WO2007107053A1 - An acid corrosion soluton for preparing polysilicon suede and the applied method of it - Google Patents

An acid corrosion soluton for preparing polysilicon suede and the applied method of it Download PDF

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Publication number
WO2007107053A1
WO2007107053A1 PCT/CN2006/001078 CN2006001078W WO2007107053A1 WO 2007107053 A1 WO2007107053 A1 WO 2007107053A1 CN 2006001078 W CN2006001078 W CN 2006001078W WO 2007107053 A1 WO2007107053 A1 WO 2007107053A1
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polycrystalline silicon
etching solution
preparing
acid etching
acid
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PCT/CN2006/001078
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English (en)
French (fr)
Inventor
Jingjia Ji
Yusen Qin
Zhengrong Shi
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Wuxi Suntech Power Co Ltd
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Wuxi Suntech Power Co Ltd
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Priority to EP06741966A priority Critical patent/EP2006892A4/en
Priority to US12/225,382 priority patent/US8298438B2/en
Priority to JP2009500687A priority patent/JP4916546B2/ja
Priority to AU2006340678A priority patent/AU2006340678B2/en
Publication of WO2007107053A1 publication Critical patent/WO2007107053A1/zh
Anticipated expiration legal-status Critical
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K13/00—Etching, surface-brightening or pickling compositions
    • C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
    • C09K13/08—Etching, surface-brightening or pickling compositions containing an inorganic acid containing a fluorine compound
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F77/00—Constructional details of devices covered by this subclass
    • H10F77/70—Surface textures, e.g. pyramid structures
    • H10F77/703—Surface textures, e.g. pyramid structures of the semiconductor bodies, e.g. textured active layers
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P50/00—Etching of wafers, substrates or parts of devices
    • 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

