CN1384080A - 陶瓷的制造方法 - Google Patents

陶瓷的制造方法 Download PDF

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CN1384080A
CN1384080A CN02119065A CN02119065A CN1384080A CN 1384080 A CN1384080 A CN 1384080A CN 02119065 A CN02119065 A CN 02119065A CN 02119065 A CN02119065 A CN 02119065A CN 1384080 A CN1384080 A CN 1384080A
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ceramic
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CN1226235C (zh
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小川弘纯
木村雅彦
安藤阳
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Murata Manufacturing Co Ltd
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Abstract

本发明提供一种陶瓷的制造方法,该方法在烧结中可以采用通常的烧结炉,如果采用相同的材料,可以制造取向度比采用TGG法制造的取向陶瓷的取向度高的取向陶瓷。将板状陶瓷粉末与陶瓷原料的煅烧粉末混合,得到混合粉末。然后,得到含有混合粉末、溶剂和粘合剂的陶瓷生料。将陶瓷生料成形,形成片。将层压了多个片的层压物L在模具10中沿单轴方向加压,使层压物L的与加压轴平行方向的长度比加压之前小,使层压物L的与加压轴垂直面的面积比加压之前大,形成取向成形体。烧成该取向成形体,进行烧结。

Description

陶瓷的制造方法
技术领域
本发明涉及陶瓷的制造方法，特别涉及作为例如压电体材料等电子材料使用的取向陶瓷的制造方法。
背景技术
在作为本发明背景的现有陶瓷的制造方法中，有层压陶瓷未烧结片，压接并烧结的方法。在该方法中，以不增大与加压轴垂直方向的面积的方式压制陶瓷未烧结片。采用该方法得到的陶瓷，结晶粒子不发生取向。所谓取向，表示形状异向性大的结晶粒子的方向全部一致的状态。
另一方面，目前，特别是例如作为压电体材料等电子材料使用的陶瓷，已知结晶粒子发生取向的取向陶瓷是有用的。例如，在压电体材料中，通过使Na0.5Bi4.5Ti4O15等层状钙钛矿化合物陶瓷发生取向，在圆柱状振子的厚度方向的基本振动中，机电耦合系数增大到通常的无取向陶瓷的约2.2倍，这可由T.TAKENAKA等的报告知道(Sensor andMaterials，Vol，1，35(1988))。而且，通过采用超导材料制造YBa2Cu3O7-δ的取向陶瓷，与无取向陶瓷相比，临界电流密度提高到约12倍，这是由S.Jin等报告的(Physical Review B，vol.37，No.13，7850(1988))。
目前，作为取向陶瓷的制造方法，有热铸造法和模板颗粒生长法(Templated Grain Growth)(TGG)等。
T.TAKENAKA等采用热铸造法制造Na0.5Bi4.5Ti4O15取向陶瓷。所谓热铸造法是对成形体加压的同时进行热处理(烧结)的方法。采用该方法，可以得到取向度高的取向陶瓷。这时，取向陶瓷的取向度采用Rottgering法测定，达到了98％。
另外，Seong-Hyeon Hong等采用TGG法制造Bi4(Ti3.06Nb0.04)O12的取向陶瓷。所谓TGG法，是在成形之前预先混入具有形状异向性的陶瓷结晶粒子的方法。采用这种方法，用Rottgering法测定得到的取向陶瓷的取向度为96％，压电常数d33上升到无取向陶瓷的约1.5倍(J.Am.Ceram.Soc.，vol.83，113(2000))。
