WO2012058822A1 - Method for passivating black silicon - Google Patents

Method for passivating black silicon Download PDF

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Publication number
WO2012058822A1
WO2012058822A1 PCT/CN2010/078462 CN2010078462W WO2012058822A1 WO 2012058822 A1 WO2012058822 A1 WO 2012058822A1 CN 2010078462 W CN2010078462 W CN 2010078462W WO 2012058822 A1 WO2012058822 A1 WO 2012058822A1
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Prior art keywords
gas
black silicon
passivation
silicon
plasma
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PCT/CN2010/078462
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French (fr)
Chinese (zh)
Inventor
夏洋
刘邦武
李超波
刘杰
李勇滔
陈瑶
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中国科学院微电子研究所
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Publication of WO2012058822A1 publication Critical patent/WO2012058822A1/en

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
    • H01L31/186—Particular post-treatment for the devices, e.g. annealing, impurity gettering, short-circuit elimination, recrystallisation
    • H01L31/1868—Passivation
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34—Nitrides
    • C23C16/345—Silicon nitride
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • the present invention relates to the field of optoelectronic device manufacturing technology, and in particular, to a black silicon passivation method. Background technique
  • Black silicon is a revolutionary new material structure in the electronics industry, usually referred to as a silicon surface or a silicon-based film with a high absorption rate.
  • Chinese Patent Specification CN 101734611 A (Publication Date: June 16, 2010) discloses a method for preparing black silicon based on maskless deep reactive ion etching, the principle of which is to immerse the silicon wafer in a plasma atmosphere, using The silicon wafer is alternately processed by etching and passivation, and the surface of the silicon wafer forms an inverted pyramid structure after several times of alternating processing.
  • Black silicon has a wide range of applications in many fields due to its special structure.
  • Eric Mazur et al. when studying the optoelectronic properties of black silicon, surprisingly found that this surface microstructured silicon material has peculiar optical properties, and it absorbs almost all of the near-ultra-near-infrared light (wavelength 0.25-2.5 um). It has good visible and infrared luminescent properties, and also has good field emission characteristics.
  • the strong absorption properties of black silicon make it an ideal material for the preparation of high-efficiency solar cells.
  • black silicon has a non-flat inverted pyramid, a forest-like spike or a needle-like knot due to its surface.
  • the structure of the surface area of the black silicon has a large surface state, and the surface has many dangling bonds, thereby reducing the conversion efficiency of the solar cell prepared by the black silicon.
  • black silicon has become more difficult to pass black silicon passivation due to its inverted pyramid, forest-like nail shape or needle shape.
  • the technical problem to be solved by the present invention is to provide a black silicon passivation method for reducing the surface density of black silicon.
  • a black silicon passivation method comprising:
  • the black silicon prepared by the plasma immersion ion implantation technique is placed in a chamber of the passivation device; the process parameter of the passivation device is adjusted to reach a preset working range, and the mixed gas is introduced into the passivation device,
  • the mixed gas includes a reaction gas
  • a passivation film is deposited on the surface of the black silicon by plasma enhanced chemical vapor deposition.
  • the step of depositing a passivation film on the surface of the black silicon by using plasma enhanced chemical vapor deposition specifically includes:
  • the reaction gas is reacted in a plasma atmosphere, and a product is deposited on the surface of the black silicon to form a passivation film.
  • the process parameters include the background pressure and working pressure of the chamber, the temperature of the sample stage, the flow rate of the mixed gas, the ratio, the velocity of the extracted gas, and the output power and frequency of the plasma power source.
  • the background pressure of the chamber ranges from 10 to 12 Pa to 1 Pa, and the working pressure range is 10- 3 Pa ⁇ 10000Pa, sample temperature in the range of 10 to 1000 units.
  • C the output power of the plasma power supply is 0 ⁇ 2000w, and the frequency is 13.56MHz.
  • the passivation film is a silicon nitride or silicon oxide film.
  • the reaction gas includes silane and ammonia gas, or silane and nitrogen; the silane gas flow rate is 1 to 1000 sccm, the ammonia The gas or nitrogen gas flow rate is from 1 to 1000 sccm, and the volume ratio of the silane to ammonia or nitrogen is from 0.01 to 100.
  • the reaction gas includes silane and laughing gas; the silane gas flow rate is l ⁇ 1000 sccm, and the laughing gas flow rate is l ⁇ 1000 sccm, the volume ratio of the silane to the laughing gas is 0.01 to 100.
  • the mixed gas further includes a dilution gas for diluting the silane; and the dilution gas is one or more of argon gas, helium gas, nitrogen gas and hydrogen gas.
