CN101646633A - 尖晶石烧结体、其制造方法、透明基板和液晶投影仪 - Google Patents
尖晶石烧结体、其制造方法、透明基板和液晶投影仪 Download PDFInfo
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Abstract
本发明提供组成为MgO·nAl2O3(1.05≤n≤1.30)、Si元素的含量为20ppm以下的尖晶石烧结体及其制造方法,该制造方法具备以下工序:由Si元素的含量为50ppm以下、纯度为99.5质量%以上的尖晶石粉末形成成型体的工序;通过在真空中在1500℃~1700℃下对成型体进行烧结,形成密度95%以上的烧结体的第一烧结工序;和在1600℃~1800℃下对烧结体进行加压烧结的第二烧结工序。
Description
技术领域
本发明涉及透明性及其稳定性优良的尖晶石烧结体及其制造方法。另外,本发明还涉及由该尖晶石烧结体构成的透明基板和具备该透明基板的液晶投影仪。
背景技术
尖晶石烧结体是晶型为不具有偏振性的立方晶、在氧化物陶瓷中具有较高的导热性、在从中红外区域到可见区域显示出透明性的材料,因此,作为液晶投影仪或背投影电视机等各种电子设备等的偏振片或防尘窗等透光窗或者透镜等透明基板材料而备受瞩目。
图2表示液晶投影仪的一般结构。如图2所示,从金属卤化物灯或氙灯等光源1投射来的光由反射板2反射,透过紫外线截止滤光片3等后,被导入积分仪偏振转换光学系统4中。接着,通过根据光的波长进行透射和反射的分色镜5分解为红(R)、绿(G)、蓝(B)各原色,利用全反射镜6,使各分解光分别通过偏振片7和防尘窗8,在交叉二向色棱镜9中合成后,通过投射透镜系统10进行扩大,在前方的屏幕上投影出图像11。对于具有这种结构的液晶投影仪用的偏振片或防尘窗等透光窗或者透光透镜等透明基板的材料,即使是具有厚度的原材,也要求稳定的高透光率。
例如,报道有Al2O3和MgO的组成比为0.53∶0.47~0.58∶0.42的范围、且在厚度为1mm时的波长600nm的光线的线性透射率为75%以上的多晶透明尖晶石烧结体(参照日本特开昭59-121158号公报(专利文献1))。但是,该尖晶石烧结体的波长600nm的光线的最高线性透射率为约84%以下,且波长450nm的光线的线性透射率低,因此,虽然能在中红外区域内使用,但难以在要求高透射特性的可见区域内利用。
另外,报道有将纯度为99.5%以上、比表面积为10m2/g以上的尖晶石粉末在真空中在1200℃~1700℃下热压后,进行HIP(Hot IsostaticPressing,热等静压加工法)的透光性尖晶石烧结体的制造方法(参照日本特开平02-018354号公报(专利文献2))。根据该方法制造的尖晶石烧结体在波长3μm~5μm的红外区域显示出最高85%的线性透射率,但是,波长0.4μm~3μm的光线的线性透射率平均为75%,因此,该尖晶石烧结体也难以在要求高透光特性的可见区域内利用。
另一方面,报告有将纯度为99.9%以上的尖晶石粉末预成型后,进行热压,对得到的尖晶石烧结体进行HIP的透明多晶体的制造方法(参照日本特开2005-070734号公报(专利文献3))。该透明多晶体的波长400nm~800nm的光线的线性透射率平均为84%,但是,该尖晶石烧结体的透射性存在偏差,根据测定试样的不同线性透射率为80%以下等,烧结体的稳定性存在问题。另外,烧结体的厚度为10mm以上时,中心部产生非均相,存在线性透射率降低的问题。
专利文献1:日本特开昭59-121158号公报
专利文献2:日本特开平02-018354号公报
专利文献3:日本特开2005-070734号公报
发明内容