如上所述，采用现有的陶瓷制造方法，得到的陶瓷的结晶粒子不发生取向。
另一方面，采用上述热铸造法和TGG法，得到的陶瓷的结晶粒子发生取向。
但是，热铸造法除了需要采用可加压烧结的特殊热处理装置之外，还是采用间歇处理的热处理的制造方法，因此，成本变高，不适合大量生产。
与此相对，TGG法由于不需要采用间歇处理的加压烧结，因此适合于大量生产。
但是，采用TGG法，与热铸造法相比，得到的陶瓷的结晶粒子的取向度低。
为了提高取向化的特性，例如提高机电耦合系数，必须实现更高的取向度。对于取向度来说，因取向化陶瓷的种类、制造条件和评价方法等的不同而不同，因此难以进行单纯的比较，但是，通常，采用TGG法与热铸造法相比，难以获得高取向的陶瓷。
在表1中，表示我们进行的采用CaBi4Ti4O15+0.5重量％MnCO3的现有的陶瓷制造方法与热铸造法、TGG法的比较结果。
                      表1
            TGG法是压延率＝1的现有方法
现有的陶瓷制造方法   热铸造法    TGG法
    取向度          0％     98％     91％
厚度滑动振动的机电耦合系数 15％ 35.1％ 30.5％
由表1可知，与现有的陶瓷制造方法相比，采用热铸造法和TGG法制造的陶瓷的结晶粒子发生取向，但是，采用TGG法制造的陶瓷与采用热铸造法制造的陶瓷相比，取向度低，特性的提高也比热铸造法的小。
发明内容
因此，本发明的主要目的是提供一种陶瓷的制造方法，该方法在烧结中可以采用通常的烧结炉，如果采用相同的材料，可以制造取向度比采用TGG法制造的取向陶瓷的取向度高的取向陶瓷。
本发明的另一目的是提供一种陶瓷的制造方法，该方法在烧结中可采用通常的烧结炉，如果采用相同的材料，可制造取向度比采用TGG法制造的取向陶瓷的取向度高且与采用热铸造法制造的取向陶瓷的取向度程度相同的取向陶瓷。
本发明的又一目的是提供一种陶瓷的制造方法，该方法在烧结中可以采用通常的烧结炉，如果采用相同的材料，可以制造取向度比采用TGG法制造的取向陶瓷的取向度高且烧结密度高的取向陶瓷。
本发明的陶瓷制造方法是包括：得到陶瓷生料的工序，该陶瓷生料含有将具有形状异向性的陶瓷结晶粒子、陶瓷原料粉末和陶瓷原料的煅烧粉末中的任意一种或者二种混合而成的混合粉末；成形陶瓷生料形成成形体的工序；在单轴方向对成形体加压，使成形体的与加压轴平行方向的长度比加压以前小，使成形体的与加压轴垂直面的面积比加压以前大，形成取向成形体的工序；和烧结取向成形体的烧结工序的陶瓷制造方法。
在本发明的陶瓷制造方法中，对于与加压轴平行方向的长度，优选取向成形体的长度为成形体长度的1/2以下。
另外，在本发明的陶瓷制造方法中，相对于混合粉末100重量％，优选具有形状异向性的陶瓷结晶粒子为25～52重量％。
而且，在本发明的陶瓷制造方法中，优选具有形状异向性的陶瓷结晶粒子是扁平状的，其最大直径与高度的比即长宽比为5～10。另外，该长宽比也是陶瓷结晶粒子的长轴尺寸与短轴尺寸的比。
另外，在本发明的陶瓷制造方法中，具有形状异向性的陶瓷结晶粒子优选具有层状钙钛矿型结晶结构。
在本发明的陶瓷制造方法中，在烧结中可采用通常的烧结炉，如果采用相同的材料，可以制造取向度比采用TGG法制造的取向陶瓷的取向度高的取向陶瓷。即，在本发明的陶瓷制造方法中，可降低陶瓷的生产成本，同时与TGG法相比，能够提高制造的陶瓷的取向度。
另外，在本发明的陶瓷制造方法中，对于与加压轴平行方向的长度，如果取向成形体的长度是成形体长度的1/2以下，可得到取向度更高的陶瓷，例如可得到与采用热铸造法得到的陶瓷的取向度相同程度的陶瓷。
而且，在本发明的陶瓷制造方法中，如果相对于混合粉末100重量％，具有形状异向性的陶瓷结晶粒子为25～52重量％，则可得到取向度高、烧结密度也高的陶瓷。
另外，在本发明的陶瓷制造方法中，如果具有形状异向性的陶瓷结晶粒子为扁平状，并且其最大直径与高度的长宽比为5～10，则可得到取向度更高的陶瓷。另外，如果该长宽比大于10，则陶瓷的密度降低。