  • the invention adopts plasma enhanced chemical vapor deposition method to passivate black silicon prepared by plasma immersion ion implantation technology, saturates a large number of dangling bonds on the surface of black silicon, and reduces the surface state density of black silicon, thereby improving utilization. Conversion efficiency of solar cells prepared from black silicon. DRAWINGS
  • FIG. 1 is a flow chart of a method for passivating black silicon by plasma enhanced chemical vapor deposition according to an embodiment of the present invention
  • FIG. 2 is a scanning electron microscope top view of a black silicon structure prepared by plasma immersion ion implantation
  • Figure 3 is another black silicon structure scanning electron microscope prepared by plasma immersion ion implantation. Topographical map
  • Figure 4 is a topographical view of another black silicon structure scanning electron microscope prepared by plasma immersion ion implantation
  • FIG. 5 is a top view of a scanning electron microscope after passivation of black silicon according to an embodiment of the present invention
  • FIG. 6 is a schematic diagram of a black silicon single-sided passivation structure according to an embodiment of the present invention.
  • FIG. 7 is a schematic diagram of a black silicon double-sided passivation structure in an embodiment of the present invention. detailed description
  • Plasma Enhanced Chemistry Vapor Deposition is a method in which a sample is placed on a sample stage in a deposition chamber, a process gas is introduced into the chamber, and a plasma glow discharge generates a plasma under the action of a plasma power source.
  • the reaction gas is more susceptible to decomposition, dissociation and ionization, thereby increasing the activity of the reactants, and the product is adsorbed on the surface of the sample to form a thin film.
  • the main mechanism for the passivation of black silicon by the PECVD growth film is that the mixed gas introduced into the deposition chamber is discharged under the action of the plasma power source to generate plasma, and the reaction gases in the mixed gas such as silane (SiH 4 ) and ammonia are used. Gas (NH 3 ) is easily reacted in a plasma atmosphere to form SiN x and H 2 , and SiN x is deposited on the surface of black silicon.
  • the surface passivation effect of the SiN x layer is attributed to the relatively low surface state density and appropriate density.
  • the surface of the fixed charge; in the plasma atmosphere and the reaction process contains a large amount of H, SiN x : H H through the vacancy diffusion mechanism and hydrogen molecular diffusion mechanism can saturate the surface of the black silicon material and the dangling bonds in the body, thus completing the black silicon Passivation.
  • an embodiment of the present invention provides a method for passivating black silicon by plasma enhanced chemical vapor deposition, the method comprising: Step 210, placing black silicon prepared by plasma immersion ion implantation technology in a deposition chamber of the passivation device;
  • the passivation device is a plasma enhanced chemical vapor deposition device, and black silicon is placed in the deposition chamber of the device and placed on the sample stage;
  • Step 212 Adjust a process parameter of the passivation device to a preset working range, where the process parameters include a background pressure and a working pressure of the deposition chamber, a temperature of the sample stage, a flow rate of the mixed gas, and a ratio , the speed of the extracted gas, and the output power and frequency of the plasma power supply; these process parameters can be preset according to the actual conditions during processing, or can be modified on-site as needed during the processing, so that these parameters meet the process requirements.
  • the process parameters include a background pressure and a working pressure of the deposition chamber, a temperature of the sample stage, a flow rate of the mixed gas, and a ratio , the speed of the extracted gas, and the output power and frequency of the plasma power supply; these process parameters can be preset according to the actual conditions during processing, or can be modified on-site as needed during the processing, so that these parameters meet the process requirements.
  • the background pressure of the deposition chamber may range from 10 to 12 Pa to 1 Pa, preferably from 10 to 8 Pa to 10 to 3 Pa, and more preferably from 10 to 10 7 Pa ⁇ 10 - 5 Pa
  • the working pressure of the deposition chamber may range from 10 - 3 Pa to 1000OOPa, preferably from 0.1 Pa to lOOOPa, more preferably from 0.5 Pa to 500 Pa;
  • the temperature of the sample stage may range from 10 to 1000 ° C, preferably from 100 to 500 ° C, and more preferably from 250 to 450. C;
  • the output power of the plasma power source is 0 ⁇ 2000w, and the frequency is 13.56MHz;
  • the gas to be introduced is a mixed gas, including a reaction gas, for example, a silicon nitride film deposited on the black silicon, the reaction gas may be SiH 4 and NH 3 , or SiH 4 and N 2 , and the flow rate of the SiH 4 gas may be l ⁇ 1000sccm, preferably 10 ⁇ 300 sccm, NH 3 or N 2 gas flow rate is l ⁇ 1000sccm, preferably 10 ⁇ 300 sccm, and the volume ratio of silane SiH 4 to NH 3 or N 2 is 0.01 ⁇ 100
  • the mixed gas may further include a diluent gas
  • the SiH 4 may be diluted with one or more of N 2 , Ar, He, H 2 , preferably SiH 4 and NH diluted with Ar 3 is a process gas, and the volume ratio of the diluted SiH 4 to NH 3 gas is 0.01 to 100, preferably 0.1 to 10, and the flow rate of the diluted Si
  • the silicon oxide film is deposited on the black silicon, and the reaction gas may be silane SiH 4 and laughing gas N 2 0.