Definitions

  • the present invention relates to an acid etching solution for preparing a polycrystalline silicon suede for a solar cell, and a method for preparing a polycrystalline silicon suede for a solar cell using the acid etching solution.
  • No. 1 invention patent application discloses a method for preparing polycrystalline silicon suede by replacing the traditional NaOH and K0H etching solution with an acid etching solution, and removing the damaged layer generated on the surface of the polycrystalline silicon sheet during the cutting process. At the same time, the original surface of the polysilicon body is preserved, so that the desired suede surface is formed on the surface of the polysilicon after the damaged layer is removed.
  • the method can meet the requirements for large-scale preparation of polycrystalline suede, since the oxidizing agent in the acid etching solution used is Cr0 3 or K 2 Cr 2 0 7 or a mixture thereof, there is a treatment of wastewater generated in the production process. The cost is relatively high, especially the heavy metal emissions in the Xiamen water are harmful to the environmental pollution. Summary of the invention
  • the primary object of the present invention is to provide an acid etching solution which is easy to handle and has a low processing cost for waste acid produced in production, and a further object of the present invention is to provide an acid corrosion using the present invention.
  • an acid etching solution for preparing a polycrystalline silicon suede of the present invention is prepared by mixing an oxidizing agent and a hydrofluoric acid solution, which is nitrate or nitrous acid m.
  • the nitrate is sodium nitrate or nitric acid or ammonium nitrate
  • the nitrite is sodium nitrite or sodium bromine or ammonium nitrite.
  • the concentration of the oxidizing agent is from 1.00 to 10 moles per liter, and the concentration of the hydrofluoric acid is from 10 to 25 moles per liter.
  • the oxidant concentration is from 0.3 to 5 moles per liter, and the hydrofluoric acid concentration is from 15 to 22 moles per liter.
  • a method for preparing polycrystalline silicon suede using the above acid etching solution specifically: The cut polycrystalline silicon wafer is placed in an acid etching solution for corrosion reaction, the reaction time is 30 seconds to 20 minutes, and the temperature of the acid etching solution is -10 °C - 25 °C.
  • the reaction temperature is from 0 °C to 15 °C.
  • the reaction time is from 1 minute to 10 minutes.
  • FIG. 1 is an enlarged view of a scanning electron microscopy of a polycrystalline silicon surface after etching in Example 1;
  • FIG. 2 is an enlarged view of the scanning electron microscopy of the polycrystalline silicon surface after the etching of the embodiment 2;
  • Fig. 3 is an enlarged view of the scanning electron microscopy of the polycrystalline silicon surface after the etching of the embodiment 3.
  • DETAILED DESCRIPTION OF THE INVENTION Example 1
  • Example 1 The surface morphology of the etched polysilicon is shown in Figure 1.
  • Example 1 The surface morphology of the etched polysilicon is shown in Figure 1.
  • the pressure of 2.34 moles of NH4N02 to 1 liter of 20 moles / liter of hydrofluoric acid, mixing evenly, the temperature of the solution is controlled at -10 degrees, placed in a 125 * 125 polycrystalline silicon sheet, etched for 20 minutes.
  • the polycrystalline silicon wafer is then made into a solar cell.
  • the conversion efficiency, fill factor, open circuit voltage and current of the solar cell were 15.38%, 0. 768, 61 1 mV and 5.12 amps, respectively.
  • the surface morphology of the etched polysilicon is shown in Figure 2. 5 ⁇ NaN02 ⁇ After adding 1.
  • concentration of the oxidizing agent and hydrofluoric acid in the acid etching solution of the present invention, and the solution temperature and etching time in the preparation of the polycrystalline silicon suede are not limited to the range of values disclosed in the embodiments of the present invention, according to the teachings and the
  • the specific performance requirements of the polysilicon after corrosion can be appropriately adjusted for the values of the concentrations, temperature, time and other parameters involved.
  • the time and temperature of the corrosion can be suitably lengthened and increased or decreased to obtain polycrystalline silicon having the desired pile surface.
  • the solution temperature and concentration of hydrofluoric acid, the etching time which preclude the use of 10-25 mole liter concentration hydrofluoric acid solution / in particular 15-22 mol / liter concentration hydrofluoric acid solution, and
  • the concentration of the oxidizing agent dissolved therein is controlled at Q.1 - 10 mol / liter, especially 0.3 - 5 mol / liter, while controlling the temperature of the solution at - 1 (TC - 25 ° C, especially 0 ° C - 15 ° C range , and control the corrosion time between 30 seconds and 20 minutes, especially 1 minute to 10 minutes, to achieve the desired corrosion effect, while meeting the production efficiency requirements.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Weting (AREA)
  • Silicon Compounds (AREA)

