CN115386847B - 一种蓝色铜合金薄膜的制备方法 - Google Patents
一种蓝色铜合金薄膜的制备方法 Download PDFInfo
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- 229910000881 Cu alloy Inorganic materials 0.000 title claims abstract description 36
- 241000530268 Lycaena heteronea Species 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 31
- 239000011248 coating agent Substances 0.000 claims abstract description 25
- 238000000576 coating method Methods 0.000 claims abstract description 25
- 239000002131 composite material Substances 0.000 claims abstract description 16
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052786 argon Inorganic materials 0.000 claims abstract description 7
- 239000011521 glass Substances 0.000 claims description 24
- 239000010949 copper Substances 0.000 claims description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 238000004544 sputter deposition Methods 0.000 claims description 11
- 238000000151 deposition Methods 0.000 claims description 9
- 230000008021 deposition Effects 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 239000004642 Polyimide Substances 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 229920001721 polyimide Polymers 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 abstract description 32
- 239000000956 alloy Substances 0.000 abstract description 32
- 125000004430 oxygen atom Chemical group O* 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 76
- 230000000052 comparative effect Effects 0.000 description 19
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 9
- 229910002058 ternary alloy Inorganic materials 0.000 description 8
- 238000004506 ultrasonic cleaning Methods 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000013077 target material Substances 0.000 description 3
- 239000003086 colorant Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 238000005566 electron beam evaporation Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 241001270131 Agaricus moelleri Species 0.000 description 1
- 229910017985 Cu—Zr Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 235000005811 Viola adunca Nutrition 0.000 description 1
- 240000009038 Viola odorata Species 0.000 description 1
- 235000013487 Viola odorata Nutrition 0.000 description 1
- 235000002254 Viola papilionacea Nutrition 0.000 description 1
- -1 ZnS Chemical compound 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 1
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002120 nanofilm Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C9/00—Alloys based on copper