  • the flow rate of the SiH 4 gas is 1 to 1000 sccm, preferably 10 to 300 sccm, and N 2 0
  • the gas flow rate is from 1 to 1000 sccm, preferably from 10 to 300 sccm, and the volume ratio of silane SiH 4 to N 2 0 is from 0.01 to 100, preferably from 0.1 to 10;
  • a diluent gas may be further included in the mixed gas to which the silicon oxide film is deposited, and the SiH 4 may be diluted with one or more of N 2 , Ar, He, H 2 , preferably Ar diluted SiH 4 and N 2 0 are process gases, and the volume ratio between the diluted SiH 4 and N 2 0 gas is 0.01 to 100, preferably 0.1 to 10, and the diluted SiH 4 and N 2 0
  • the flow rate of the gas may be from 1 to 1000 sccm, preferably from 10 to 300 sccm;
  • Step 214 the passivation device gas discharge generates a plasma
  • Step 216 the reaction gas reacts in a plasma atmosphere
  • Step 218 a part of the reaction product is deposited on the surface of the black silicon to form a silicon nitride or silicon oxide passivation film; the low surface state density of the film and the saturation of the H on the black silicon surface and the internal dangling bonds during the deposition process, so that the black silicon surface The density of states is reduced, thereby achieving passivation of black silicon.
  • Figure 2, Figure 3, and Figure 4 show the shape of a black silicon structure scanning electron microscope.
  • Fig. 5 is a scanning electron microscope topographical view of the black silicon after passivation using an embodiment of the present invention.
  • 6 and 7 are schematic diagrams showing the structure of single-side passivation and double-sided passivation of a black silicon structure by using an embodiment of the present invention, 301 is black silicon prepared by plasma immersion ion implantation technology, and 302 is an embodiment using the present invention.

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Abstract

Disclosed is a method for passivating a black silicon, which comprises: positioning a black silicon in a chamber of a passivation apparatus; adjusting process parameters of the passivation apparatus to a preset working range; feeding a gas mixture into the passivation apparatus, wherein the gas mixture includes reaction gases; depositing a passivation film on the surface of the black silicon by plasma enhanced chemical vapour deposition. The method reduces the surface state density of the black silicon and thus improves the conversion efficiency of the solar cell which is made of black silicon.

Description

一种黑娃純化方法  Black wax purification method
技术领域 Technical field
本发明涉及光电子器件制造技术领域， 尤其是涉及一种黑硅钝化方法。 背景技术  The present invention relates to the field of optoelectronic device manufacturing technology, and in particular, to a black silicon passivation method. Background technique
黑硅是一种电子产业革命性的新型材料结构， 通常是指吸收率很高的硅表 面或硅基薄膜。  Black silicon is a revolutionary new material structure in the electronics industry, usually referred to as a silicon surface or a silicon-based film with a high absorption rate.
20世纪 90年代末，哈佛大学 Eric Mazur教授研究组在飞秒激光与物质相互 作用研究的过程中， 发现利用飞秒激光在一定气体环境下照射硅片可在硅表面 激光辐照区产生微米量级的尖峰结构。 接着他们发展了这种微观构造硅表面的 新技术 _利用飞秒激光在一定气体环境下刻蚀硅， 制备出具有一定刻蚀面积的 新材料， 原本是灰色有光泽的硅表面在刻蚀过的地方肉眼看去完全变成了黑色， 因而这种新的硅材料也被称为"黑硅"。 中国专利说明书 CN 101734611 A (公开 日： 2010年 6月 16日）公开了一种基于无掩膜深反应离子刻蚀制备黑硅的方法， 其原理是将硅片浸没在等离子体气氛中， 采用刻蚀与钝化的方式交替对硅片进 行处理， 一段时间的数次交替处理后硅片表面形成倒立金字塔结构。  In the late 1990s, Professor Eric Mazur of Harvard University studied the femtosecond laser-substance interaction process and found that using a femtosecond laser to irradiate a silicon wafer in a certain gas environment can produce micron in the laser irradiation area of the silicon surface. Level spike structure. Then they developed a new technology for this micro-structured silicon surface. Using a femtosecond laser to etch silicon under a certain gas environment, a new material with a certain etched area was prepared. The gray shiny silicon surface was etched. The place is completely blackened by the naked eye, so this new silicon material is also called "black silicon." Chinese Patent Specification CN 101734611 A (Publication Date: June 16, 2010) discloses a method for preparing black silicon based on maskless deep reactive ion etching, the principle of which is to immerse the silicon wafer in a plasma atmosphere, using The silicon wafer is alternately processed by etching and passivation, and the surface of the silicon wafer forms an inverted pyramid structure after several times of alternating processing.
黑硅由于其特殊的结构使其在多个领域都有广泛的应用。 Eric Mazur等在研 究黑硅的光电性质时惊奇地发现这种表面微结构的硅材料具有奇特的光学性 质， 它对近紫外-近红外波段的光（波长为 0.25-2.5um ) 几乎全部吸收， 并具有 良好的可见和红外发光特性， 同时还具有良好的场致发射特性等。 这使得黑硅 在红外探测器、 太阳能电池以及平板显示器等领域具有重要的潜在应用价值。 尤其是黑硅的强吸收特性， 使其成为制备高效太阳能电池的理想材料。  Black silicon has a wide range of applications in many fields due to its special structure. Eric Mazur et al., when studying the optoelectronic properties of black silicon, surprisingly found that this surface microstructured silicon material has peculiar optical properties, and it absorbs almost all of the near-ultra-near-infrared light (wavelength 0.25-2.5 um). It has good visible and infrared luminescent properties, and also has good field emission characteristics. This makes black silicon an important potential application in the fields of infrared detectors, solar cells, and flat panel displays. In particular, the strong absorption properties of black silicon make it an ideal material for the preparation of high-efficiency solar cells.