本发明是鉴于上述现状而完成的,其目的在于,提供具有对波长350nm~450nm的可见光线也能充分使用的80%以上的线性透射率、并能得到稳定的高透射率的尖晶石烧结体。另外,提供即使用具有厚度的原材也能够得到对可见区域的光线具有稳定的高透射率的尖晶石烧结体及其制造方法。另外,提供由上述尖晶石烧结体构成的液晶投影仪用透明基板及具备该透明基板的液晶投影仪。
本发明的尖晶石烧结体的组成为MgO·nAl2O3(1.05≤n≤1.30),Si元素的含量为20ppm以下。该烧结体优选下述形态:在厚度为1mm时的波长350nm~450nm的光线的线性透射率为80%以上。
本发明提供一种尖晶石烧结体的制造方法,所述尖晶石烧结体的组成为MgO·nAl2O3(1.05≤n≤1.30)、Si元素的含量为20ppm以下,所述制造方法具备以下工序:由Si元素的含量为50ppm以下、纯度为99.5质量%以上的尖晶石粉末形成成型体的工序;通过在真空中在1500℃~1700℃下对成型体进行烧结,形成密度95%以上的烧结体的第一烧结工序;和在1600℃~1800℃下对烧结体进行加压烧结的第二烧结工序。
通过第一烧结工序形成的烧结体能够使Si元素的含量为20ppm以下。另外,第一烧结工序优选下述形式:在50Pa以下的压力下进行,并且当设从烧结体的中心部到烧结体的外侧的最小厚度为D(mm)、从1000℃升温到最高温度为止的升温时间为t分钟时,具有如下关系:
D=a×t1/2
1≤a≤3
本发明的透明基板由尖晶石烧结体构成,适合作为液晶投影仪用透明基板,特别优选表面具有涂层的形态。本发明的液晶投影仪的特征在于,具备该透明基板和发出可见光线的光源。
发明效果
本发明能够提供具有对可见光线也能充分使用的稳定的透光性的尖晶石结构的烧结体。另外,由于透光性高,因此,由来自光源的光造成的热吸收也少,能够对液晶的升温进行散热。根据该特性,作为液晶投影仪用透明基板有用。
附图说明
图1是表示波长350nm的光线的线性透射率与Si元素的含量的关系的图。
图2是表示液晶投影仪的一般结构的图。
符号说明
1光源、2反射板、3紫外线截止滤光片、4积分仪偏振变换光学系统、5分色镜、6全反射镜、7偏振片、8防尘窗、9交叉二向色棱镜、10投射透镜系统、11图像。
具体实施方式
(尖晶石烧结体)
本发明的尖晶石烧结体的组成为MgO·nAl2O3(1.05≤n≤1.30),Si元素的含量为20ppm以下。该尖晶石烧结体在厚度1mm时的波长350nm~450nm的可见光线的线性透射率优选为80%以上,更优选为82%以上,特别优选为84%以上,线性透射率足够高。另外,能够得到稳定的高透射率,偏差小。并且,即使用具有厚度的材料,也能得到对可见光线的稳定的高透射率。因此,适合作为包括发光二极管、激光设备、液晶投影仪、背投影电视机或数字微镜器件等发光装置用的偏振片或防尘窗等透光窗、或者透光透镜在内的透明基板的材料。因此,具备本发明的透明基板的液晶投影仪,对来自光源的可见光线的线性透射率高,照度不均小。
线性透射率是与入射光线的光轴平行的直线上的透射光的强度相对于入射光的强度的比率,可以使用CCD进行测定。因此,对各波长的光线的线性透射率越高,得到的透射光越强,透过的透镜或透射窗所吸收的光能越少,因此,能够抑制透镜或透射窗的发热。
尖晶石烧结体中含有组成为MgO·nAl2O3(1.05≤n≤1.30)、由MgO(氧化镁)和Al2O3(氧化铝)组成的氧化物。尖晶石烧结体由于晶型为立方晶,因此,晶界处不易发生光的散射,烧结成高密度时,能够得到良好的透光性。通过使1.05≤n≤1.30,能够减少MgO的固溶量,减小微观上的晶格的偏差和变形,改善透光性。从该观点考虑,优选1.07≤n≤1.125。
