JP5875591B2 - 改善された電解条件に基づく、光電池用途用i−iii−vi族層の化学量論比の制御 - Google Patents
改善された電解条件に基づく、光電池用途用i−iii−vi族層の化学量論比の制御 Download PDFInfo
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- 238000005868 electrolysis reaction Methods 0.000 title description 9
- 238000000151 deposition Methods 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 23
- 230000008021 deposition Effects 0.000 claims description 20
- 150000001875 compounds Chemical class 0.000 claims description 12
- 238000004070 electrodeposition Methods 0.000 claims description 11
- 229910021476 group 6 element Inorganic materials 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 230000009471 action Effects 0.000 claims description 3
- 238000010408 sweeping Methods 0.000 claims description 3
- 239000010410 layer Substances 0.000 description 118
- 239000000758 substrate Substances 0.000 description 41
- 229910052738 indium Inorganic materials 0.000 description 29
- 229910052751 metal Inorganic materials 0.000 description 29
- 239000002184 metal Substances 0.000 description 29
- 239000010949 copper Substances 0.000 description 28
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 27
- 229910052802 copper Inorganic materials 0.000 description 22
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 18
- 229910052733 gallium Inorganic materials 0.000 description 14
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 12
- 239000000463 material Substances 0.000 description 10
- 239000000203 mixture Substances 0.000 description 7
- 239000003792 electrolyte Substances 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 229910052750 molybdenum Inorganic materials 0.000 description 4
- 239000011733 molybdenum Substances 0.000 description 4
- 238000000137 annealing Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000013019 agitation Methods 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- DVRDHUBQLOKMHZ-UHFFFAOYSA-N chalcopyrite Chemical compound [S-2].[S-2].[Fe+2].[Cu+2] DVRDHUBQLOKMHZ-UHFFFAOYSA-N 0.000 description 2
- 229910052951 chalcopyrite Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 238000004876 x-ray fluorescence Methods 0.000 description 2
- DOBUSJIVSSJEDA-UHFFFAOYSA-L 1,3-dioxa-2$l^{6}-thia-4-mercuracyclobutane 2,2-dioxide Chemical compound [Hg+2].[O-]S([O-])(=O)=O DOBUSJIVSSJEDA-UHFFFAOYSA-L 0.000 description 1
- 229910001182 Mo alloy Inorganic materials 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- WUUZKBJEUBFVMV-UHFFFAOYSA-N copper molybdenum Chemical compound [Cu].[Mo] WUUZKBJEUBFVMV-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002471 indium Chemical class 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910000370 mercury sulfate Inorganic materials 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000005289 physical deposition Methods 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000005486 sulfidation Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- H01L31/0248—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 characterised by their semiconductor bodies
- H01L31/0256—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 characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
- H01L31/0322—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312 comprising only AIBIIICVI chalcopyrite compounds, e.g. Cu In Se2, Cu Ga Se2, Cu In Ga Se2
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25D5/611—Smooth layers
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Description
a)電極の表面にI族元素および/またはIII族元素を含む層状構造を電着させるステップと、