但是， 黑硅由于其表面为非平坦的倒立金字塔、 森林状的釘状或针状等结 构， 使得黑硅表面面积存在很大的表面态， 且表面的悬挂键多， 从而降低了黑 硅制备的太阳能电池的转换效率。 另外， 黑硅由于具有倒立金字塔、 森林状的 釘状或针状等结构， 使得黑硅钝化变得更加困难。 However, black silicon has a non-flat inverted pyramid, a forest-like spike or a needle-like knot due to its surface. The structure of the surface area of the black silicon has a large surface state, and the surface has many dangling bonds, thereby reducing the conversion efficiency of the solar cell prepared by the black silicon. In addition, black silicon has become more difficult to pass black silicon passivation due to its inverted pyramid, forest-like nail shape or needle shape.
发明内容 Summary of the invention
本发明要解决的技术问题是提供一种黑硅钝化方法， 以减小黑硅表面态密 度。  The technical problem to be solved by the present invention is to provide a black silicon passivation method for reducing the surface density of black silicon.
为了达到上述目的， 本发明采用的技术方案为： 一种黑硅钝化方法， 所述 方法包括：  In order to achieve the above object, the technical solution adopted by the present invention is: A black silicon passivation method, the method comprising:
将利用等离子体浸没离子注入技术制备的黑硅放置于钝化装置的腔室内； 调整所述钝化装置工艺参数达到预设定的工作范围， 向所述钝化装置通入 混合气体， 所述混合气体包括反应气体；  The black silicon prepared by the plasma immersion ion implantation technique is placed in a chamber of the passivation device; the process parameter of the passivation device is adjusted to reach a preset working range, and the mixed gas is introduced into the passivation device, The mixed gas includes a reaction gas;
利用等离子体增强化学气相沉积， 在所述黑硅表面沉积钝化薄膜。  A passivation film is deposited on the surface of the black silicon by plasma enhanced chemical vapor deposition.
上述方案中， 所述利用等离子体增强化学气相沉积， 在所述黑硅表面沉积 钝化薄膜的步骤具体包括：  In the above solution, the step of depositing a passivation film on the surface of the black silicon by using plasma enhanced chemical vapor deposition specifically includes:
在等离子体电源的作用下， 所述混合气体在所述钝化装置中放电产生等离 子体；  Dissolving the mixed gas in the passivation device to generate a plasma under the action of a plasma power source;
所述反应气体在等离子体气氛中发生反应， 生成物沉积在所述黑硅表面形 成钝化薄膜。  The reaction gas is reacted in a plasma atmosphere, and a product is deposited on the surface of the black silicon to form a passivation film.
上述方案中， 所述工艺参数包括腔室的本底压强和工作压强， 样片台的温 度， 混合气体的流量、 比例， 抽取气体的速度， 以及等离子体电源的输出功率 和频率。  In the above solution, the process parameters include the background pressure and working pressure of the chamber, the temperature of the sample stage, the flow rate of the mixed gas, the ratio, the velocity of the extracted gas, and the output power and frequency of the plasma power source.
上述方案中， 所述腔室的本底压强范围为 10-12Pa~lPa, 工作压强范围为 10—3Pa~10000Pa, 样片台的温度范围为 10~1000。C, 等离子体电源的输出功率为 0~2000w, 频率为 13.56MHz。 In the above solution, the background pressure of the chamber ranges from 10 to 12 Pa to 1 Pa, and the working pressure range is 10- 3 Pa ~ 10000Pa, sample temperature in the range of 10 to 1000 units. C, the output power of the plasma power supply is 0~2000w, and the frequency is 13.56MHz.
上述方案中， 所述钝化薄膜为氮化硅或氧化硅薄膜。  In the above solution, the passivation film is a silicon nitride or silicon oxide film.
上述方案中， 当利用等离子体增强化学气相沉积氮化硅薄膜钝化黑硅时， 所述反应气体包括硅烷和氨气， 或硅烷和氮气； 所述硅烷气体流量为 l~1000sccm, 所述氨气或氮气气体流量为 l~1000sccm, 所述硅烷与氨气或氮气 的体积比为 0.01 ~100。  In the above solution, when the silicon nitride is passivated by the plasma enhanced chemical vapor deposition silicon nitride film, the reaction gas includes silane and ammonia gas, or silane and nitrogen; the silane gas flow rate is 1 to 1000 sccm, the ammonia The gas or nitrogen gas flow rate is from 1 to 1000 sccm, and the volume ratio of the silane to ammonia or nitrogen is from 0.01 to 100.