通常,使尖晶石烧结体的透光性降低的因素有金属杂质的混入,作为金属杂质,可以列举Si、Ti、Na、K、Ca、Fe、C等。这些金属杂质来自于原料粉末,并混入烧结体中。这些金属杂质中,通过使Si元素的含量为20ppm以下,能够稳定地得到高透光性。从该观点考虑,Si元素的含量更优选10ppm以下,特别优选5ppm以下。通过如此控制Si元素的含量,即使在厚度10mm以上的尖晶石烧结体中也能得到均匀的透光性。Si元素在烧结时与尖晶石粉末反应而生成液相。该液相具有促进尖晶石粉末的烧结性的效果,但如果该液相残留在晶界上,则成为非均相,使透光率降低。
由于Si元素以外的金属杂质例如包括Na、K、Ca或Fe等在内的杂质的混入,尖晶石烧结体的透光性、透光性的偏差及制造上的稳定性会受到不良影响。因此,尖晶石粉末中的MgO·nAl2O3的纯度设定为99.5质量%以上,优选99.9质量%以上,更优选99.99质量%以上。
由尖晶石烧结体构成的液晶投影仪用透明基板,从提高透光性和表面稳定性的观点考虑,优选表面具有涂层的形态。涂层即使为单层也有效,但是,从在通常使用的波长400nm~700nm的区域得到稳定的透射特性的观点考虑,更优选具有多层涂层的形态。设置多个涂层时,涂布材料优选SiO2、TiO2、Al2O3、Y2O3、Ta2O5、ZrO2等金属氧化物或MgF2、YF3、LaF3、CeF3、BaF2等金属氟化物。该涂层的膜厚优选总计5μm以下。单面上具有如此得到的涂层的尖晶石烧结体的平均透射率,在波长400nm~700nm的区域优选90%以上,更优选91%以上,特别优选92%以上。
(尖晶石烧结体的制造方法)
本发明的尖晶石烧结体的制造方法具备:由Si元素的含量为50ppm以下、纯度为99.5质量%以上的尖晶石粉末形成成型体的工序;通过在真空中在1500℃~1700℃下对成型体进行烧结,形成密度95%以上的烧结体的第一烧结工序;和在1600℃~1800℃下对烧结体进行加压烧结的第二烧结工序。根据该方法,能够制造组成为MgO·nAl2O3(1.05≤n≤1.30),Si元素的含量为20ppm以下的尖晶石烧结体,能够提供具有稳定的高透光率、且透光率的偏差小的透镜或透光窗。
首先,通过冲压成型或CIP(Cool Isostatic Pressing,冷等静压加工法)使尖晶石粉末成型。然后,在第一烧结工序中,在真空中在1500℃~1700℃下对成型体进行烧结,形成密度95%以上的烧结体。通过在真空气氛中进行烧结,能够使由作为杂质的Si元素生成的液相在真空中蒸发而除去。从该观点考虑,真空度优选50Pa以下,更优选20Pa以下。
第一烧结工序的条件因Si元素的量和烧结体的厚度而异,但优选下述方式:当设从烧结体的中心部到烧结体的外侧的最小厚度为D(mm),从1000℃升温到最高温度为止的升温时间为t分钟时,具有如下关系:
D=a×t1/2
1≤a≤3
由后述的实施例2的结果表明,通过在这样的范围内升温,当尖晶石粉末中的Si元素的含量为50ppm以下时,在第一烧结工序结束后,能够使Si元素的含量降低到20ppm以下,从而能够得到高透光率的尖晶石烧结体。从进一步降低烧结体中的Si元素含量、提高尖晶石烧结体的透光率的观点考虑,尖晶石粉末中的Si元素含量优选30ppm以下。当尖晶石粉末中的Si元素的含量为50ppm以上时,通过进一步延长第一烧结工序中在真空气氛中的升温时间,能够降低烧结体中的Si元素含量。
另外,从得到密度95%以上的高密度烧结体的观点考虑,第一烧结工序中的温度优选1500℃以上。从提高烧结体的透光率的观点考虑,烧结体的密度更优选95%以上。本说明书中,密度是指根据阿基米德法计算出的相对密度。另一方面,从抑制真空中的MgO的蒸发、防止冷却时Al2O3作为第二相析出、维持高透光性的观点考虑,烧结温度优选1700℃以下,更优选1650℃以下。
