CN1017164B - 在硅或砷化镓基底上制备反射防止膜的方法 - Google Patents
在硅或砷化镓基底上制备反射防止膜的方法Info
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- 229910001218 Gallium arsenide Inorganic materials 0.000 title claims abstract description 13
- 239000011248 coating agent Substances 0.000 title claims description 4
- 238000000576 coating method Methods 0.000 title claims description 4
- 238000002360 preparation method Methods 0.000 title claims description 3
- 229910052710 silicon Inorganic materials 0.000 title claims description 3
- 239000010703 silicon Substances 0.000 title claims description 3
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 title description 11
- 239000000758 substrate Substances 0.000 title description 11
- 238000001704 evaporation Methods 0.000 claims abstract description 23
- 230000008020 evaporation Effects 0.000 claims abstract description 22
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 15
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 238000010894 electron beam technology Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000003287 optical effect Effects 0.000 abstract 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- 239000013307 optical fiber Substances 0.000 abstract 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 abstract 1
- 229910001928 zirconium oxide Inorganic materials 0.000 abstract 1
- 239000000463 material Substances 0.000 description 13
- 229910010413 TiO 2 Inorganic materials 0.000 description 6
- 239000000470 constituent Substances 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 238000002310 reflectometry Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000003292 diminished effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000012887 quadratic function Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
本发明涉及一种含有氧化钛和氧化锆的蒸镀用的氧化钇组成物，及用这种组成物作为蒸镀材料制造用于如硅或GaAs那样的III-V族化合物半导体用的反射防止膜，该反射防止膜能使被蒸镀物上的表面反射率几乎为零。而且，由于时效变化小，动作时间可以延长。
Description
本发明涉及蒸镀用的氧化钇组成物及反射防止膜的制造方法。
如在Appl.Phys.Lett Vo L.47、NO.5，第450页和Applied Optics，Vol.23，NO.1，第161页上说明的那样，人们通常使用ZrO2或Si3N4作为蒸镀材料对由Si或GaAs制成的元件进行反射防止膜的形成。这是因为这些元件的折射率为3.5，要求反射防止膜的折射率值在理论上为