上述方案中， 当利用等离子体增强化学气相沉积氧化硅薄膜钝化黑硅时， 所述反应气体包括硅烷和笑气； 所述硅烷气体流量为 l~1000sccm, 所述笑气气 体流量为 l~1000sccm, 所述硅烷与笑气的体积比为 0.01~100。  In the above solution, when the black silicon is passivated by the plasma enhanced chemical vapor deposition silicon oxide film, the reaction gas includes silane and laughing gas; the silane gas flow rate is l~1000 sccm, and the laughing gas flow rate is l~ 1000 sccm, the volume ratio of the silane to the laughing gas is 0.01 to 100.
上述方案中， 所述混合气体中还包括稀释气体， 用来稀释所述硅烷； 所述 稀释气体为氩气、 氦气、 氮气和氢气中的一种或多种。  In the above solution, the mixed gas further includes a dilution gas for diluting the silane; and the dilution gas is one or more of argon gas, helium gas, nitrogen gas and hydrogen gas.
与现有技术相比， 本发明技术方案产生的有益效果如下：  Compared with the prior art, the beneficial effects produced by the technical solution of the present invention are as follows:
本发明采用等离子体增强化学气相沉积法， 对利用等离子体浸没离子注入 技术制备的黑硅进行钝化， 饱和了黑硅表面大量的悬挂键， 减小了黑硅表面态 密度， 从而提高了利用黑硅制备的太阳能电池的转换效率。 附图说明  The invention adopts plasma enhanced chemical vapor deposition method to passivate black silicon prepared by plasma immersion ion implantation technology, saturates a large number of dangling bonds on the surface of black silicon, and reduces the surface state density of black silicon, thereby improving utilization. Conversion efficiency of solar cells prepared from black silicon. DRAWINGS
图 1 为本发明实施例提供的一种利用等离子体增强化学气相沉积钝化黑硅 的方法流程图；  1 is a flow chart of a method for passivating black silicon by plasma enhanced chemical vapor deposition according to an embodiment of the present invention;
图 2 为利用等离子体浸没离子注入制备的一种黑硅结构扫描电子显微镜形 貌图；  2 is a scanning electron microscope top view of a black silicon structure prepared by plasma immersion ion implantation;
图 3 为利用等离子体浸没离子注入制备的另一种黑硅结构扫描电子显微镜 形貌图； Figure 3 is another black silicon structure scanning electron microscope prepared by plasma immersion ion implantation. Topographical map
图 4 为利用等离子体浸没离子注入制备的又一种黑硅结构扫描电子显微镜 形貌图；  Figure 4 is a topographical view of another black silicon structure scanning electron microscope prepared by plasma immersion ion implantation;
图 5为本发明实施例对黑硅进行钝化后的扫描电子显微镜形貌图； 图 6为本发明实施例中黑硅单面钝化结构示意图；  5 is a top view of a scanning electron microscope after passivation of black silicon according to an embodiment of the present invention; FIG. 6 is a schematic diagram of a black silicon single-sided passivation structure according to an embodiment of the present invention;
图 7为本发明实施例中黑硅双面钝化结构示意图。 具体实施方式  FIG. 7 is a schematic diagram of a black silicon double-sided passivation structure in an embodiment of the present invention. detailed description
下面结合附图和实施例对本发明技术方案进行详细描述。  The technical solutions of the present invention are described in detail below with reference to the accompanying drawings and embodiments.
等离子体增强化学气相沉积 ( Plasma Enhanced Chemistry Vapor Deposition, PECVD )是将试样放在沉积腔室内的样片台上， 腔室内通入工艺气体， 在等离 子体电源的作用下气体辉光放电产生等离子体， 在等离子体气氛中反应气体更 易受激分解、 离解和离化， 从而提高反应物的活性， 生成物吸附在试样表面， 沉积形成薄膜。  Plasma Enhanced Chemistry Vapor Deposition (PECVD) is a method in which a sample is placed on a sample stage in a deposition chamber, a process gas is introduced into the chamber, and a plasma glow discharge generates a plasma under the action of a plasma power source. In the plasma atmosphere, the reaction gas is more susceptible to decomposition, dissociation and ionization, thereby increasing the activity of the reactants, and the product is adsorbed on the surface of the sample to form a thin film.
本发明利用 PECVD生长薄膜对黑硅进行钝化的主要机理是：沉积腔室内通 入的混合气体在等离子体电源作用下放电产生等离子体， 混合气体中的反应气 体如硅烷（SiH4 )和氨气（NH3 )在等离子体气氛中容易发生反应， 生成 SiNx 和 H2, SiNx沉积在黑硅的表面， SiNx层的表面钝化效果归功于相对较低的表面 态密度和适当密度的表面固定电荷； 等离子体气氛中和反应过程中含有大量的 H, SiNx:H中 H通过空位扩散机制和氢气分子扩散机制能够饱和黑硅材料表面 和体内悬挂键， 从而完成对黑硅的钝化。 The main mechanism for the passivation of black silicon by the PECVD growth film is that the mixed gas introduced into the deposition chamber is discharged under the action of the plasma power source to generate plasma, and the reaction gases in the mixed gas such as silane (SiH 4 ) and ammonia are used. Gas (NH 3 ) is easily reacted in a plasma atmosphere to form SiN x and H 2 , and SiN x is deposited on the surface of black silicon. The surface passivation effect of the SiN x layer is attributed to the relatively low surface state density and appropriate density. The surface of the fixed charge; in the plasma atmosphere and the reaction process contains a large amount of H, SiN x : H H through the vacancy diffusion mechanism and hydrogen molecular diffusion mechanism can saturate the surface of the black silicon material and the dangling bonds in the body, thus completing the black silicon Passivation.
