技术领域technical field
本发明提供一种制备柔性硅基砷化镓薄膜电池的方法，属于薄膜电池制造领域。The invention provides a method for preparing a flexible silicon-based gallium arsenide thin-film battery, which belongs to the field of thin-film battery manufacturing.
背景技术Background technique
GaAs电池具有稳定性好、抗辐照能力强、光电转换效率最高等特特点，是一种最具潜质的空间能源产品。目前，美日欧等西方发达国家竞相开发高效、轻质的GaAs薄膜电池，满足各自航天军事领域以及未来太空电站建设的需要；同时柔性的高效砷化镓电池也能满足地面的特殊应用。GaAs是一种直接带隙半导体材料，可以做成多结电池，有效提高光电转换效率。GaAs battery has the characteristics of good stability, strong radiation resistance, and the highest photoelectric conversion efficiency. It is a space energy product with the most potential. At present, Western developed countries such as the United States, Japan and Europe are competing to develop high-efficiency and light-weight GaAs thin-film batteries to meet the needs of their respective aerospace and military fields and future space power station construction; at the same time, flexible and high-efficiency GaAs batteries can also meet special applications on the ground. GaAs is a direct bandgap semiconductor material, which can be made into multi-junction cells to effectively improve the photoelectric conversion efficiency.
传统的GaAs/Ge电池，由于基底采用镓、锗等元素的稀有，外延设备和工艺复杂，使得高效GaAs电池不但制造成本高昂，而且质量大，难以实现大规模应用，尤其是航天事业。而Si基GaAs电池，由于硅元素在地壳中储量极为丰富，提炼难度较少，生产成本较低，可用于开发低成本的多结高效GaAs电池，同时轻、薄且柔性的基底能满足未来卫星、空间站以及太空（月球）基地建设的大规模能源供应需要。因此，开发高效、低成本的柔性多结GaAs薄膜电池是未来航空航天的必然选择。Traditional GaAs/Ge batteries, due to the rare elements such as gallium and germanium used as substrates, and complex epitaxy equipment and processes, make high-efficiency GaAs batteries not only high in manufacturing costs, but also high in quality, making it difficult to achieve large-scale applications, especially in the aerospace industry. As for Si-based GaAs batteries, since silicon is extremely abundant in the earth's crust, it is less difficult to refine and lower in production cost. It can be used to develop low-cost multi-junction high-efficiency GaAs batteries. At the same time, the light, thin and flexible substrate can meet the needs of future satellites. , space station and space (moon) base construction of large-scale energy supply needs. Therefore, the development of high-efficiency and low-cost flexible multi-junction GaAs thin-film batteries is an inevitable choice for future aerospace.
发明内容Contents of the invention
本发明的目的在于：提供一种制备柔性硅基砷化镓薄膜电池的方法，制备出薄膜电池总厚度约为50微米，柔性、可卷曲，比功率大于2000W/Kg的优质电池，该电池在航天电源领域有着独特的优势，同时其高效、柔性的特点也在地面移动电源如单兵作战等领域有特殊应用。同时，以单晶硅替代单晶锗、单晶砷化镓作为衬底，能大大降低多结砷化镓电池的成本。The object of the present invention is to provide a method for preparing flexible silicon-based gallium arsenide thin-film batteries, to prepare a high-quality battery with a total thickness of about 50 microns, flexibility and rollability, and a specific power greater than 2000W/Kg. The space power supply field has unique advantages, and its high efficiency and flexibility are also used in special applications in ground mobile power supplies such as individual combat. At the same time, using single crystal silicon instead of single crystal germanium and single crystal gallium arsenide as the substrate can greatly reduce the cost of multi-junction gallium arsenide cells.