第一烧结工序结束后,在第二烧结工序中,通过HIP等在1600℃~1800℃下对烧结体进行加压烧结。在温度1600℃~1800℃、压力约100MPa下进行HIP时,通过塑性变形和扩散机制促进空孔的去除,因此,能够更加高密度化,进一步提高透光率。HIP中使用的气体优选Ar气、N2气等惰性气体、O2气或这些气体的混合气体,混合O2气时,能够防止脱氧造成的透光性的降低。
在透明基板的表面形成涂层优选利用物理蒸镀法的方式,可以实施溅射法、离子镀膜法、真空蒸镀法等。进行离子辅助或等离子体辅助时,涂膜性能提高,因此优选。
(实施例1~7)
本实施例中,在50ppm以下对作为原料的尖晶石粉末中的Si元素的含量进行各种变更,形成尖晶石烧结体后,研究透光率。首先,使用纯度为99.5质量%、杂质元素含量如表1所示的尖晶石粉末,成型后,通过CIP加工为Φ95mm×L95mm。然后,在1℃/分钟的升温条件下,在压力为20Pa的真空中,在1600℃下实施第一烧结工序。所得烧结体的密度为95%~97%。
第一烧结工序的升温条件为:从烧结体的中心部到烧结体的外侧的最小厚度D为39mm,从1000℃升温到最高温度1600℃为止以1℃/分钟进行升温,因此升温时间t为600分钟。因此,根据D=a×t1/2,计算出a为1.6,满足1≤a≤3。
然后,使用Ar气,在1700℃、100MPa下进行HIP,实施第二烧结工序。所得烧结体为Φ82mm×L78mm,通过ICP发射光谱分析(Inductively Coupled Plasma Atomic Emission Spectometry,电感耦合等离子体原子发射光谱法)可知组成为MgO·1.07Al2O3,1.05≤n≤1.30。切割该烧结体的中央部后,进行研磨,使用分光光谱仪(日立高新技术公司制U-4100)测定厚度1mm时的波长350nm和450nm的光线的线性透射率。另外,将其中心部粉碎,通过ICP发射光谱分析测定Si元素的含量。测定结果示于表1。
由表1的结果表明,使用Si元素的含量为50ppm以下的尖晶石粉末,通过本发明的方法,能够制造组成为MgO·nAl2O3(1.05≤n≤1.30)、Si元素的含量为20ppm以下的尖晶石烧结体。另外,尖晶石烧结体的线性透射率均为80%以上,可知透光率的偏差小。
表1
(实施例8~10和参考例1)
本实施例中,改变第一烧结工序中的升温时间t(D一定),研究由D=a×t1/2求出的a值与Si元素含量及烧结体的透光性的关系。
使用实施例5中使用的尖晶石粉体,通过在第一烧结工序中不改变D值而改变升温时间t,使a的值如表2所示那样变化,其它条件与实施例5相同,制造尖晶石烧结体。与实施例5同样地进行测定,测定通过第一烧结工序形成的烧结体的Si元素含量和第二烧结工序结束后的烧结体的线性透射率。测定结果示于表2。
表2
由表2的结果表明,在满足1≤a≤3的情况下,当尖晶石粉末中的Si元素的含量为50ppm以下时,第一烧结工序结束后,能够使Si元素的含量降低至20ppm以下,且尖晶石烧结体的线性透射率均为80%以上。
将实施例2和4及参考例1的尖晶石烧结体沿厚度方向每隔5mm进行切割,将各试样加工成厚度1mm,对波长350nm的光线的线性透射率与Si元素的含量的关系进行测定。其结果示于图1。由图1的结果表明,Si元素的含量多的试样,线性透射率的偏差大,与此相对,Si元素的含量为20ppm以下的试样,表现出稳定的高透射特性。
本次公开的实施方式及实施例从任何角度来说都应视为例示性而非限制性的。本发明的范围如权利要求书所示而不受上述说明的限制,并包含权利要求等效物的含义和范围内的所有变更。