如图 1 所示， 本发明实施例提供了一种利用等离子体增强化学气相沉积钝 化黑硅的方法， 该方法包括： 步骤 210,将利用等离子体浸没离子注入技术制备的黑硅放置于钝化装置的 沉积腔室内； As shown in FIG. 1, an embodiment of the present invention provides a method for passivating black silicon by plasma enhanced chemical vapor deposition, the method comprising: Step 210, placing black silicon prepared by plasma immersion ion implantation technology in a deposition chamber of the passivation device;
钝化装置为等离子体增强化学气相沉积装置， 黑硅放置在该装置的沉积腔 室内， 并且放置于样品台上；  The passivation device is a plasma enhanced chemical vapor deposition device, and black silicon is placed in the deposition chamber of the device and placed on the sample stage;
步骤 212, 调整所述钝化装置的工艺参数， 使之达到预设定的工作范围， 所 述工艺参数包括沉积腔室的本底压强和工作压强， 样片台的温度， 混合气体的 流量、 比例， 抽取气体的速度， 以及等离子体电源的输出功率和频率； 这些工 艺参数可根据加工时的实际情况来预先设定， 也可在加工过程中根据需要现场 修改， 从而使这些参数达到合乎工艺要求的数值范围或预先设定的数值范围； 沉积腔室的本底压强范围可为 10—12Pa ~ lPa, 优选地可为 10—8Pa ~ 10—3Pa, 更为优选地可为 10—7Pa ~ 10—5Pa,沉积腔室的工作压强范围可为 10—3Pa ~ lOOOOPa, 优选地可为 O.lPa ~ lOOOPa, 更为优选地可为 0.5Pa ~ 500Pa; Step 212: Adjust a process parameter of the passivation device to a preset working range, where the process parameters include a background pressure and a working pressure of the deposition chamber, a temperature of the sample stage, a flow rate of the mixed gas, and a ratio , the speed of the extracted gas, and the output power and frequency of the plasma power supply; these process parameters can be preset according to the actual conditions during processing, or can be modified on-site as needed during the processing, so that these parameters meet the process requirements. The range of values or the range of values set in advance; the background pressure of the deposition chamber may range from 10 to 12 Pa to 1 Pa, preferably from 10 to 8 Pa to 10 to 3 Pa, and more preferably from 10 to 10 7 Pa ~ 10 - 5 Pa, the working pressure of the deposition chamber may range from 10 - 3 Pa to 1000OOPa, preferably from 0.1 Pa to lOOOPa, more preferably from 0.5 Pa to 500 Pa;
样片台的温度范围可为 10-1000°C, 优选地可为 100-500°C, 更为优选地可 为 250-450。C;  The temperature of the sample stage may range from 10 to 1000 ° C, preferably from 100 to 500 ° C, and more preferably from 250 to 450. C;
等离子体电源的输出功率为 0~2000w, 频率为 13.56MHz;  The output power of the plasma power source is 0~2000w, and the frequency is 13.56MHz;
通入气体为混合气体， 包括反应气体， 如以在所述黑硅上沉积氮化硅薄膜 为例，反应气体可为 SiH4和 NH3,或 SiH4和 N2, SiH4气体流量可为 l~1000sccm, 优选地可为 10 ~ 300 sccm, NH3或 N2气体流量为 l~1000sccm,优选地可为 10 ~ 300 sccm, 硅烷 SiH4与 NH3或 N2的体积比为 0.01 ~ 100, 优选地可为 0.1 ~ 10; 混合气体中还可以包括稀释气体， SiH4可用 N2、 Ar、 He、 H2中的一种或多 种气体稀释， 优选地用 Ar稀释的 SiH4与 NH3为工艺气体， 稀释后的 SiH4与 NH3气体之间的体积比为 0.01 ~ 100,优选地可为 0.1 ~ 10,稀释后的 SiH4与 NH3 的气体的流量均可为 1 ~ 1000 sccm, 优选地可为 10 ~ 300 sccm; 如以在所述黑硅上沉积氧化硅薄膜为例， 反应气体可为硅烷 SiH4和笑气 N20, SiH4气体流量为 l~1000sccm, 优选地可为 10 ~ 300 sccm, N20气体流量 为 l~1000sccm, 优选地可为 10 ~ 300 sccm, 硅烷 SiH4与 N20 的体积比为 0.01-100, 优选地可为 0.1 ~ 10; The gas to be introduced is a mixed gas, including a reaction gas, for example, a silicon nitride film deposited on the black silicon, the reaction gas may be SiH 4 and NH 3 , or SiH 4 and N 2 , and the flow rate of the SiH 4 gas may be l~1000sccm, preferably 10 ~ 300 sccm, NH 3 or N 2 gas flow rate is l~1000sccm, preferably 10 ~ 300 sccm, and the volume ratio of silane SiH 4 to NH 3 or N 2 is 0.01 ~ 100 Preferably, it may be 0.1 to 10; the mixed gas may further include a diluent gas, and the SiH 4 may be diluted with one or more of N 2 , Ar, He, H 2 , preferably SiH 4 and NH diluted with Ar 3 is a process gas, and the volume ratio of the diluted SiH 4 to NH 3 gas is 0.01 to 100, preferably 0.1 to 10, and the flow rate of the diluted SiH 4 and NH 3 gases may be 1 to 1000. Sccm, preferably 10 to 300 sccm; For example, the silicon oxide film is deposited on the black silicon, and the reaction gas may be silane SiH 4 and laughing gas N 2 0. The flow rate of the SiH 4 gas is 1 to 1000 sccm, preferably 10 to 300 sccm, and N 2 0 The gas flow rate is from 1 to 1000 sccm, preferably from 10 to 300 sccm, and the volume ratio of silane SiH 4 to N 2 0 is from 0.01 to 100, preferably from 0.1 to 10;