为实现上述目的，本发明的技术方案是：For realizing the above object, technical scheme of the present invention is:
一种柔性硅基砷化镓电池的制备方法，包括以下步骤：A method for preparing a flexible silicon-based gallium arsenide battery, comprising the following steps:
1）在850℃-900℃的温度下，干氧氧化30min-60min，在硅衬底A和硅衬底B上分别生长SiO2层；所述SiO2层的厚度为20nm-50nm；1) At a temperature of 850°C-900°C, dry oxygen oxidation for 30min-60min, and grow SiO2 layers on silicon substrate A and silicon substrate B respectively; the thickness of the SiO2 layer is 20nm-50nm;
2）经过清洗后将硅衬底A的SiO2层界面和硅衬底B的SiO2层界面键合，然后从室温升温至750℃-850℃，然后在750℃-850℃热处理时间60min-120min；2) After cleaning, bond theSiO2 layer interface of silicon substrate A with theSiO2 layer interface of silicon substrate B, then raise the temperature from room temperature to 750°C-850°C, and then heat treatment at 750°C-850°C for 60min- 120min;
3）热处理后，经过粗磨、粗抛和精抛，将硅衬底A的厚度减薄，制备成厚度小于48微米的超薄硅衬底A；3) After the heat treatment, the thickness of the silicon substrate A is reduced through rough grinding, rough polishing and fine polishing, and an ultra-thin silicon substrate A with a thickness of less than 48 microns is prepared;
4）经过清洗后，采用超高真空化学气相沉积，在600℃-700℃的温度下在超薄硅衬底A表面生长Ge-Si缓冲层；所述Ge-Si缓冲层的厚度为1-2微米；4) After cleaning, use ultra-high vacuum chemical vapor deposition to grow a Ge-Si buffer layer on the surface of the ultra-thin silicon substrate A at a temperature of 600°C-700°C; the thickness of the Ge-Si buffer layer is 1- 2 microns;
5）然后采用MOCVD在Ge-Si缓冲层上依次生长Ge电池层、隧道层、GaAs电池层、隧道结层、GaInP电池层、窗口层和接触层；5) Then use MOCVD to sequentially grow Ge battery layer, tunnel layer, GaAs battery layer, tunnel junction layer, GaInP battery layer, window layer and contact layer on the Ge-Si buffer layer;
6）采用光刻胶将硅衬底A层、Ge-Si缓冲层、Ge电池层、隧道层、GaAs电池层、隧道结层、GaInP电池层、窗口层和接触层包覆，采用碱腐蚀去除下表面硅衬底B，采用氢氟酸腐蚀去除SiO2层；6) Cover silicon substrate A layer, Ge-Si buffer layer, Ge battery layer, tunnel layer, GaAs battery layer, tunnel junction layer, GaInP battery layer, window layer and contact layer with photoresist, and remove them by alkali etching The silicon substrate B on the lower surface is etched with hydrofluoric acid to remove the SiO2 layer;
7）去除光刻胶；7) Remove the photoresist;
8）制作电极，电极加固；8) Make electrodes and reinforce them;
9）镀减反射膜层。9) Plating anti-reflection coating.
其中，步骤1）中所述硅衬底A优选为半导体级P型硅，硅衬底B优选为太阳能级P型硅。Wherein, the silicon substrate A in step 1) is preferably semiconductor-grade P-type silicon, and the silicon substrate B is preferably solar-grade P-type silicon.
步骤1）中所述SiO2层厚度优选为40nm-50nm。The thickness of the SiO2 layer in step 1) is preferably 40nm-50nm.
步骤2）中所述室温优选20℃-25℃。The room temperature in step 2) is preferably 20°C-25°C.
步骤3）中所述超薄硅衬底A的厚度优选为40微米-48微米。The thickness of the ultra-thin silicon substrate A in step 3) is preferably 40 microns-48 microns.
步骤4）中所述Ge-Si缓冲层优选Ge的组分含量由内至外按比例增加，Si的组分含量由内至外同比例减少，实现从Si到Ge的过渡；其中靠近超薄硅衬底A的一侧为内。In the Ge-Si buffer layer described in step 4), the composition content of Ge preferably increases proportionally from the inside to the outside, and the composition content of Si decreases in the same proportion from the inside to the outside, so as to realize the transition from Si to Ge; wherein the ultrathin One side of the silicon substrate A is inside.
步骤6）优选腐蚀硅衬底B采用质量浓度为20%-50%的KOH溶液，腐蚀SiO2层采用质量浓度为10%-20%的HF溶液。Step 6) Preferably, a KOH solution with a mass concentration of 20%-50% is used for etching the silicon substrate B, and an HF solution with a mass concentration of 10%-20% is used for etching the SiO2 layer.
步骤8）所述制作电极优选为：上下表面的电极采用蒸镀技术或者激光转印技术来制备，上表面电极材料是银，图形为栅线结构；下表面电极材料为铝，全部覆盖。Step 8) The fabrication of electrodes is preferably as follows: the electrodes on the upper and lower surfaces are prepared by evaporation technology or laser transfer printing technology, the electrode material on the upper surface is silver, and the pattern is a grid line structure; the electrode material on the lower surface is aluminum, which is completely covered.
步骤9）所述减反射膜优选为硫化锌和氟化镁的双层减反射膜结构。Step 9) The anti-reflection film is preferably a double-layer anti-reflection film structure of zinc sulfide and magnesium fluoride.
与现有技术相比，本发明的优势是：Compared with prior art, the advantage of the present invention is:
1、 本发明的方法可以制备出薄膜电池总厚度小于50微米，柔性、可卷曲，单片面积可以大于80cm2，转换效率超过30%，比功率大于2000W/Kg的超薄高效电池。1. The method of the present invention can prepare a thin-film battery with a total thickness of less than 50 microns, flexible and rollable, an ultra-thin high-efficiency battery with a single sheet area greater than 80cm2 , a conversion efficiency of more than 30%, and a specific power greater than 2000W/Kg.