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
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- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
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Abstract
一种蓝色铜合金薄膜的制备方法，其先取Cu‑Mo‑Zr复合靶置于真空室内抽真空，在真空度达到1*10‑3～9*10‑3Pa后，再向真空室内通入高纯氩气至真空室气压达到0.3～1.0MPa后，采用直流磁控溅射镀膜机使Cu‑Mo‑Zr复合靶溅射沉积于基体上，即得所述蓝色铜合金薄膜。本发明的通过元素Zr和Mo的加入，控制特定的真空度，使真空室内残余的氧原子进入到薄膜表面微结构的空隙、空位处，制备出蓝色合金薄膜，操作方便，成本低，绿色环保。
Description
技术领域
本发明属于纳米薄膜材料制备领域，具体涉及一种蓝色铜合金薄膜的制备方法。
背景技术
蓝色薄膜因其独特的光学性能在许多领域都得到了广泛应用。例如，蓝膜可以有效地反射蓝紫光，在农业领域可以促进农作物生长；将蓝色薄膜沉积在玻璃基底上可以作为光学滤光片，蓝色玻璃光学元件可以制备消色差镜头；在低辐射玻璃中蓝色薄膜层也起到了抵挡紫外线降低辐射的作用，蓝色薄膜在日常还可以起到装饰，遮蔽的作用。
目前，常用制备蓝色薄膜的方法有电子束蒸发法和化学染料染色法。但是，电子束蒸发过程中电子束和蒸汽粒子间的相互作用会影响膜层质量，化学染料染色过程使用大量化学试剂且获得的颜色不稳定易褪色。
发明内容
本发明的目的在于提供一种蓝色铜合金薄膜的制备方法，其能够通过溅射法一步制备出蓝色铜合金薄膜，操作方便，成本低，绿色环保。
本发明所采用的技术方案是：
一种蓝色铜合金薄膜的制备方法，包括以下步骤：
（1）取Cu-Mo-Zr复合靶置于真空室内抽真空，在真空度达到1*10-3～9*10-3Pa后，向真空室内通入高纯氩气；
（2）在真空室气压达到0.3～1.0MPa后，采用直流磁控溅射镀膜机使Cu-Mo-Zr复合靶溅射沉积于基体上，即得所述蓝色铜合金薄膜。
进一步地，以质量百分比计，蓝色铜合金薄膜中Cu含量为60-85%，Mo含量为10-20%，Zr含量为5-20%。
进一步地，溅射沉积时间为5-15min。
进一步地，所述蓝色铜合金薄膜的厚度为75-300nm。
进一步地，所述直流磁控溅射镀膜机为JCP-350直流磁控溅射镀膜机。
进一步地，所述基体为玻璃、聚酰亚胺、硅片、PET中的任意一种。
进一步地，所述基体在使用前进行预处理：将基体依次经丙酮和去离子水清洗后，用氮气吹干。
本发明的有益效果：
1.本发明无需通入氮气或者氧气，采用简单环保的溅射法即可一步制备出蓝色铜合金薄膜，不同与以往蓝色薄膜（主要包括TiN等氮化物、ZnS等硫化物以及光致变色、电致变色的氧化物等）的体系和制备方法，操作方便，成本低，绿色环保。
2.本发明通过元素Zr和Mo的加入，使合金薄膜表面存在一些空隙和空位，便于O的吸附，在沉积过程中，通过控制特定的真空度，使真空室内残余的O原子进入到薄膜表面微结构的空隙、空位处，将合金薄膜中的Cu0氧化为Cu+，使合金薄膜呈现出蓝色。
3.本发明通过控制特定的薄膜厚度，当入射光照射在合金薄膜表面时，一部分光线被反射，另一部分光线透射到合金薄膜内部发生折射，当透射光达到基体的上表面时，部分透射光被反射回合金薄膜内部，最后经过合金薄膜上表面折射进入空气中，干涉发生在被合金薄膜表面反射光束和最后经过折射进入空气中的光束之间，通过控制合金薄膜的厚度可以改变两列光的光程差，波长与光程差相同或相近或成倍数关系的光将得到加强，其它波长的光将变弱，光程差小的复合后得到加强光的频率偏高而呈现出明显的蓝色。
附图说明
图1为实施例1所制备75nm厚蓝色铜合金薄膜的外观形貌图；
图2为实施例1所制备75nm厚蓝色铜合金薄膜的表面形貌图；
图3为对比例1所制备合金薄膜的外观形貌图；
图4为对比例2所制备合金薄膜的外观形貌图；
图5为对比例3所制备合金薄膜的外观形貌图；
图6为对比例4所制备合金薄膜的外观形貌图；
图7为实施例3所制备蓝色铜合金薄膜的表面形貌图；
图8为对比例3所制备薄膜的表面形貌图；
图9为实施例3所制备蓝色铜合金薄膜的Cu 2P轨道的XPS谱图；
图10为实施例3所制备蓝色铜合金薄膜的Cu的LMM的XPS图谱；
图11为对比例3所制备薄膜的Cu 2P轨道的XPS谱图；
图12为对比例3所制备薄膜的Cu的LMM的XPS图谱。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
本发明提供一种蓝色铜合金薄膜的制备方法，包括以下步骤：
（1）取Cu-Mo-Zr复合靶置于真空室内抽真空，在真空度达到1*10-3～9*10-3Pa后，向真空室内通入高纯氩气；
（2）在真空室气压达到0.3～1.0MPa后，采用直流磁控溅射镀膜机使Cu-Mo-Zr复合靶溅射沉积于基体上，即得所述蓝色铜合金薄膜。
其中，以质量百分比计，蓝色铜合金薄膜中Cu含量为60-85%，Mo含量为10-20%，Zr含量为5-20%。
溅射沉积时间为5-15min。
蓝色铜合金薄膜的厚度为75-300nm。
直流磁控溅射镀膜机为JCP-350直流磁控溅射镀膜机。
基体为玻璃、聚酰亚胺、硅片、PET中的任意一种。
基体在使用前进行预处理：将基体依次经丙酮和去离子水清洗后，用氮气吹干。
实施例1
(1)、玻璃基体清洗
将玻璃基体置入装有丙酮的烧杯中，将该烧杯放入超声波清洗机中超声清洗10分钟，然后再将清洗后的玻璃放入装有去离子水的烧杯中超声清洗5分钟，将清洗好的玻璃基体用氮气吹干，然后将该基体固定到磁控溅射镀膜机基片台上。