同沉积氮化硅薄膜一样， 在沉积氧化硅薄膜所通入混合气体中还可以包括 稀释气体， SiH4可用 N2、 Ar、 He、 H2中的一种或多种气体稀释， 优选地用 Ar 稀释的 SiH4与 N20为工艺气体， 稀释后的 SiH4与 N20气体之间的体积比为 0.01 ~ 100,优选地可为 0.1 ~ 10,稀释后的 SiH4与 N20的气体的流量均可为 1 ~ 1000 sccm, 优选地可为 10 - 300 sccm; As with the deposited silicon nitride film, a diluent gas may be further included in the mixed gas to which the silicon oxide film is deposited, and the SiH 4 may be diluted with one or more of N 2 , Ar, He, H 2 , preferably Ar diluted SiH 4 and N 2 0 are process gases, and the volume ratio between the diluted SiH 4 and N 2 0 gas is 0.01 to 100, preferably 0.1 to 10, and the diluted SiH 4 and N 2 0 The flow rate of the gas may be from 1 to 1000 sccm, preferably from 10 to 300 sccm;
步骤 214, 钝化装置气体放电产生等离子体；  Step 214, the passivation device gas discharge generates a plasma;
步骤 216, 反应气体在等离子体气氛中发生反应；  Step 216, the reaction gas reacts in a plasma atmosphere;
在等离子体气氛中， 由于高能电子的有效碰撞， 使得有关的化学键被打开， 之后又重新组合成生成物；  In a plasma atmosphere, due to the effective collision of high-energy electrons, the relevant chemical bonds are opened and then recombined into a product;
步骤 218,部分反应生成物沉积在黑硅表面，形成氮化硅或氧化硅钝化薄膜； 薄膜的低表面态密度及沉积过程中 H对黑硅表面及内部悬挂键的饱和， 使 得黑硅表面态密度减小， 从而实现对黑硅的钝化。  Step 218, a part of the reaction product is deposited on the surface of the black silicon to form a silicon nitride or silicon oxide passivation film; the low surface state density of the film and the saturation of the H on the black silicon surface and the internal dangling bonds during the deposition process, so that the black silicon surface The density of states is reduced, thereby achieving passivation of black silicon.
图 2、 图 3、 图 4分别为一种黑硅结构扫描电子显微镜形貌图。 图 5是利用 本发明实施例对所述黑硅进行钝化后的扫描电子显微镜形貌图。 图 6、 7分别为 利用本发明实施例对黑硅结构进行单面钝化和双面钝化的结构示意图， 301为利 用等离子体浸没离子注入技术制备的黑硅， 302为利用本发明实施例对黑硅进行 钝化所形成的氮化硅或氧化硅钝化薄膜。  Figure 2, Figure 3, and Figure 4 show the shape of a black silicon structure scanning electron microscope. Fig. 5 is a scanning electron microscope topographical view of the black silicon after passivation using an embodiment of the present invention. 6 and 7 are schematic diagrams showing the structure of single-side passivation and double-sided passivation of a black silicon structure by using an embodiment of the present invention, 301 is black silicon prepared by plasma immersion ion implantation technology, and 302 is an embodiment using the present invention. A silicon nitride or silicon oxide passivation film formed by passivating black silicon.
以上所述的具体实施例， 对本发明的目的、 技术方案和有益效果进行了进 一步详细说明。 应当认识到， 以上所述内容仅为本发明的具体实施方式， 并不 用于限制本发明。 凡在本发明的实质和基本原理之内， 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 objects, technical solutions and advantageous effects of the present invention are further described in detail in the specific embodiments described above. It should be recognized that the above description is only a specific embodiment of the present invention, and is not It is intended to limit the invention. All modifications, equivalents, improvements, etc., made within the spirit and scope of the invention are intended to be included within the scope of the invention.

