CN108447789A - 一种柔性薄膜变容管的制备方法 - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 72
- 239000011787 zinc oxide Substances 0.000 claims abstract description 36
- 238000004544 sputter deposition Methods 0.000 claims abstract description 27
- 239000000758 substrate Substances 0.000 claims abstract description 27
- 239000007789 gas Substances 0.000 claims abstract description 24
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 14
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 14
- 229910052738 indium Inorganic materials 0.000 claims abstract description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052786 argon Inorganic materials 0.000 claims abstract description 9
- 239000011889 copper foil Substances 0.000 claims abstract description 9
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 7
- 229910052751 metal Inorganic materials 0.000 claims abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000001301 oxygen Substances 0.000 claims abstract description 3
- 239000010408 film Substances 0.000 claims description 65
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 25
- 239000010409 thin film Substances 0.000 claims description 8
- 238000004070 electrodeposition Methods 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 6
- 230000003746 surface roughness Effects 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 claims description 5
- 238000004062 sedimentation Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims 1
- 238000000151 deposition Methods 0.000 abstract description 4
- 230000008021 deposition Effects 0.000 abstract description 4
- 229960001296 zinc oxide Drugs 0.000 description 26
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000007790 solid phase Substances 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000004891 communication Methods 0.000 description 3
- QFUKUPZJJSMEGE-UHFFFAOYSA-N 5-(hydroxymethyl)-1-(3-methylbutyl)pyrrole-2-carbaldehyde Chemical compound CC(C)CCN1C(CO)=CC=C1C=O QFUKUPZJJSMEGE-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
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Abstract
本发明公开了一种柔性薄膜变容管的制备方法，以铜箔作柔性衬底，将掺杂Al、Ga或In的氧化锌为靶材，系统的本底真空度抽至3.0×10‑ 3Pa以下，使用Ar气体作为溅射气体溅射掺杂Al、Ga或In的氧化锌薄膜层，沉积得到50～1000nm厚的掺杂Al、Ga或In的氧化锌薄膜层：再以BaZr0.2Ti0.8O3为靶材，系统的本底真空抽至1.0×10‑3Pa以下，使用Ar和O2作为溅射气体，氧气和氩气的分压比为1：4～15，沉积得到150～800nm的BaZr0.2Ti0.8O3薄膜层；再在BZT薄膜层和底电极掺杂Al、Ga或In的氧化锌层表面制备金属电极，制得柔性薄膜变容管。本发明的柔性薄膜变容管的介电调谐率≥50％@100kHz，介电损耗<0.03，在柔性曲率半径为5.0mm时，性能变化率≤10％。
Description
技术领域
本发明属于一种以成分为特征的陶瓷组合物，尤其涉及一种柔性薄膜变容管及其制备方法。
背景技术
变容管在通讯电子电路中有着重要的应用，其可实现通讯信号的接收和发射。目前，随着移动通讯设备向着柔性化方向的发展，传统的硬质薄膜变容管已经不能满足柔性电子电路的需求，继续开发柔性的薄膜变容管，以实现与柔性电路相匹配和兼容。
BaZr0.2Ti0.8O3(BZT)作为目前研究最为广泛的介电调谐薄膜材料，其具有介电调谐率高和介电常数大的优点，常被用来在硅基衬底上制备硬质变容管。由于柔性衬底和制备技术的限制，目前还未出现以其为基础制备的柔性变容管。本发明将解决BZT制备柔性薄膜变容管的技术难题，并制备出性能优良的柔性变容管。
发明内容
本发明的目的，在于克服现有技术中的不足，解决BZT即BaZr0.2Ti0.8O3制备柔性薄膜变容管的技术难题，利用磁控溅射沉积技术，提供一种成本低廉而性能优良的BaZr0.2Ti0.8O3基柔性变容管的制备方法。
本发明通过如下技术方案予以实现。
一种柔性薄膜变容管的制备方法，具有如下步骤：
(1)将铜箔表面清洗干净放入磁控溅射腔体内的样品台上，作为柔性衬底；
(2)将掺杂Al、Ga或In的氧化锌靶材装入磁控溅射的靶头上；
靶材与衬底的距离为40～90mm；
(3)待步骤(2)完成后，将磁控溅射系统的本底真空度抽至3.0×10-3Pa以下，使用Ar气体作为溅射气体溅射掺杂Al、Ga或In的氧化锌薄膜层，溅射功率为30～180W，衬底温度为室温到600℃，进行沉积得到50～1000nm厚的掺杂Al、Ga或In的氧化锌薄膜层
(4)取出衬底，在掺杂Al、Ga或In的氧化锌层表面用掩模版遮盖，留出底电极位置后，再将其放入磁控溅射腔体内的样品台上；
(5)将BZT即BaZr0.2Ti0.8O3靶材装入磁控溅射靶头；
(6)将磁控溅射系统的本底真空抽至1.0×10-3Pa以下，然后加热衬底至400～700℃；使用Ar和O2作为溅射气体，氧气和氩气的分压比为1：4～15，溅射功率为50～200W，进行沉积得到BZT薄膜层，该薄膜层厚度为150～800nm；
(7)步骤(6)结束后，在BZT薄膜层和底电极掺杂Al、Ga或In的氧化锌层表面上面利用掩膜版制备金属电极，进行介电调谐和柔性性能测试。制得柔性薄膜变容管。
所述步骤(1)的铜箔的厚度为1微米～1毫米，纯度≥98％，表面粗糙度≤300纳米。
所述步骤(2)是将掺杂Al的氧化锌靶材装入磁控溅射的靶头上；
所述步骤(2)的所述靶材为任意市售或者采用常规的固相烧结法自制而成。
所述步骤(3)或步骤(6)的Ar和O2的纯度均在99.99％以上。
