述对该圆板进行抛光后，进行清洗，除去表面的粒子(particle)、污染物质等。接下来，以该圆板为支撑基板，实施支撑基板与功能性基板的直接接合，得到复合基板。即，首先，通过氩的离子束将支撑基板和功能性基板各自的接合面活化，然后，使两个接合面相对，以10tonf进行按压，接合而得到复合基板。作为功能性基板，使用铌酸锂(LN)基板。接合性的评价如下：根据IR透射图像，将接合面积比例为90％以上的复合基板评价为“最佳”，将接合面积比例为80％以上且低于90％的复合基板评价为“良”，将接合面积比例低于80％的复合基板评价为“差”。
4.评价结果
实验例1～3的含有多铝红柱石的烧结体是将多铝红柱石原料和氮化硅原料混合制成混合原料粉末，将该混合原料粉末烧成而得到的，但是，氮化硅的一部分因烧成而变化为硅铝氧氮陶瓷。实验例1～3的含有多铝红柱石的烧结体包含氮化硅等，因此，与实验例4的多铝红柱石单体的烧结体相比，杨氏模量及4点弯曲强度得到提高。即，杨氏模量提高到240GPa以上，4点弯曲强度提高到320MPa以上。另外，实验例1～3的含有多铝红柱石的烧结体在40～400℃下的热膨胀系数低于4.3ppm/℃(3.5～4.1ppm/℃)，其值比实验例4的多铝红柱石单体的烧结体低。此外，实验例1～3的含有多铝红柱石的烧结体及实验例4的多铝红柱石单体的烧结体的开口气孔率为0.5％以下(低于0.1％)、平均结晶粒径为1.5μm以下(1.0～1.2μm)，因此，研磨面的中心线平均粗糙度Ra低至1.1nm以下(0.9～1.1nm)。因此，将从实验例2～4的烧结体上切出的圆板与功能性基板直接接合时的接合性均为接合面积比例在90％以上的“最佳”，将从实验例1的烧结体上切出的圆板与功能性基板直接接合时的接合性为接合面积比例在80％以上且低于90％的“良”。应予说明，研磨面的中心线平均粗糙度Ra为像这样小的值还有助于使气孔的数量为3个以下(零)。
应予说明，实验例1～3相当于本发明的实施例，实验例4相当于比较例。这些实验例并没有对本发明作任何限定。
本申请以2016年3月23日所申请的日本专利申请第2016－058970号为主张优先权的基础，通过引用将其全部内容都包含在本说明书当中。

Claims (7)

1.一种含有多铝红柱石的烧结体，其除了含有多铝红柱石以外，还含有氮化硅及硅铝氧氮陶瓷，其中，
40～400℃下的热膨胀系数为4.1ppm/℃以下，
开口气孔率为0.1％以下，
平均结晶粒径为1.2μm以下。
2.根据权利要求1所述的含有多铝红柱石的烧结体，其中，
研磨面的每100μm×100μm面积中存在的最大长度1μm以上的气孔的数量为10个以下。
3.根据权利要求1所述的含有多铝红柱石的烧结体，其中，
杨氏模量为240GPa以上。
4.根据权利要求1～3中的任意一项所述的含有多铝红柱石的烧结体，其中，
4点弯曲强度为320MPa以上。
5.根据权利要求1～3中的任意一项所述的含有多铝红柱石的烧结体，其中，
研磨面的中心线平均粗糙度Ra为1.5nm以下。
6.一种含有多铝红柱石的烧结体的制法，是制造权利要求1～5中的任意一项所述的含有多铝红柱石的烧结体的方法，其包括以下工序：
(a)将平均粒径1.5μm以下的多铝红柱石粉末70～90体积％和平均粒径1μm以下的氮化硅粉末10～30体积％按合计为100体积％进行混合，得到混合原料粉末；
(b)将所述混合原料粉末成型为规定形状的成型体，将所述成型体以压制压力20～300kgf/cm2、烧成温度1525～1700℃进行热压烧成，由此，得到含有多铝红柱石的烧结体。
7.一种复合基板，其是将功能性基板和支撑基板接合而得到的复合基板，其中，
所述支撑基板为权利要求1～5中的任意一项所述的含有多铝红柱石的烧结体。
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