Claims

权 利 要 求 书 Claim
1、 一种黑硅钝化方法， 其特征在于， 所述方法包括：  A black silicon passivation method, the method comprising:
将利用等离子体浸没离子注入技术制备的黑硅放置于钝化装置的腔室内； 调整所述钝化装置工艺参数达到预设定的工作范围， 向所述钝化装置通入 混合气体， 所述混合气体包括反应气体；  The black silicon prepared by the plasma immersion ion implantation technique is placed in a chamber of the passivation device; the process parameter of the passivation device is adjusted to reach a preset working range, and the mixed gas is introduced into the passivation device, The mixed gas includes a reaction gas;
利用等离子体增强化学气相沉积， 在所述黑硅表面沉积钝化薄膜。  A passivation film is deposited on the surface of the black silicon by plasma enhanced chemical vapor deposition.
2、 如权利要求 1所述的黑硅钝化方法， 其特征在于， 所述利用等离子体增 强化学气相沉积， 在所述黑硅表面沉积钝化薄膜的步骤具体包括：  2. The black silicon passivation method according to claim 1, wherein the step of depositing a passivation film on the surface of the black silicon by plasma enhanced chemical vapor deposition comprises:
在等离子体电源的作用下， 所述混合气体在所述钝化装置中放电产生等离 子体；  Dissolving the mixed gas in the passivation device to generate a plasma under the action of a plasma power source;
所述反应气体在等离子体气氛中发生反应， 生成物沉积在所述黑硅表面形 成钝化薄膜。  The reaction gas is reacted in a plasma atmosphere, and a product is deposited on the surface of the black silicon to form a passivation film.
3、 如权利要求 1所述的黑硅钝化方法， 其特征在于： 所述工艺参数包括腔 室的本底压强和工作压强， 样片台的温度， 混合气体的流量、 比例， 抽取气体 的速度， 以及等离子体电源的输出功率和频率。  3. The black silicon passivation method according to claim 1, wherein: the process parameters include a background pressure and a working pressure of the chamber, a temperature of the sample stage, a flow rate of the mixed gas, a ratio, and a velocity of the extracted gas. , and the output power and frequency of the plasma power supply.
4、 如权利要求 3所述的黑硅钝化方法， 其特征在于： 所述腔室的本底压强 范围为 10—12Pa~lPa, 工作压强范围为 10—3Pa~10000Pa, 样片台的温度范围为 10~1000。C, 等离子体电源的输出功率为 0~2000w, 频率为 13.56MHz。 4. The black silicon passivation method according to claim 3, wherein: the background pressure of the chamber ranges from 10 to 12 Pa to 1 Pa, and the working pressure ranges from 10 to 3 Pa to 10000 Pa. The temperature range is from 10 to 1000. C, the output power of the plasma power supply is 0~2000w, and the frequency is 13.56MHz.
5、 如权利要求 1或 2所述的黑硅钝化方法， 其特征在于： 所述钝化薄膜为 氮化硅或氧化硅薄膜。  The black silicon passivation method according to claim 1 or 2, wherein the passivation film is a silicon nitride or silicon oxide film.
6、 如权利要求 5所述的黑硅钝化方法， 其特征在于： 当利用等离子体增强 化学气相沉积氮化硅薄膜钝化黑硅时， 所述反应气体包括硅烷和氨气， 或硅烷 和氮气； 所述硅烷气体流量为 l~1000sccm , 所述氨气或氮气气体流量为 l~1000sccm, 所述硅烷与氨气或氮气的体积比为 0.01~100。 6. The black silicon passivation method according to claim 5, wherein: when the silicon nitride is passivated by a plasma enhanced chemical vapor deposition silicon nitride film, the reaction gas comprises silane and ammonia, or silane and Nitrogen gas; the silane gas flow rate is l~1000sccm, and the ammonia gas or nitrogen gas flow rate is l~1000sccm, the volume ratio of the silane to ammonia or nitrogen is 0.01~100.
7、 如权利要求 5所述的黑硅钝化方法， 其特征在于： 当利用等离子体增强 化学气相沉积氧化硅薄膜钝化黑硅时， 所述反应气体包括硅烷和笑气； 所述硅 烷气体流量为 l~1000sccm, 所述笑气气体流量为 l~1000sccm, 所述硅烷与笑气 的体积比为 0.01 ~100。  7. The black silicon passivation method according to claim 5, wherein: when the black silicon is passivated by a plasma enhanced chemical vapor deposition silicon oxide film, the reaction gas comprises silane and laughing gas; and the silane gas The flow rate is from l to 1000 sccm, the flow rate of the laughing gas is from 1 to 1000 sccm, and the volume ratio of the silane to the laughing gas is from 0.01 to 100.
8、 如权利要求 6或 7所述的黑硅钝化方法， 其特征在于： 所述混合气体中 还包括稀释气体， 用来稀释所述硅烷； 所述稀释气体为氩气、 氦气、 氮气和氢 气中的一种或多种。  The black silicon passivation method according to claim 6 or 7, wherein: the mixed gas further comprises a diluent gas for diluting the silane; and the diluent gas is argon gas, helium gas, nitrogen gas And one or more of hydrogen.
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