所述步骤(3)或步骤(6)的薄膜层厚度通过调节工艺参数或者沉积时间来控制。
本发明的柔性薄膜变容管的介电调谐率≥50％@100kHz，介电损耗<0.03，在柔性曲率半径为5.0mm时，性能变化率≤10％。其调谐率高、柔性性能良好，且器件稳定性好，为柔性电子通讯设备的开发和应用提供了优良的电子元器件基础。
附图说明
图1是实施例1柔性BZT薄膜的变容调谐性能图。
具体实施方式
下面结合具体实施例进一步阐述本发明，应理解，这些实施例仅用于说明本发明而不用于限制本发明的保护范围。
实施例1
(1)将纯度为99％、面粗糙度为100nm、厚度为100um的铜箔表面清洗干净，放入磁控溅射腔体内的样品台上，作为柔性衬底；
(2)将Al掺杂的氧化锌靶材装入磁控溅射的靶头上，靶材和衬底距离60mm。
(3)待步骤(2)完成后，将磁控溅射系统的本底真空度抽至3.0×10-4Pa，使用Ar气体作为溅射气体溅射Al掺杂的氧化锌薄膜层，Ar的纯度为99.99％，射功率为80W，衬底温度为300℃，进行沉积得到200nm厚的Al掺杂氧化锌薄膜层。
(4)取出衬底，在Al掺杂的氧化锌薄膜层表面用掩模版遮盖，留出底电极位置后，再将其放入磁控溅射腔体内的样品台上。
(5)将BZT即BaZr0.2Ti0.8O3靶材装入磁控溅射靶头；该BZT靶材采用固相烧结法制备而成，所用原料BaCO3、TiO2和ZrO2的纯度均在99％以上。
(6)将磁控溅射系统的本底真空抽至3.0×10-4Pa，然后加热衬底至700℃；使用Ar和O2(比例5:1)作为溅射气体，Ar和O2的纯度均为99.99％，为100W，进行沉积得到250纳米厚的BZT薄膜层。
(7)步骤(6)结束后，在BZT薄膜层和底电极掺杂氧化锌薄膜层表面上面利用掩膜版制备金属电极，制得柔性薄膜变容管，进行介电调谐和柔性性能测试。
图1揭示了实施例1的柔性BZT薄膜变容管的调谐性能，其调谐率为71％，介电损耗为0.022。在曲率半径为5.0mm时，其调谐率为68％，介电损耗为0.023。
实施例2
(1)将纯度为99％、面粗糙度为100nm、厚度为100um的铜箔表面清洗干净，并放入磁控溅射腔体内的样品台上，作为柔性衬底。
(2)将Al掺杂的氧化锌靶材装入磁控溅射的靶头上，靶材和衬底距离60mm。
(3)待步骤(2)完成后，将磁控溅射系统的本底真空度抽至5.0×10-4Pa，使用Ar气体作为溅射气体溅射Al掺杂的氧化锌薄膜层，Ar的纯度99.99％，溅射功率为80W，衬底温度为500℃，进行沉积得到100nm厚的Al掺杂氧化锌薄膜层。
(4)取出衬底，在Al掺杂的氧化锌薄膜层表面用掩模版遮盖，留出底电极位置后，再将其放入磁控溅射腔体内的样品台上。
(5)将BZT即BaZr0.2Ti0.8O3靶材装入磁控溅射靶头；该BZT靶材采用固相烧结法制备而成，所用原料BaCO3、TiO2和ZrO2的纯度均在99％以上。
(6)将磁控溅射系统的本底真空抽至3.0×10-4Pa，然后加热衬底至700℃；使用Ar和O2(比例4:1)作为溅射气体，Ar和O2的纯度均为99.99％，溅射功率为80W，进行沉积得到200纳米厚的BZT薄膜层。
(7)步骤(6)结束后，在BZT薄膜层和底电极掺杂氧化锌薄膜层表面上面利用掩膜版制备金属电极，制得柔性薄膜变容管，进行介电调谐和柔性性能测试。
实施例2的变容管其调谐率为65％，介电损耗为0.027。在曲率半径为5.0mm时，其调谐率为59％，介电损耗为0.029。
实施例3
(1)将纯度为99％、表面粗糙度为100nm、厚度为100um的铜箔表面清洗干净，并放入磁控溅射腔体内的样品台上，作为柔性衬底。
(2)将Al掺杂的氧化锌靶材装入磁控溅射的靶头上，靶材和衬底距离60mm。
(3)待步骤(2)完成后，将磁控溅射系统的本底真空度抽至9.0×10-4Pa，使用Ar气体作为溅射气体溅射Al掺杂的氧化锌薄膜层，Ar的纯度99.99％，溅射功率为80W，衬底温度为100℃进行沉积得到400nm厚的Al掺杂氧化锌薄膜层。
(4)取出衬底，在Al掺杂的氧化锌薄膜层表面用掩模版遮盖，留出底电极位置后，再将其放入磁控溅射腔体内的样品台上。
(5)将BZT即BaZr0.2Ti0.8O3靶材装入磁控溅射靶头；该BZT靶材采用固相烧结法制备而成，所用原料BaCO3、TiO2和ZrO2的纯度均在99％以上。