＝1.87。折射率大致能满足1.87的蒸镀材料是ZrO2和Si3N4。这些材料的块状的折射率各为2.05和1.98，然而在作为薄膜使用的情况下，通过调整蒸镀条件，可以达到折射率n＝1.87。关于这个事实显示在T.L.Paoli，Appl.Phys.Lett.47（5），450（1985），第450页和G.Eisens-tein，Appl.Optics，23（1），161（1984），第162页上。以往在使用ZrO2或Si3N4那样的蒸镀组成物来生成用于Si或GaAs的反射防止膜时，即使能使反射率达到零，但由于反射率的时效变化特性关系，未必就能满意。因此，历来的组成物，尽管其初期特性能满足要求，但存在时效变化大的缺点。
本发明的为解决上述问题，提供了一种蒸镀用的氧化钇组成物。此外，另一个目的是提供一种制造化学上安定的、耐久性好的、反射防止性能优良的蒸镀膜的方法和材料。
涉及本发明的蒸镀用氧化钇组合物是一种含有氧化钛和氧化锆的组合物。另外，涉及另一个发明的反射防止膜的制造方法是使用了含有氧化钛和氧化锆的蒸镀用氧化钇的方法。
用本发明的蒸镀用氧化钇组成物，可获得折射率可接近于理论
上的要求值1.87的薄膜，且时效变化也变小了。
实施例
在研究对于生成用于GaAs或Si的反射防止膜所必需的蒸镀材料时，弄清了作为时效变化小的材料，Y2O3是一种优良的材料。然而，由于它的折射率略小一点，不是最合适的，因此要避免单独使用Y2O3。
因此，把Y2O3和折射率大的物质组合起来，以得到所希望的材料。在想要得到混合膜时，希望各种物质各自的蒸气压要接近。那是因为在蒸镀中蒸镀材料的组份会起变化。因为在2300℃～2600℃的温度范围内，Y2O3和ZrO2的蒸气压几乎是相等的，所以以Y2O3和ZrO2作为主要的混合物质，再为了补正折射率起见添加一些TiO2能减轻ZrO2所特有的在膜厚方向的组份的不均匀性。
当使表面反射率R为零时，表面反射率R随薄膜的折射率nf变动的变化最小。也就是说，使表面反射率为零是得到时效变化小的反射防止膜的必要条件。
如式（1）所示，表面反射率R是薄膜的折射率nf的二次函数：
R＝（ (n0·n3-nf 2)/(n0·n3+nf 2) )2……（1）
式中，no是入射介质的折射率，当λ射介质是空气时，no＝1.00。ns是基片的折射率，当基片是GaAs时，ns＝3.5。
把（1）式简化就成了（2）式：
R∝（nf-1.87）2……（2）
表面反射率R随薄膜的折射率nf的变化而引起的变化如式（3）所示，可理解为nf越接近1.88，变化率越小。
(dR)/(dnf) ∝2(nf-1.87) ……（3）
单独用Y2O3所得到的表面反射率R（%）从图1可知如表1所示。
表1
物质 基片的折射率 表面反射率
nsR（%）
C-Si 3.3 0.25
GaAs 3.5 0.6
a-Si 3.8 1.4
如设计一种混合膜，使所得的折射率可满足以下条件，即表面反射率R为0.25%以下，则根据图1，式（4）可成立。
1.732＜nf＜2.048 ……（4）
又，可满足表面反射率为0.05%以下的nf，从图2可知式（5）可成立：
1.775＜nf＜1.992 ……（5）
根据图3，可满足（4）式或（5）式的TiO2和ZrO2的混合率如表2所示。
表2
表面反射率 TiO2ZrO2
R（%） （wt%） （wt%）
R≤0.25 0～7.3 0～90
R≤0.25 0.5～4.8 0～80
但是，由图3可明显地得出表2中的TiO2和ZrO2的含量比例是相互对应的，即，若满足R≤0.05（也即，1.775＜nf＜1.992）;TiO2和ZrO2的含量应在附图4中的ABC范围内;图4中的A点：TiO2＝4.8%，ZrO2＝0%，B点：TiO2＝0.5%，ZrO2＝0%;以及C点：TiO2＝0.5%ZrO2＝80%;并且，A、B、C三点分别对应于图3中A′、
B′、C′三点的TiO2和ZrO2含量;也就是说，只有图4中A、B、C、范围内的TiO2和ZrO2含量才能保证R≤0.05。
实施例1
在氧化钇中加入重量比为10%的氧化锆、1%的氧化钛后使之充分混合，以500kg/cm2的压力冲压成型后，在约1300℃下进行约3小时的烧结从而得到蒸镀试验用的片剂（タブレト）。接着把这个试剂填入配置在蒸镀装置中的电子枪里。排气至真空度达6.666×10-3Pa后，也注意玻璃基片的上面和GaAs基片上的情况，边加大电子枪的输出功率，提高片剂的温度使其溶化，再在基片温度300℃下进行蒸镀直至光学膜厚达到nd＝120nm。被蒸镀于玻璃基片上的本试剂的蒸镀膜，其折射率，n＝1.84，也无吸收，对GaAs基片的粘着力大，而且化学上安定、耐久性好，在GaAs基片上的表面反射率几乎为0%，而且作为长时间内能保持其初期特性的反射防止用材料得到了极其满意的薄膜。
实施例2
在氧化钇中加入重量比为20%的氧化锆和1.5%氧化钛后，用上述实施例同样的方法得到片剂。用与上述实施例同样的方法，在基片温度120℃下，在GaAs-GaAlAs系的激光二极管的端面上进行蒸镀的结果，激光发射面的反射率几乎成为零，开始显示出SLD（超级发光二极管）的特性。
这个特性可持续较长时间。
比较例
在氧化钇中加入重量比为20%的氧化锆和8%的氧化钛，以上述实施例1同样的方法得到片剂。取基片温度为120℃，其它的条件以与实施例2同样的方法在GaAs-GaAlAs系的激光二极管的端面上进行蒸镀。其结果为，表面反射率显示约1.2%，没能得到作为SLD元件的特性。
