CN105506551A - 一种用于电致变色玻璃镀膜的钨镍合金靶材的制备方法 - Google Patents
一种用于电致变色玻璃镀膜的钨镍合金靶材的制备方法 Download PDFInfo
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Abstract
本发明公开了一种用于电致变色玻璃镀膜的钨镍合金靶材的制备方法,包括如下步骤:(1)按如下重量百分比称取各组分:高纯钨粉25~55%、高纯镍粉25~55%和高纯三氧化钨粉10~25%;(2)将上述各组分置于V形混料器中混合均匀,得混合粉末;(3)将上述混合粉末置于真空热压烧结模具内,再装入真空热压烧结炉至1400~1500℃加压真空烧结保温100~150min,随炉冷却获得所述钨镍合金靶材。本发明的制备的钨镍合金靶材密度高、纯度高。
Description
技术领域
本发明属于合金靶材制备技术领域,具体涉及一种用于电致变色玻璃镀膜的钨镍合金靶材的制备方法。
背景技术
民用波音787飞机窗户或高端住宅窗户所使用的电致变色玻璃,仅通过电流的改变,就让窗户变色,从而实现光线是否可以穿过窗户达到室内或机内的作用。上述电致变色玻璃需要用钨镍合金靶材来镀膜。现有技术制备的上述钨镍合金靶材的变色作用和镀膜质量仍然不够稳定,导致电致变色玻璃的良品率偏低,成本较高。且现有的上述靶材的制备方法多产生废料废酸等污染物。
发明内容
本发明的目的在于提供一种用于电致变色玻璃镀膜的钨镍合金靶材的制备方法,其电致变色原理是W+5得电子变成W+4、失电子变成W+6从而起到变色的作用。
本发明的具体技术方案如下:
一种用于电致变色玻璃镀膜的钨镍合金靶材的制备方法,其特征在于:包括如下步骤:
(1)按如下重量百分比称取各组分:纯度≥99.999%且平均费氏粒度为1.0μm~20.0μm的钨粉25~55%、纯度≥99.95%且平均费氏粒度为1.0μm~20.0μm的镍粉25~55%和纯度≥99.95%且平均费氏粒度为1.0μm~20.0μm的三氧化钨粉10~25%;
(2)将上述各组分置于V形混料器中以15~22r/min的转速混合均匀,得混合粉末;
(3)将上述混合粉末置于真空热压烧结模具内,再装入真空热压烧结炉内以4~9℃/min速率升温至1400~1500℃的烧结温度,加压至28~37MPa,保温100~150min进行真空热压烧结,真空热压烧结加压完成后关闭加热电源随炉冷却获得密度≥99%理论密度且纯度≥99.99%的钨镍合金靶材。
在本发明的一个优选实施方案中,所述步骤(1)为:按如下重量百分比称取各组分:纯度≥99.999%且平均费氏粒度为1.0μm~20.0μm的钨粉30~50%、纯度≥99.95%且平均费氏粒度为1.0μm~20.0μm的镍粉30~50%和纯度≥99.95%且平均费氏粒度为1.0μm~20.0μm的三氧化钨粉10~20%。
在本发明的一个优选实施方案中,所述步骤(2)为:将上述各组分置于V形混料器中以20r/min的转速混合均匀,得混合粉末。
在本发明的一个优选实施方案中,所述步骤(3)中的升温速率为5~8℃/min。
在本发明的一个优选实施方案中,所述步骤(3)中的烧结温度为1400~1450℃。
在本发明的一个优选实施方案中,所述步骤(3)中加压至30~35MPa。
在本发明的一个优选实施方案中,所述步骤(3)中保温时间为120~140min。
本发明的有益效果是:
1、本发明的制备的钨镍合金靶材密度高、纯度高,用于制备电致变色玻璃的电致变色膜,使其变色作用更加稳定,镀膜质量更为良好,提高了电致变色玻璃的良品率,降低了成本;
2、本发明的镍粉的加入是为了制备出以钨镍粉末为基体配合少量三氧化钨为调节剂的新型合金粉末,用此新型合金粉末制备出钨镍合金靶材,在镀膜溅射过程中更好的与基板结合;
3、本发明的三氧化钨的加入是为了在镀膜初期,钨镍靶材具有钨的氧化物以起到调节剂的作用,从而更快的让W+5得电子变成W+4、失电子变成W+6从而起到变色的作用;