(6)将磁控溅射系统的本底真空抽至6.0×10-4Pa，然后加热衬底至500℃；使用Ar和O2(比例4:1)作为溅射气体，Ar和O2的纯度均为99.99％，溅射功率为120W，进行沉积得到300纳米厚的BZT薄膜层。
(7)步骤(6)结束后，在BZT薄膜层和底电极掺杂氧化锌薄膜层表面上面利用掩膜版制备金属电极，制得柔性薄膜变容管，进行介电调谐和柔性性能测试。
实施例3的变容管其调谐率为55％，介电损耗为0.030。在曲率半径为5.0mm时，其调谐率为52％，介电损耗为0.035。
实施例4
(1)将纯度为99％、表面粗糙度为200nm、厚度为100um的铜箔表面清洗干净，并放入磁控溅射腔体内的样品台上作为柔性衬底。
(2)将Al掺杂的氧化锌靶材装入磁控溅射的靶头上，靶材和衬底距离60mm。
(3)待步骤2完成后，将磁控溅射系统的本底真空度抽至9.0×10-4Pa，使用Ar气体作为溅射气体溅射Al掺杂的氧化锌薄膜层，Ar的纯度99.99％，溅射功率为80W，衬底温度为400℃进行沉积得到300nm厚的Al掺杂氧化锌薄膜层。
(4)取出衬底，在Al掺杂的氧化锌薄膜层表面用掩模版遮盖，留出底电极位置后，再将其放入磁控溅射腔体内的样品台上。
(5)将BZT即BaZr0.2Ti0.8O3靶材装入磁控溅射靶头；该BZT靶材采用固相烧结法制备而成，所用原料BaCO3、TiO2和ZrO2的纯度均在99％以上。
(6)将磁控溅射系统的本底真空抽至6.0×10-4Pa，然后加热衬底至600℃；使用Ar和O2(比例4:1)作为溅射气体，Ar和O2的纯度均为99.99％，溅射功率为60W，进行沉积得到100纳米厚的BZT薄膜层。
(7)步骤(6)结束后，在BZT薄膜层和底电极掺杂氧化锌薄膜层表面上面利用掩膜版制备金属电极，制得柔性薄膜变容管，进行介电调谐和柔性性能测试。
实施例4的变容管其调谐率为62％，介电损耗为0.026。在曲率半径为5.0mm时，其调谐率为60％，介电损耗为0.031。
Claims (6)
1.一种柔性薄膜变容管的制备方法，具有如下步骤：
(1)将铜箔表面清洗干净放入磁控溅射腔体内的样品台上，作为柔性衬底；
(2)将掺杂Al、Ga或In的氧化锌靶材装入磁控溅射的靶头上；
靶材与衬底的距离为40～90mm；
(3)待步骤(2)完成后，将磁控溅射系统的本底真空度抽至3.0×10-3Pa以下，使用Ar气体作为溅射气体溅射掺杂Al、Ga或In的氧化锌薄膜层，溅射功率为30～180W，衬底温度为室温到600℃，进行沉积得到50～1000nm厚的掺杂Al、Ga或In的氧化锌薄膜层。
(4)取出衬底，在掺杂Al、Ga或In的氧化锌层表面用掩模版遮盖，留出底电极位置后，再将其放入磁控溅射腔体内的样品台上；
(5)将BZT即BaZr0.2Ti0.8O3靶材装入磁控溅射靶头；
(6)将磁控溅射系统的本底真空抽至1.0×10-3Pa以下，然后加热衬底至400～700℃；使用Ar和O2作为溅射气体，氧气和氩气的分压比为1：4～15，溅射功率为50～200W，进行沉积得到BZT薄膜层，该薄膜层厚度为150～800nm；
(7)步骤(6)结束后，在BZT薄膜层和底电极掺杂Al、Ga或In的氧化锌层表面利用掩膜版制备金属电极，制得柔性薄膜变容管。
2.根据权利要求1所述的一种柔性薄膜变容管的制备方法，其特征在于，所述步骤(1)的铜箔的厚度为1微米～1毫米，纯度≥98％，表面粗糙度≤300纳米。
3.根据权利要求1所述的一种柔性薄膜变容管的制备方法，其特征在于，所述步骤(2)是将掺杂Al的氧化锌靶材装入磁控溅射的靶头上。
4.根据权利要求1所述的一种柔性薄膜变容管的制备方法，其特征在于，所述步骤(2)的靶材为任意市售或者采用常规的固相烧结法自制而成。
5.根据权利要求1所述的一种柔性薄膜变容管的制备方法，其特征在于，所述步骤(3)或步骤(6)的Ar和O2的纯度均在99.99％以上。
6.根据权利要求1所述的一种柔性薄膜变容管的制备方法，其特征在于，所述步骤(3)或步骤(6)的薄膜层厚度通过调节工艺参数或者沉积时间来控制。
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