而且，在本发明的陶瓷制造方法中，如果具有形状异向性的陶瓷结晶粒子具有层状钙钛矿型结晶构造，则取向陶瓷取向度增高的效果变得显著，可得到具有良好的压电特性的陶瓷。作为这样具有层状钙钛矿型结晶构造的物质，可举出例如BiWO6、CaBi2Nb2O9、SrBi2Nb2O9、BaBi2Nb2O9、PbBi2Nb2O9、CaBi2Ta2O9、SrBi2Ta2O9、BaBi2Ta2O9、PbBi2Ta2O9、Bi3TiNbO9、Bi3TiTaO9、Bi4Ti3O12、SrBi3Ti2NbO12、BaBi3Ti2NbO12、PbBi3Ti2NbO12、CaBi4Ti4O15、SrBi4Ti4O15、BaBi4Ti4O15、PbBi4Ti4O15、Na0.5Bi4.5Ti4O18、K0.5Bi4.5Ti4O16、Ca2Bi4Ti5O18、Sr2Bi4Ti5O18、Ba2Bi4Ti5O18、Pb2Bi4Ti5O18、Bi8Ti3WO18、Bi7Ti4NbO21、Bi10Ti3W3O30或者将这些物质多个组合的物质等。
本发明的上述目的、其它目的、特征和优点从参照附图进行的以下发明实施方案的详细说明更加清楚。
附图说明
图1是表示本发明的陶瓷制造方法一个实例的工序的图解图。
图2是表示以往陶瓷制造方法一个实例的工序的图解图。
图3是表示实施例和采用TGG法制造的样品中板状陶瓷粉末的含量和取向度的关系的曲线。
图4是表示实施例和采用TGG法制造的样品中板状陶瓷粉末的含量和密度的关系的曲线。
图5是表示实施例和采用TGG法制造的样品中长宽比与取向度的关系的曲线。
其中，10-模具，L-层压物。
具体实施方式
(实施例)
作为起始原料，准备Bi2O3、TiO2、CaCO3和MnCO3，称取这些原料，使组成为CaBi4Ti4O15+0.5重量％MnCO3，采用球磨机进行湿式混合约16小时，得到混合物。将得到的混合物干燥后，在900℃下煅烧2小时，得到陶瓷原料的煅烧粉末。然后，将煅烧粉末与NaCl混合，使之重量为1∶1，在950℃～1050℃下进行10小时的热处理(烧结)。从该烧成料中除去NaCl，得到CaBi4Ti4O15的陶瓷粉末。该陶瓷粉末采用扫描型电子显微镜可确认形状具有异向性并形成板状。另外，该板状陶瓷粉末的高度与最大直径的比即长宽比为10左右。另外，将该板状陶瓷粉末50重量份和上述煅烧粉末50重量份的混合粉末、适量的有机粘合剂、分散剂、消泡剂和表面活性剂混合，制成陶瓷生料。采用刮刀法将该陶瓷生料成形为片，得到成为成形体的片。该片的厚度为40～100μm。将该片重叠，使厚度为1.25mm、1.7mm、2mm、3.3mm，在单轴方向进行加压，同时相互粘接，制造作为取向成形体的样品。在单轴方向进行加压时，如图1所示，将重叠的片的层压物L放入模具10中后进行加压，制造样品。这时，通过调节模具10的大小，调整厚度，使1.25mm、1.7mm、2mm、3.3mm的层压物L的压延率分别为0.8、0.6、0.5、0.3，使压接后的厚度约为1mm。压延率是在将片重叠的层压物L中，加压后的厚度H1相对于加压前的厚度H0，用下式定义。
压延率＝H1/H0
为了进行比较，作为现有技术的TGG法，如图2所示，采用与片同样大小的模具1，对于上述叠合的片的层压物L，使与加压轴平行方向的长度和与加压方向垂直面的面积与加压之前相比没有变化，即压延率为1.0，将片相互粘接制造样品。
然后，将这些样品在1150℃下进行2个小时的热处理(烧成)并烧结，通过Rottgering法测定样品表面的取向度。
所谓Rottgering法是测定样品取向度的一个方法。即，将来自无取向样品的各结晶面(hk1)的反射强度作为I(hk1)，其合计为∑I(hk1)。来自其中(001)面的反射强度I(001)的合计为∑I(001)，它们的比Po用下式求出。
Po＝{∑I(001)/∑I(hk1)}
同样，对于取向样品，对反射强度求出∑I(hk1)和∑I(001)，用下式求出它们的比作为P。
P＝{∑I(001)/∑I(hk1)}
另外，采用Po和P用下式求出取向度F。
F＝{(P-Po)/(1-Po)}×100(％)
另外，为了进行比较，通过热铸造法制造与上述实施例的样品同样组成的样品。所谓热铸造法是烧成过程中对样品施加单轴压力的方法。这时，在与上述实施例中采用的煅烧粉末同样的煅烧粉末中混合有机粘合剂，采用压制成形制成直径17mm、高度8mm左右的圆柱样品。将该样品在1150℃下热处理(烧成)2个小时，在热处理过程中对样品施加全压500kg左右的单轴压力。