2、 本发明的方法制备的电池在航天电源领域有着独特的优势，同时其高效、柔性的特点也在地面移动电源如单兵作战等领域有特殊应用。2. The battery prepared by the method of the present invention has unique advantages in the field of aerospace power supplies, and at the same time, its high efficiency and flexibility also have special applications in the fields of ground mobile power supplies such as individual combat.
3、 本发明的方法制备的电池以单晶硅替代单晶锗、单晶砷化镓作为衬底，能大大降低多结砷化镓电池的成本。3. The battery prepared by the method of the present invention uses single crystal silicon instead of single crystal germanium and single crystal gallium arsenide as the substrate, which can greatly reduce the cost of the multi-junction gallium arsenide battery.
4、 本发明的方法制备的电池以柔性的超薄硅作为最终衬底，能获得极大的比功率（>2000W/Kg），大大降低空间电源的发射成本。4. The battery prepared by the method of the present invention uses flexible ultra-thin silicon as the final substrate, which can obtain extremely high specific power (>2000W/Kg), and greatly reduce the launch cost of space power.
附图说明Description of drawings
图1 是超薄硅衬底的制备流程示意图；Figure 1 is a schematic diagram of the preparation process of an ultra-thin silicon substrate;
图2是柔性硅基砷化镓薄膜电池的制备流程示意图；Figure 2 is a schematic diagram of the preparation process of a flexible silicon-based gallium arsenide thin film battery;
图3是本发明制备的柔性硅基砷化镓薄膜电池的结构示意图；Fig. 3 is a schematic structural view of a flexible silicon-based gallium arsenide thin-film battery prepared by the present invention;
其中，1是硅硅片A，2是硅硅片B，3是SiO2层，4是减薄后的硅片A（厚度<48um），5是Ge-Si缓冲层，6是外延层，7是光刻胶，8是正面电极，9是背面电极，10是减反射膜层 ；11是欧姆接触层，12是窗口层，13是GaInP电池，14是隧道结，15是GaAs电池，16是Ge电池 ，17是键合后的SiO2层。Among them, 1 is silicon silicon wafer A, 2 is silicon silicon wafer B, 3 is SiO2 layer, 4 is thinned silicon wafer A (thickness <48um), 5 is Ge-Si buffer layer, 6 is epitaxial layer, 7 is a photoresist, 8 is a front electrode, 9 is a back electrode, 10 is an anti-reflection film layer; 11 is an ohmic contact layer, 12 is a window layer, 13 is a GaInP battery, 14 is a tunnel junction, 15 is a GaAs battery, 16 is the Ge cell and 17 is theSiO2 layer after bonding.
具体实施方式Detailed ways
为了进一步说明本发明的结构和特征，以下结合实施例及附图对本发明作进一步说明。In order to further illustrate the structure and features of the present invention, the present invention will be further described below in conjunction with the embodiments and accompanying drawings.
实施例1：Example 1:
如图1和图2所示，本发明提供一种制备柔性硅基砷化镓薄膜电池的方法，包括以下步骤：As shown in Figure 1 and Figure 2, the present invention provides a method for preparing a flexible silicon-based gallium arsenide thin film battery, comprising the following steps:
1）采用热氧化法，在硅衬底A和硅衬底B上生长50nm厚的SiO2层，温度900度；2）经过15%的HCl溶液洗后，兆声处理，然后将硅衬底A和B的SiO2界面在键合设备中完成键合，然后从室温逐渐升温至850℃，在850℃下热处理时间60min；1) Using the thermal oxidation method, grow a 50nm thick SiO2 layer on the silicon substrate A and silicon substrate B at a temperature of 900 degrees; 2) After washing with 15% HCl solution, megasonic treatment, and then the silicon substrate The SiO2 interface of A and B is bonded in the bonding equipment, and then the temperature is gradually raised from room temperature to 850°C, and the heat treatment time is 60min at 850°C;
3）经过粗磨、粗抛和精抛，将硅衬底A减薄至45-48微米厚，制作成超薄硅衬底A；3) Thin the silicon substrate A to a thickness of 45-48 microns after rough grinding, rough polishing and fine polishing, and make an ultra-thin silicon substrate A;
4）清洗后采用超高真空CVD（VHT-CVD），650度，在硅衬底A表面生长Ge-Si缓冲层2微米；4) After cleaning, use ultra-high vacuum CVD (VHT-CVD) at 650 degrees to grow a 2 micron Ge-Si buffer layer on the surface of silicon substrate A;
5）采用MOCVD在Ge-Si缓冲层上依次生长Ge电池层、隧道层、GaAs电池层、隧道结层、GaInP电池层、窗口层和接触层。（如图3所示）5) The Ge cell layer, the tunnel layer, the GaAs cell layer, the tunnel junction layer, the GaInP cell layer, the window layer and the contact layer are sequentially grown on the Ge-Si buffer layer by MOCVD. (As shown in Figure 3)
6）采用光刻胶将上表面及侧面进行保护，采用20% KOH溶液腐蚀下表面硅衬底B，采用10%氢氟酸腐蚀SiO2层；6) Use photoresist to protect the upper surface and side surfaces, use 20% KOH solution to etch the lower surface silicon substrate B, and use 10% hydrofluoric acid to etch the SiO2 layer;
7）去除光刻胶；7) Remove the photoresist;
8）采用激光转印技术印刷正面Ag电极和背面Al背场，烘干炉600度下电极加固。8) The front Ag electrode and the back Al back field are printed by laser transfer printing technology, and the electrode is strengthened in a drying oven at 600 degrees.