从上记的结果可见，蒸镀用氧化钇组合物中所含有的氧化锆的量为0～90%重量，0～80%重量为好;含有的氧化钛的量为0～7.3%重量，0.5～4.8%重量为好。
作为被蒸镀物的另一个适用例，可以在由Si半导体制成的发光二极管、光电二极管等上用作反射防止膜。
在上述实施例中，是就电子枪加热的方法进行说明的，但用作为溅射的靶子的方法也可期待同样的效果。
如上所述，由于本发明由Si或GaAs制成的半导体的折射率来生成反射防止膜而把由氧化钇、氧化锆、氧化钛组成的混合组合物作蒸镀材料，故能使被蒸镀物上的表面反射率几乎为零。此外，由于时效变化小，动作时间可以延长。
下面是对附图的简单说明。图1和图2是薄膜的折射率与表面反射率的关系的示意图，图3是TiO2的混合量与薄膜的折射率的关系的示意图。
Claims (1)
- 一种在硅或砷化镓基底上制备改射防止膜的方法，其特征在于在氧化钇中加入0.5-4.8%(重量)氧化钛和80-0%(重量)氧化锆(在图4中所示的ABC范围内的氧化钛和氧化锆)经充分混合后以500Kg/cm2的压力冲压成型后，在约1300℃下进行3小时的烧结得到蒸镀用的片剂，将所述的片剂配置在蒸镀装置中的电子枪里，排气至真空度达6.666×10-3帕，并加大电子枪的输出功率，提高片剂的温度使之熔化，再在基底温度为120°-300℃下进行蒸镀。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62023946A JPS63192856A (ja) | 1987-02-04 | 1987-02-04 | 蒸着用酸化イツトリウム組成物及び反射防止膜の製造方法 |
| JP23946/87 | 1987-02-04 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN87107819A CN87107819A (zh) | 1988-08-17 |
| CN1017164B true CN1017164B (zh) | 1992-06-24 |
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| CN87107819A Expired CN1017164B (zh) | 1987-02-04 | 1987-11-12 | 在硅或砷化镓基底上制备反射防止膜的方法 |
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| JP (1) | JPS63192856A (zh) |
| KR (1) | KR910008716B1 (zh) |
| CN (1) | CN1017164B (zh) |
| DE (2) | DE3890060C2 (zh) |
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| WO (1) | WO1988005963A1 (zh) |
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| JP2850371B2 (ja) * | 1989-06-19 | 1999-01-27 | 松下電器産業株式会社 | 画像出力装置 |
| CN102140621A (zh) * | 2011-03-10 | 2011-08-03 | 苏州大学 | 一种致密复合二氧化钛薄膜的制备方法 |
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| US4246043A (en) * | 1979-12-03 | 1981-01-20 | Solarex Corporation | Yttrium oxide antireflective coating for solar cells |
| DE3613501A1 (de) * | 1986-04-22 | 1987-10-29 | Stefan Dipl Ing Donnerhack | Verfahren zur antikatalytischen beschichtung von thermoelementen |
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| Publication number | Publication date |
|---|---|
| DE3890060C2 (de) | 1990-08-16 |
| CN87107819A (zh) | 1988-08-17 |
| KR910008716B1 (ko) | 1991-10-19 |
| SE8803506L (sv) | 1988-10-03 |
| DE3890060T (zh) | 1989-03-23 |
| JPS63192856A (ja) | 1988-08-10 |
| SE8803506D0 (sv) | 1988-10-03 |
| KR890700927A (ko) | 1989-04-28 |
| WO1988005963A1 (en) | 1988-08-11 |
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