(2)、靶材准备及真空度控制
镀膜采用JCP-350直流磁控溅射镀膜机，在镀膜机的靶位放置好Cu-Mo-Zr复合靶，将靶材和玻璃基体放置好以后将镀膜机的真空室关闭，并开启机械泵、分子泵对真空室抽真空，使真空度达到1*10-3Pa。
(3)、沉积制备三元蓝色铜合金膜
当真空室真空度达到1*10-3 时，向真空室通入高纯氩气使真空室内的气压达到0.3Pa，然后接通Cu-Mo-Zr复合靶的电源开始溅射，溅射功率为100W，在玻璃基体上沉积三元合金薄膜，沉积时间5分钟，以质量百分比计，三元合金薄膜中Cu、Mo、Zr的含量分别为85%，10%，5%，薄膜厚度为75nm，即可制备出三元合金蓝色铜合金薄膜，其宏观形貌如图1所示，表面形貌如图2所示。
实施例2
(1)、玻璃基体清洗
将玻璃基体置入装有丙酮的烧杯中，将该烧杯放入超声波清洗机中超声清洗10分钟，然后再将清洗后的玻璃放入装有去离子水的烧杯中超声清洗5分钟，将清洗好的玻璃基体用氮气吹干，然后将该基体固定到磁控溅射镀膜机基片台上。
(2)、靶材准备及真空度控制
镀膜采用JCP-350直流磁控溅射镀膜机，在镀膜机的靶位放置好Cu-Mo-Zr复合靶，将靶材和玻璃基体放置好以后将镀膜机的真空室关闭，并开启机械泵、分子泵对真空室抽真空，使真空度达到9*10-3Pa。
(3)、沉积制备三元蓝色铜合金薄膜
当真空室真空度达到9*10-3 时，向真空室通入高纯氩气使真空室内的气压达到0.6Pa，然后接通Cu-Mo-Zr复合靶的电源开始溅射，溅射功率为100W，在玻璃基体上沉积三元合金薄膜，沉积时间15分钟，以质量百分比计，薄膜中Cu、Mo、Zr的含量分别为72%，16%，12%，厚度为300nm，即可制备出三元合金蓝色铜合金薄膜。
实施例3
(1)、玻璃基体清洗
将玻璃基体置入装有丙酮的烧杯中，将该烧杯放入超声波清洗机中超声清洗10分钟，然后再将清洗后的玻璃放入装有去离子水的烧杯中超声清洗5分钟，将清洗好的玻璃基体用氮气吹干，然后将该基体固定到磁控溅射镀膜机基片台上。
(2)、靶材准备及真空度控制
镀膜采用JCP-350直流磁控溅射镀膜机，在镀膜机的靶位放置好Cu-Mo-Zr复合靶，将靶材和玻璃基体放置好以后将镀膜机的真空室关闭，并开启机械泵、分子泵对真空室抽真空，使真空度达到5*10-3Pa。
(3)、沉积制备三元蓝色铜合金膜
当真空室真空度达到5*10-3 时，向真空室通入高纯氩气使真空室内的气压达到1.0Pa，然后接通Cu-Mo-Zr复合靶的电源开始溅射，溅射功率为100W，在玻璃基体上沉积三元合金薄膜，沉积时间10分钟，以质量百分比计，合金薄膜中Cu、Mo、Zr的含量分别为60%，20%，20%，厚度为200nm，即可制备出三元合金蓝色铜合金薄膜。
对比例1
与实施例1不同的是，步骤（2）中，采用Cu-Mo复合靶，以质量百分比计，Cu的含量为80%，Mo的含量为20%。
对比例2
与实施例1不同的是，步骤（2）中，采用Cu- Zr复合靶，以质量百分比计，Cu的含量为80%，Zr的含量为的20%。
对比例3
与实施例1不同的是，步骤（2）中，真空度为3*10-4Pa。
对比例4
与实施例1不同的是，步骤（2）中，薄膜厚度为50nm。
实施例所制备出合金薄膜均为蓝色，图1为实施例1所制备出合金薄膜的灰度图，图2为其微观表面示意图，对比例1-4的合金膜均未显示出蓝色，其中，图3为对比例1制备出的合金薄膜的灰度图，其呈现出淡土黄色，图4为对比例2制备出的合金薄膜的灰度图，其呈现出深棕色，图5和图6分别为对比例3、对比例4制备出的合金薄膜的灰度图，相较对比例2，图5和图6依次呈现棕色逐渐变淡的规律。
图7为实施例3所制备合金薄膜的电镜图，图中，a1中的晶面间距为0.245nm，对应于Cu2O（111）晶面，表明当真空度为5×10-3Pa时，合金薄膜内部出现了Cu+，使薄膜的颜色为蓝色。
图8为对比例3所制备合金薄膜的电镜图，图中，b1中的晶面间距为0.212nm，对应于Cu（111）晶面，表明当真空度为3×10-4Pa时，合金薄膜为Cu0，并未出现Cu+。
图9为实施例3所制备合金薄膜Cu 2P轨道的XPS图谱，图10为实施例3所制备合金薄膜Cu的LMM的XPS图谱，图11为对比例3所制备合金薄膜Cu 2P轨道的XPS图谱，图12为对比例3所制备合金薄膜Cu的LMM的XPS图谱，由XPS图谱也可知，当真空度为5×10-3Pa时，合金薄膜中出现了Cu+，而当真空度为3×10-4Pa时，合金薄膜中只存在零价Cu。
需要说明的是，上述实施例仅用来说明本发明，但本发明并不局限于上述实施例，凡是依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰，均落入本发明的保护范围内。
Claims (4)
1.一种蓝色铜合金薄膜的制备方法，其特征在于，包括以下步骤：
（1）取Cu-Mo-Zr复合靶置于真空室内抽真空，在真空度达到1*10-3～9*10-3Pa后，向真空室内通入高纯氩气；
（2）在真空室气压达到0.3-1.0MPa后，采用直流磁控溅射镀膜机使Cu-Mo-Zr复合靶溅射沉积于基体上，即得所述蓝色铜合金薄膜，溅射沉积时间为5-15min，以质量百分比计，蓝色铜合金薄膜中Cu含量为60-85%，Mo含量为10-20%，Zr含量为5-20%，蓝色铜合金薄膜的厚度为75-300nm。
2.如权利要求1所述的一种蓝色铜合金薄膜的制备方法，其特征在于，所述直流磁控溅射镀膜机为JCP-350直流磁控溅射镀膜机。
3.如权利要求1所述的一种蓝色铜合金薄膜的制备方法，其特征在于，所述基体为玻璃、聚酰亚胺、硅片、PET中的任意一种。
4.如权利要求3所述的一种蓝色铜合金薄膜的制备方法，其特征在于，所述基体在使用前进行预处理：将基体依次经丙酮和去离子水清洗后，用氮气吹干。
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