9）镀ZnS、MgF4减反射膜。9) ZnS, MgF4 anti-reflection coating.
电池的最终结构示意图如图3所示，性能对比数据见表1。The schematic diagram of the final structure of the battery is shown in Figure 3, and the performance comparison data are shown in Table 1.
表1 电池性能对比实验数据Table 1 Experimental data of battery performance comparison
实施例2：Example 2:
本发明提供一种制备柔性硅基砷化镓薄膜电池的方法，包括以下步骤：The invention provides a method for preparing a flexible silicon-based gallium arsenide thin film battery, comprising the following steps:
1）在硅衬底A和硅衬底B上生长30nm厚的SiO2层，温度850度；1) Grow a 30nm thick SiO2 layer on silicon substrate A and silicon substrate B at a temperature of 850 degrees;
2）经过20%的HCl溶液洗后，兆声处理，然后将硅衬底A和B的SiO2界面在键合设备中完成键合，然后从室温逐渐升温至800℃，800℃热处理时间为120min；2) After washing with 20% HCl solution, megasonic treatment, and then the SiO2 interface of silicon substrate A and B is bonded in the bonding equipment, and then the temperature is gradually raised from room temperature to 800°C, and the heat treatment time at 800°C is 120min;
3）经过粗磨、粗抛和精抛，将硅衬底A减薄至40微米厚，制作成超薄硅衬底A；3) Thin the silicon substrate A to a thickness of 40 microns after rough grinding, rough polishing and fine polishing, and make an ultra-thin silicon substrate A;
4）清洗后采用超高真空CVD（VHT-CVD），700度，在硅衬底A表面生长Ge-Si缓冲层2微米；4) After cleaning, use ultra-high vacuum CVD (VHT-CVD) at 700 degrees to grow a 2 micron Ge-Si buffer layer on the surface of silicon substrate A;
5）采用MOCVD在Ge-Si缓冲层上依次生长Ge电池层、隧道层、GaAs电池层、隧道结层、GaInP电池层、窗口层和接触层。（如图3所示）5) The Ge cell layer, the tunnel layer, the GaAs cell layer, the tunnel junction layer, the GaInP cell layer, the window layer and the contact layer are sequentially grown on the Ge-Si buffer layer by MOCVD. (As shown in Figure 3)
6）采用光刻胶将上表面及侧面进行保护，采用50% KOH溶液腐蚀下表面硅衬底B，采用20%氢氟酸腐蚀SiO2层；6) Use photoresist to protect the upper surface and side surfaces, use 50% KOH solution to etch the silicon substrate B on the lower surface, and use 20% hydrofluoric acid to etch the SiO2 layer;
7）去除光刻胶；7) Remove the photoresist;
8）采用激光转印技术印刷正面Ag电极和背面Al背场，烘干炉600度下电极加固。8) The front Ag electrode and the back Al back field are printed by laser transfer printing technology, and the electrode is strengthened in a drying oven at 600 degrees.
9）镀ZnS、MgF4减反射膜。9) ZnS, MgF4 anti-reflection coating.
电池的最终结构示意图如图3所示，性能同实施例1。The final structural diagram of the battery is shown in FIG. 3 , and its performance is the same as that of Example 1.
以上所述的具体实施方式，对本发明的目的、技术方案和有益效果进行了进一步的详细说明，所应理解的是，以上所述仅为本发明的具体实施方案而已，并不用于限制本发明，凡在本发明的精神和原则之内，所做的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。The specific embodiments described above have further described the purpose, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above descriptions are only specific embodiments of the present invention and are not intended to limit the present invention. , Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included within the protection scope of the present invention.
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