如上所述制造的样品的压延率与取向度的关系如表2所示。另外，上述采用热铸造法制造的样品的取向度为98％。
       表2
        *标记为本发明范围之外
    压延率     取向度(％)
     1.0*       91
     0.8       95
     0.6       96
     0.5       98
     0.3       98
如表2所示，对于本发明的任意一种样品，取向度都在95％以上。
与此相对，采用使与加压轴平行方向的长度和与加压方向垂直的面的面积与加压之前相比没有变化即压延率为1.0的TGG法，所制造的样品的取向度为91％。
另外，由表2等可知，对于本发明的样品，在压延率为0.5以下时，即对于与加压轴平行方向的长度，取向成形体的长度为成形体长度的1/2以下时，可以获得取向度与采用热铸造法得到的取向陶瓷的取向度相同程度的取向陶瓷。
另外，作为参考，取向陶瓷CaBi4Ti4O15的取向度与厚度滑动振动的机电耦合系数的关系如表3所示。
                 表3
取向度(％)   厚度滑动振动的机电耦合系数(％)
      91             30.5
      93             31.1
      95             31.9
      96             32.7
      98             33.8
由表3可知，取向陶瓷CaBi4Ti4O15，随着取向度的提高，厚度滑动振动的机电耦合系数也提高。
在上述实施例的样品中，使板状陶瓷粉末的含量为10重量％、25重量％、45重量％、50重量％、52重量％、60重量％，测定样品的取向度和密度。这时，使板状陶瓷粉末的长宽比为10，使样品的压延率为0.5。其结果如表4所示。
                     表4
  板状陶瓷粉末的含量(重量％)     取向度(％)       密度(g/cm3)
         10     60      6.9
         25     85      7.1
         45     95      7.2
         50     98      7.2
         52     98      7.15
         60     98      6.7
长宽比＝10，压延率＝0.5
而且，作为TGG法的结果，对于表4中所示结果的样品，使压延率为1.0，制造样品，测定该样品的取向度和密度。其结果如表5所示。
                    表5
  板状陶瓷粉末的含量(重量％)     取向度(％)     密度(g/cm3)
          10      47      6.8
          25      74      6.8
          45      85      7.0
          50      91      7.0
          52      91      6.95
          60      91      6.5
长宽比＝10，压延率＝1.0
另外，表4和表5表示的结果中，板状陶瓷粉末的含量与样品取向度的关系如图3的曲线所示。
由表4、表5和图3所示的曲线可知，在实施例中，与TGG法相比，样品的取向度高。
另外，由表4和图3所示的曲线可知，在实施例中，如果板状陶瓷粉末的含量在25重量％以上，可获得85％以上的取向度，如果板状陶瓷粉末的含量在45重量％以上，可获得95％以上的取向度，如果板状陶瓷粉末的含量在50重量％以上，可获得98％以上的取向度。
而且，表4和表5表示的结果中，板状陶瓷粉末的含量和样品密度的关系如图4的曲线所示。
由表4、表5和图4表示的曲线可知，在实施例中，与TGG法相比，样品的密度高。