4、本发明的制备方法无污染,制备过程中不需要添加粘结剂,当温度和压力达到本发明的制备方法设定参数范围内,其中镍会出现少量液相使得烧结密度提高,同时加一定的压力可制备出高密度的钨镍合金靶材,不会产生任何废料、废酸等污染物。
附图说明
图1为本发明实施例1制备的钨镍合金靶材的微观组织图。
图2为本发明实施例2制备的钨镍合金靶材的微观组织图。
图3为本发明实施例3制备的钨镍合金靶材的微观组织图。
图4为本发明实施例4制备的钨镍合金靶材的微观组织图。
具体实施方式
以下通过具体实施方式结合附图对本发明的技术方案进行进一步的说明和描述。
实施例1
(1)按如下重量百分比称取各组分:纯度≥99.999%且平均费氏粒度为5.0μm的钨粉40%、纯度≥99.95%且平均费氏粒度为5.0μm的镍粉50%和纯度≥99.95%且平均费氏粒度为5.0μm的三氧化钨粉10%;
(2)将上述各组分置于V形混料器中以20r/min的转速混合均匀,得含高纯钨(W)质量百分比40%,镍(Ni)质量百分比50%,三氧化钨(WO3)质量百分比10%的混合粉末;
(3)将上述混合粉末置于真空热压烧结模具内,再装入真空热压烧结炉内以5℃/min速率升温至1430℃,加压至35MPa,保温120min进行真空热压烧结。真空热压烧结加压完成后关闭加热电源随炉冷却获得密度≥99%理论密度且纯度≥99.99%的钨镍合金靶材,其微观组织图如图1所示。将该钨镍合金靶材作为溅射靶材,采用射频反应磁控溅射在璃衬底表面沉积WO3薄膜,其中溅射功率120W,溅射60min后采用台阶仪对薄膜样品进行测量,薄膜分布均匀且厚度为140nm。
实施例2
(1)按如下重量百分比称取各组分:纯度≥99.999%且平均费氏粒度为5.0μm的钨粉50%、纯度≥99.95%且平均费氏粒度为5.0μm的镍粉40%和纯度≥99.95%且平均费氏粒度为5.0μm的三氧化钨粉10%;
(2)将上述各组分置于V形混料器中以20r/min的转速混合均匀,得含高纯钨(W)质量百分比50%,镍(Ni)质量百分比40%,三氧化钨(WO3)质量百分比10%的混合粉末;
(3)将上述混合粉末置于真空热压烧结模具内,再装入真空热压烧结炉内以5℃/min速率升温至1430℃,加压至35MPa,保温120min进行真空热压烧结。真空热压烧结加压完成后关闭加热电源随炉冷却获得密度≥99%理论密度且纯度≥99.99%的钨镍合金靶材,其微观组织图如图2所示。将该钨镍合金靶材作为溅射靶材,采用射频反应磁控溅射在璃衬底表面沉积WO3薄膜,其中溅射功率120W,溅射60min后采用台阶仪对薄膜样品进行测量,薄膜分布均匀且膜厚为138nm。
实施例3
(1)按如下重量百分比称取各组分:纯度≥99.999%且平均费氏粒度为5.0μm的钨粉50%、纯度≥99.95%且平均费氏粒度为5.0μm的镍粉30%和纯度≥99.95%且平均费氏粒度为5.0μm的三氧化钨粉20%;
(2)将上述各组分置于V形混料器中以20r/min的转速混合均匀,得含高纯钨(W)质量百分比50%,镍(Ni)质量百分比30%,三氧化钨(WO3)质量百分比20%的混合粉末;
(3)将上述混合粉末置于真空热压烧结模具内,再装入真空热压烧结炉内以5℃/min速率升温至1430℃,加压至35MPa,保温120min进行真空热压烧结。真空热压烧结加压完成后关闭加热电源随炉冷却获得密度≥99%理论密度且纯度≥99.99%的钨镍合金靶材,其微观组织图如图3所示。将该钨镍合金靶材作为溅射靶材,采用射频反应磁控溅射在璃衬底表面沉积WO3薄膜,其中溅射功率120W,溅射60min后采用台阶仪对薄膜样品进行测量,薄膜分布均匀且膜厚为142nm。
实施例4
(1)按如下重量百分比称取各组分:纯度≥99.999%且平均费氏粒度为5.0μm的钨粉30%、纯度≥99.95%且平均费氏粒度为5.0μm的镍粉50%和纯度≥99.95%且平均费氏粒度为5.0μm的三氧化钨粉20%;