产业实用性
本发明的尖晶石烧结体具有稳定的高透光性,因此,适合作为发光二极管、激光设备、液晶投影仪、背投影电视机或数字微镜器件等发光装置用的透光窗或者透光透镜的材料。
Claims (8)
1.一种尖晶石烧结体,其组成为MgO·nAl2O3,Si元素的含量为20ppm以下,其中1.05≤n≤1.30。
2.如权利要求1所述的尖晶石烧结体,其中,所述烧结体在厚度为1mm时的波长350nm~450nm的光线的线性透射率为80%以上。
3.由权利要求1所述的尖晶石烧结体构成的液晶投影仪用透明基板。
4.如权利要求3所述的透明基板,其中,所述基板的表面具有涂层。
5.一种液晶投影仪,其具备权利要求3所述的透明基板和发出可见光线的光源。
6.一种尖晶石烧结体的制造方法,所述尖晶石烧结体的组成为MgO·nAl2O3,Si元素的含量为20ppm以下,其中1.05≤n≤1.30,所述制造方法具备以下工序:
由Si元素的含量为50ppm以下、纯度为99.5质量%以上的尖晶石粉末形成成型体的工序;
通过在真空中在1500℃~1700℃下对所述成型体进行烧结,形成密度95%以上的烧结体的第一烧结工序;和
在1600℃~1800℃下对所述烧结体进行加压烧结的第二烧结工序。
7.如权利要求6所述的尖晶石烧结体的制造方法,其中,通过第一烧结工序形成的所述烧结体的Si元素的含量为20ppm以下。
8.如权利要求6所述的尖晶石烧结体的制造方法,其中,所述第一烧结工序在50Pa以下的压力下进行,并且
当设从烧结体的中心部到烧结体的外侧的最小厚度为D,从1000℃升温到最高温度为止的升温时间为t分钟时,具有如下关系:
D=a×t1/2
1≤a≤3,
其中,所述厚度D的单位为mm。
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CN102947246A (zh) * | 2010-06-22 | 2013-02-27 | 住友电气工业株式会社 | 基板、基板的制造方法及发光元件 |
CN102947246B (zh) * | 2010-06-22 | 2015-11-25 | 住友电气工业株式会社 | 基板、基板的制造方法及发光元件 |
TWI510449B (zh) * | 2010-06-22 | 2015-12-01 | Sumitomo Electric Industries | Manufacturing method of light emitting element |
CN106232552A (zh) * | 2014-05-30 | 2016-12-14 | 住友电气工业株式会社 | 液晶触摸面板保护板 |
CN106575055A (zh) * | 2014-09-12 | 2017-04-19 | 住友电气工业株式会社 | 液晶显示器保护板及液晶显示器保护板的制造方法 |
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JP2008214123A (ja) | 2008-09-18 |
WO2008108276A1 (ja) | 2008-09-12 |
TW200914392A (en) | 2009-04-01 |
EP2116519A4 (en) | 2011-03-09 |
JP4830911B2 (ja) | 2011-12-07 |
EP2116519A1 (en) | 2009-11-11 |
US20100103356A1 (en) | 2010-04-29 |
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