另外，由表4和图4所示的曲线可知，在实施例中，如果板状陶瓷粉末的含量为25～52重量％，则样品的密度增大至7.1(g/cm3)以上，如果板状陶瓷粉末的含量为45～50重量％，则样品的密度进一步增大。因此，相对于混合了板状陶瓷粉末与陶瓷原料的煅烧粉末的混合粉末100重量％，板状陶瓷粉末优选为25～52重量％，板状陶瓷粉末更优选为45～50重量％。
对于上述实施例的样品，使板状陶瓷粉末的长宽比为2、4、5、10，测定样品的取向度。这时，相对于板状陶瓷粉末和陶瓷原料的煅烧粉末的混合粉末100重量％，使板状陶瓷粉末的含量为50重量％，使样品的压延率为0.5。其结果如表6所示。
           表6
    长宽比     取向度(％)
      2       70
      4       91
      5       98
      10       98
板状陶瓷粉末的含量＝50重量％，压延率＝0.5
而且，作为TGG法的结果，对于表6中所示结果的样品，使压延率为1.0，制造样品，测定该样品的取向度。其结果如表7所示。
            表7
    长宽比     取向度(％)
      2       62
      4       83
      5       91
      10       91
板状陶瓷粉末的含量＝50重量％，压延率＝1.0
另外，表6和表7表示的结果中，板状陶瓷粉末的长宽比和样品取向度的关系如图5的曲线所示。
由表6、表7和图5所示的曲线可知，在实施例中，与TGG法相比，样品的取向度高。
另外，由表6和图5所示的曲线可知，在实施例中，如果使板状陶瓷粉末的长宽比为4以上，则可获得91％以上的取向度，如果使板状陶瓷粉末的长宽比为5以上，则可获得98％以上的取向度。另外，如果其长宽比大于10，则陶瓷的密度降低。因此，板状陶瓷粉末的长宽比优选为4～10，板状陶瓷粉末的长宽比更优选为5～10。
另外，虽然在上述实施例中，混合粉末中采用了板状陶瓷粉末，但在本发明中，也可以代替板状陶瓷粉末，采用具有其它形状异向性的陶瓷结晶粒子。
而且，虽然在上述实施例中，混合粉末中采用了陶瓷原料的煅烧粉末，但在本发明中，也可以代替陶瓷原料的煅烧粉末，采用陶瓷原料的粉末，另外，也可以与陶瓷原料的煅烧粉末一起采用陶瓷原料的粉末。
另外，虽然在上述实施例中采用了压电体材料，但在本发明中并不限于压电体材料，可以采用其它材料。
而且，虽然在上述实施例中采用刮刀法形成成形体，但在本发明中，可采用挤出、各向异性加压、压延等其它成形法形成成形体。
根据本发明，在烧结中可采用通常的烧结炉，如果采用相同的材料，可以制造取向度比采用TGG法制造的取向陶瓷的取向度高的取向陶瓷。
另外，根据本发明，在烧结中可采用通常的烧结炉，如果采用相同的材料，可制造取向度比采用TGG法制造的取向陶瓷的取向度高并且与采用热铸造法制造的取向陶瓷的取向度程度相同的取向陶瓷。
而且，根据本发明，在烧结中可采用通常的烧结炉，如果采用相同的材料，可制造取向度比采用TGG法制造的取向陶瓷的取向度高且烧结密度高的取向陶瓷。

Claims (5)

1.一种陶瓷的制造方法，包括：
得到陶瓷生料的工序，该陶瓷生料含有将具有形状异向性的陶瓷结晶粒子、陶瓷原料粉末和陶瓷原料的煅烧粉末中的任意一种或二种混和形成的混合粉末；
成形上述陶瓷生料形成成形体的工序；
在单轴方向对上述成形体进行加压，使上述成形体的与加压轴平行方向的长度比加压以前小，使上述成形体的与加压轴垂直的面的面积比加压之前大，形成取向成形体的工序；和
烧结上述取向成形体的烧成工序。
2.如权利要求1记载的陶瓷制造方法，其特征在于，在与上述加压轴平行方向的长度中，上述取向成形体的长度是上述成形体长度的1/2以下。
3.如权利要求1或2记载的陶瓷制造方法，其特征在于，相对于上述混合粉末100重量％，上述具有形状异向性的陶瓷结晶粒子为25～52重量％。
4.如权利要求1至3中任意一项记载的陶瓷制造方法，其特征在于，上述具有形状异向性的陶瓷结晶粒子是扁平状的，其最大直径与高度之比即长宽比为5～10。
5.如权利要求1至4中任意一项记载的陶瓷制造方法，其特征在于，上述具有形状异向性的陶瓷结晶粒子具有层状钙钛矿型结晶结构。
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