Description

一种用于制备多晶硅绒面的酸腐蚀溶液及其使用方法 技术领域
本发明涉及一种用于制备太阳能电池用多晶硅绒面的酸腐蚀溶 液， 以及一种利用该酸腐蚀溶液制备太阳能电池用多晶硅絨面的方 法。 背景技术
中国第 200410064831. 1号发明专利申请公开了一种制备多晶硅 绒面的方法， 该方法通过用酸腐蚀溶液替代传统的 NaOH和 K0H腐蚀 液， 在去除切割加工过程中多晶硅片表面产生的损伤层的同时，保留 多晶硅本体表面原貌，从而在去除损伤层后的多晶硅表面形成所需的 绒面。 虽然该方法能够满足大规模制备多晶硅絨面的要求， 但由于其 所用酸腐蚀溶液中的氧化剂为 Cr03或 K2Cr207或它们的混合物， 因此 存在生产过程中所产生的废水的处理成本比较高、特别是廈水中的重 金属的排放对环境污染危害比较大的缺陷。 发明内容
针对现有技术存在的问题，本发明的首要目的是提供一种生产中 所产生的废酸容易处理且处理成本很低的酸腐蚀溶液，本发明进一步 的目的是提供一种使用本发明酸腐蚀溶液制备多晶硅绒面的方法。
为达到上述目的，本发明一种用于制备多晶硅绒面的酸腐蚀溶液 为由氧化剂和氢氟酸溶液混合制成， 所述氧化剂为硝酸盐或亚硝酸 m.。
优选地， 所述硝酸盐为硝酸钠或硝酸钟或硝酸铵， 所述亚硝酸盐 为亚硝 ' 钠或亚 5肖 ^钾或亚硝酸铵。
优选地， 所述氧化剂浓度为 Q.1— 10摩尔 /升， 所述氢氟酸浓度 为 10— 25摩尔 /升。
优选地， 所述氧化剂浓度为 0.3—5摩尔 /升， 所述氢氟酸浓度为 15— 22摩尔 /升。
一种使用上述酸腐蚀溶液制备多晶硅绒面的方法， 具体为： 将切 割成的多晶硅片放入酸腐蚀溶液中进行腐蚀反应， 反应时间为 30秒 —20分钟， 酸腐蚀溶液的温度为 - 10 °C— 25 °C。
优选地， 所述反应温度为 0 °C— 15 °C。
优选地， 所述反应时间为 1分钟一 1 0分钟。
采用本发明酸腐蚀溶液进行多晶硅绒面的制备，不仅生产中产生 的废酸通过一般的中和反应即可进行有效处理，而且消除了排放废液 中的重金属对环境的危害。采用本发明酸腐蚀溶液的多晶硅绒面制备 方法既适用于间隙操作的大规模生产，也适用于连续操作的大规模生 产。 附图^明 图 1为实施例 1腐蚀后的多晶硅绒面电镜扫描放大图；
图 2为实施例 2腐蚀后的多晶硅绒面电镜扫描放大图；
图 3为实施例 3腐蚀后的多晶硅绒面电镜扫描放大图。 具体实施方式 实施例 1 , ,
力口 5 摩尔 KN03到浓度 20摩尔 /升的氢氟酸溶液中， 混合均匀， 把溶液温度控制在 20度， 放入利用线切割切制的 125 * 125的多晶硅 片， 腐蚀 1 0分钟。 然后把该多晶硅片制成太阳能电池。 该太阳能电 池的转换效率、 填充因子、 开路电压和电流分别为 14. 49%、 0. 765、 598毫伏和 4. 95安培。 腐蚀后的多晶硅表面形态如附图 1所示。 实施例 1
力口 2. 34摩尔 NH4N02到 1升 20摩尔 /升的氢氟酸， 混合均匀，把 溶液温度控制在- 10度， 放入 125 * 125的多晶硅片， 腐蚀 20分钟。 然后把该多晶硅片制成太阳能电池。该太阳能电池的转换效率， 填充 因子，开路电压和电流分别为 15. 38% , 0. 768 , 61 1毫伏和 5. 12安培。 腐蚀后的多晶硅表面形态如附图 2所示。 加 1. 17摩尔 NaN03到 1升 20摩尔 /升的氢氟酸， 混合均匀， 把 溶液温度控制在 10度，然后再加入 0. 15摩尔的 NaN02。放入 125* 125 的多晶硅片， 腐蚀 20分钟。 然后把该多晶硅片制成太阳能电池。 该 太阳能电池的转换效率， 填充因子， 开路电压和电流分别为 15. 03%, 0. 771 , 608毫伏和 5. 01安培。 腐蚀后的多晶硅表面形态如附图 3所 示。
本发明酸腐蚀溶液中氧化剂和氢氟酸的浓度，以及进行多晶硅绒 面制备时的溶液温度和腐蚀时间，并不仅限于本发明实施例中所披露 的取值范围， 根据本发明的教导和对腐蚀后的多晶硅具体性能的要 求， 可对所涉及的浓度、 温度、 时间等参数的取值进行适当调整。 如 根据氢氟酸溶液的浓度以及溶液中氧化剂含量高低的不同，可适当延 长和提高或缩短和降低腐蚀的时间和温度，以得到具有所需绒面的多 晶硅。
对于氧化剂、 氢氟酸的浓度和溶液温度、 腐蚀时间的具体取值， 其中釆用 10— 25摩尔 /升浓度的氢氟酸溶液尤其 15— 22摩尔 /升浓度 的氢氟酸溶液， 并且将其中溶入的氧化剂浓度控制在 Q.1— 10摩尔 / 升尤其是 0.3— 5摩尔 /升， 同时将溶液温度控制在- 1 (TC— 25 °C特别 是 0 °C— 15 °C范围， 以及将腐蚀时间控制在 30秒一 20分钟特别是 1 分钟一 10分钟， 可达到所需的腐蚀效果， 同时满足生产效率的要求。