(2)将上述各组分置于V形混料器中以20r/min的转速混合均匀,得含高纯钨(W)质量百分比30%,镍(Ni)质量百分比50%,三氧化钨(WO3)质量百分比20%的混合粉末;
(3)将上述混合粉末置于真空热压烧结模具内,再装入真空热压烧结炉内以5℃/min速率升温至1430℃,加压至35MPa,保温120min进行真空热压烧结。真空热压烧结加压完成后关闭加热电源随炉冷却获得密度≥99%理论密度且纯度≥99.99%的钨镍合金靶材,其微观组织图如图4所示。将该钨镍合金靶材作为溅射靶材,采用射频反应磁控溅射在璃衬底表面沉积WO3薄膜,其中溅射功率120W,溅射60min后采用台阶仪对薄膜样品进行测量,薄膜分布均匀且膜厚为139nm。
本领域普通技术人员可知,本发明的组分和技术参数在下述范围内变化时,仍能够得到与上述实施例相同或相近的技术效果,仍然属于本发明的保护范围:
一种用于电致变色玻璃镀膜的钨镍合金靶材的制备方法,其特征在于:包括如下步骤:
(1)按如下重量百分比称取各组分:纯度≥99.999%且平均费氏粒度为1.0μm~20.0μm的钨粉25~55%、纯度≥99.95%且平均费氏粒度为1.0μm~20.0μm的镍粉25~55%和纯度≥99.95%且平均费氏粒度为1.0μm~20.0μm的三氧化钨粉10~25%;
(2)将上述各组分置于V形混料器中以15~22r/min的转速混合均匀,得混合粉末;
(3)将上述混合粉末置于真空热压烧结模具内,再装入真空热压烧结炉内以4~9℃/min(优选5~8℃/min)速率升温至1400~1500℃(优选1400~1450℃)的烧结温度,加压至28~37MPa(优选30~35MPa),保温100~150min(优选120~140min)进行真空热压烧结。真空热压烧结加压完成后关闭加热电源随炉冷却获得密度≥99%理论密度且纯度≥99.99%的钨镍合金靶材。
以上所述,仅为本发明的较佳实施例而已,故不能依此限定本发明实施的范围,即依本发明专利范围及说明书内容所作的等效变化与修饰,皆应仍属本发明涵盖的范围内。
Claims (7)
1.一种用于电致变色玻璃镀膜的钨镍合金靶材的制备方法,其特征在于:包括如下步骤:
(1)按如下重量百分比称取各组分:纯度≥99.999%且平均费氏粒度为1.0μm~20.0μm的钨粉25~55%、纯度≥99.95%且平均费氏粒度为1.0μm~20.0μm的镍粉25~55%和纯度≥99.95%且平均费氏粒度为1.0μm~20.0μm的三氧化钨粉10~25%;
(2)将上述各组分置于V形混料器中以15~22r/min的转速混合均匀,得混合粉末;
(3)将上述混合粉末置于真空热压烧结模具内,再装入真空热压烧结炉内以4~9℃/min速率升温至1400~1500℃的烧结温度,加压至28~37MPa,保温100~150min进行真空热压烧结,真空热压烧结加压完成后关闭加热电源随炉冷却获得密度≥99%理论密度且纯度≥99.99%的钨镍合金靶材。
2.如权利要求1的制备方法,其特征在于:所述步骤(1)为:按如下重量百分比称取各组分:纯度≥99.999%且平均费氏粒度为1.0μm~20.0μm的钨粉30~50%、纯度≥99.95%且平均费氏粒度为1.0μm~20.0μm的镍粉30~50%和纯度≥99.95%且平均费氏粒度为1.0μm~20.0μm的三氧化钨粉10~20%。
3.如权利要求1的制备方法,其特征在于:所述步骤(2)为:将上述各组分置于V形混料器中以20r/min的转速混合均匀,得混合粉末。
4.如权利要求1的制备方法,其特征在于:所述步骤(3)中的升温速率为5~8℃/min。
5.如权利要求1的制备方法,其特征在于:所述步骤(3)中的烧结温度为1400~1450℃。
6.如权利要求1的制备方法,其特征在于:所述步骤(3)中加压至30~35MPa。
7.如权利要求1的制备方法,其特征在于:所述步骤(3)中保温时间为120~140min。
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