Claims

一种用于制备多晶硅绒面的酸腐蚀溶液， 该酸腐蚀溶液为由氧 化剂和氢氟酸溶液混合制成， 其特征在于， 所述氧化剂为硝酸 盐或亚硝酸盐。
如权利要求 1所述的一种用于制备多晶硅绒面的酸腐蚀溶液， 其特征在于， 所述硝酸盐为硝酸钠或硝酸钾或硝酸铵， 所述亚 硝酸盐为亚硝酸钠或权亚硝酸钾或亚硝 S交铵。
如权利要求 1所述的一种用于制备多晶硅绒面的酸腐蚀溶液， 其特征在于， 所述氧化剂浓度为 G.1— 10摩尔 /升， 所述氢氟酸 浓度为 10—25摩尔 /升。
如权利要求 1所述的一种用于制备求多晶硅绒面的酸腐蚀溶液， 其特征在于， 所述氧化剂浓度为 0.3—5摩尔 /升， 所述氢氟酸 浓度为 15— 22摩尔 /升。
一种使用如权利要求 1或 2或 3所述酸腐蚀溶液制备多晶硅绒 面的方法， 其特征在于， 具体为： 将切割成的多晶硅片放入酸 腐蚀溶液中进行腐蚀反应， 反应时间为 30秒一 20分钟， 酸腐 蚀溶液的温度为 - 10 Ό— 25 Ό。
如权利要求 4所述的一种制备多晶硅絨面的方法，其特征在于， 所述反应温度为 0°C— 15 °C。
如权利要求 4所述的一种制备多晶硅绒面的方法，其特征在于， 所述反应时间为 1分钟一10分钟。
PCT/CN2006/001078 2006-03-21 2006-05-24 An acid corrosion soluton for preparing polysilicon suede and the applied method of it Ceased WO2007107053A1 (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
EP06741966A EP2006892A4 (en) 2006-03-21 2006-05-24 ACID CORROSION SOLUTION FOR PREPARING POLYSILICIUM VELOUR AND APPLIED METHOD THEREFOR
US12/225,382 US8298438B2 (en) 2006-03-21 2006-05-24 Acid corrosion solution for preparing polysilicon suede and the applied method of it
JP2009500687A JP4916546B2 (ja) 2006-03-21 2006-05-24 多結晶シリコンのテクスチャ表面形成用酸腐食溶液およびその使用方法
AU2006340678A AU2006340678B2 (en) 2006-03-21 2006-05-24 An acid corrosion solution for preparing polysilicon suede and the applied method of it

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CN200610065676.4 2006-03-21
CNB2006100656764A CN100467670C (zh) 2006-03-21 2006-03-21 一种用于制备多晶硅绒面的酸腐蚀溶液及其使用方法

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EP (1) EP2006892A4 (zh)
JP (1) JP4916546B2 (zh)
KR (1) KR101028000B1 (zh)
CN (1) CN100467670C (zh)
AU (1) AU2006340678B2 (zh)
RU (1) RU2400862C2 (zh)
WO (1) WO2007107053A1 (zh)

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JP2009530834A (ja) 2009-08-27
CN100467670C (zh) 2009-03-11
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RU2400862C2 (ru) 2010-09-27
EP2006892A1 (en) 2008-12-24
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