b)この構造に少なくとも1つのVI族元素を組み込んでI−III−VI族化合物を得るステップとを含む方法を提案する。
Cu−In型でよく、もしくはIn−Cuでもよく、
また、Cu−In−Ga型でよく、もしくはCu−Ga−Inでもよい。
In−Ga−Cuでよく、もしくはIn−Cu−Gaでもよく、
または、元素Gaが最初に堆積される変形形態では、Ga−In−Cuでよく、もしくはGa−Cu−Inでもよい。
掃引周波数が約0.25Hzのとき53nmであり、輝度が(0から100%までのスケールで)約36%になるように影響を及ぼす。
裏面電極が基板の裏面に接触面を備えるように、裏面電極を基板の裏面に配置するステップと、
基板の表面に生成された最初の金属層(例えばモリブデンの層)上に、I族またはIII族の層を堆積するステップであって、このI族またはIII族の層が、この層の全表面にわたって平均厚さの3%未満の厚さ均一性を有するステップと
を含む。
最終的に得られたI−III−VI族の層上に半導体材料を含むn型層を堆積し、ここで、このn型層がI−III−VI族の層とp−nダイオード接合を形成することから成るステップ
を計画することができる。
透明な導電層(典型的にはZnO)を堆積するステップ
を続けることができる。
基板SUBの少なくとも2つの側面に接する、シーフ(thief)を形成する要素(上記のCA1、CA2のフレーム)を有する支持体に基板を配置し、ここで、支持体は支持体電極を備え、基板は基板の表面上に裏面電極を備えるステップ、
第1のタンクの中に基板と支持体を配置し、ここで、第1のタンクは第1のタンク電極を有し、さらに第1のタンクは銅電解液を含むステップ、
シーフの電流密度を第1のシーフ電流密度に維持し、裏面電極の電流密度を裏面電流密度に維持しながら、支持体電極と第1のタンク電極に電位差を与えることによって励起するステップ、
撹拌器を、裏面電極に対して第1の撹拌器距離で、裏面電極表面上の第1の電解液中を繰り返し移動させて、銅金属層の全表面の第1の平均厚さの3%未満の第1の厚さ均一性で銅金属層が電着されるように、裏面電極上に第1の金属層を電着させるステップ、
第2のタンクの中に基板と、その支持体(前記第1の支持体と同一のものであってよい)を配置し、ここで、第2のタンクは第2のタンク電極を有し、さらに第2のタンクはインジウム電解液を含むステップ、
第2のシーフの電流密度を第2のシーフ電流密度に維持し、銅金属層の電流密度を銅金属層電流密度に維持しながら、第2の支持体電極と第2のタンク電極に電位差を与えることによって励起するステップ、
任意選択で、別の撹拌器を、基板に対して第2の撹拌器距離で、銅金属層表面上のインジウム電解液中を繰り返し移動させて、インジウム金属層の全表面の平均厚さの3%未満の第2の厚さ均一性でインジウム金属層が電着されるように、銅層上にインジウム金属層を電着させるステップ、
を設けることができる。
第3のタンクの中に基板と、その支持体(前記第1の支持体と同一のものであってよい)を配置し、ここで、第3のタンクは少なくとも1つの第3のタンク電極を有し、さらに第3のタンクはガリウム電解液を含み、
第3のシーフの電流密度を第3のシーフ電流密度に維持し、インジウム金属層の電流密度を第3の金属層電流密度に維持しながら、第3の支持体電極と第3のタンク電極を逆極性で励起し、
第3の撹拌器を、インジウム金属層に対して第3の撹拌器距離で、インジウム金属層表面上のガリウム電解液中を繰り返し移動させて、ガリウム金属層の全表面の平均厚さの3%未満の第3の厚さ均一性でガリウム金属層が電着されるように、インジウム金属層上にガリウム金属層を電着させる
ことができる。
以下の要素:第1のタンク、第2のタンクおよび第3のタンクの少なくとも2つが同一のものであることができ、
および/または、以下の要素:第1のタンク電極、第2のタンク電極および第3のタンク電極の少なくとも2つが同一のものであることができ、
および/または、以下の要素:第1の撹拌器、第2の撹拌器および第3の撹拌器の少なくとも2つが同一のものであることができる。
0.5mA/cm2と100mA/cm2の間にある第1のシーフ電流密度を加え、0.5mA/cm2と100mA/cm2の間にある裏面電流密度で裏面電極に電流密度を加えるステップ、
第1の金属層の全表面にわたって第1の平均厚さの3%未満の第1の厚さ均一性を得るステップ、
第2のシーフ電流密度を加え、第1の金属層電流密度で第1の金属層に電流密度を加えるステップ、
第2の撹拌器を、基板に対して第2の撹拌器距離で、0.2Hzと1.8Hzの間に含まれる周波数で繰り返し移動させるステップ、
第2の金属層の全表面にわたって平均厚さの3%未満の第2の厚さ均一性を得るステップ、
第3のシーフ電流密度を加え、第2の金属層電流密度で第2の金属層に電流密度を加えるステップ、
第3の撹拌器を、第3の電解液中を、0.3Hzから1.8Hzの周波数で繰り返し移動させるステップ、
第3の金属層の全表面にわたって平均厚さの3%未満の第3の厚さ均一性を有する第3の金属層(例えばガリウム)を電着させるステップ
を実施することができる。
撹拌器の移動振幅S、
撹拌器の移動速度、
各撹拌器の幅W(例えば三角形の底辺で測定される)、
2つの連続した撹拌器の間の距離M(中心から中心)、
などの撹拌器の移動パラメータを注意深く選択する必要がある。
これらの結果が以下に示される。
図5に示されるように、特に8つの撹拌器の場合、変動率が2%未満であるトポグラフィ均一性(層の反射率と関連した「グレー」スケールで、したがって光学的的な面によって測定された)
確認できるとしても、3cm未満の上記のハイドロメカニカル「マーク」間の距離。
Claims (11)
- 光電池用途用の薄層形態のI−III−VI族化合物の製造方法であって、
a)電極(SUB)の表面にI族元素および/またはIII族元素を含む層状構造を電着させるステップと、
b)前記構造に少なくとも1つのVI族元素を組み込んでI−III−VI族化合物を得るステップとを含み、
前記電着ステップが、前記電極の表面の前に少なくとも2つの電解槽撹拌器を伴い、前記撹拌器が、同一速度および同一振幅で、前記電極の表面と平行に段階的な前後移動する機械的に掃引させる動作を含み、
各撹拌器が所定の厚さを有し、前記撹拌器が所定の間隔をおいて配置されており、各撹拌器の移動振幅が、撹拌器間の間隔よりも大きく、1つの撹拌器の厚さよりも小さく、撹拌器間の間隔の2倍未満であることを特徴とする、製造方法。 - 前記電着ステップが、前記層の厚さを、前記堆積を受ける電極の全表面にわたって厚さ均一性のばらつきを平均厚さの3%未満に制御することを含むことを特徴とする、請求項1に記載の方法。
- 前記撹拌器が、2つの逆三角形(T1、T2)を有する断面を含み、前記電極に最も近い三角形(T2)の底辺が、前記電極(SUB)の表面と平行であることを特徴とする、請求項1または2に記載の方法。
- 前記電極の大きさが700cm2以上であることを特徴とする、請求項1〜3のいずれか1項に記載の方法。
- 前記機械的掃引が、0.2〜1.8Hzの間に含まれる周波数で動作されることを特徴とする、請求項1〜4のいずれか一項に記載の方法。
- 前記撹拌器が、前記電極から5mm未満だけ離して配置されることを特徴とする、請求項1〜5のいずれか一項に記載の方法。
- 前記電極がフレーム(CA1、CA2)によって境界をつけられ、前記移動の振幅が前記フレームを越えて広がることを特徴とする、請求項1〜6のいずれか一項に記載の方法。
- 各撹拌器の速度が、1秒につき1移動振幅より大きいことを特徴とする、請求項1〜7のいずれか一項に記載の方法。
- 各撹拌器の速度が0.2m/s以下であることを特徴とする、請求項1〜8のいずれか一項に記載の方法。
- 前記電極が、前記電解槽の中で、前記前後移動と平行な方向に毎分0.5〜2メートルの速度で移動されることを特徴とする、請求項1〜9のいずれか一項に記載の方法。
- 前記機械的掃引動作が、60cm×120cmの寸法のプレートに対して少なくとも4つの撹拌器を伴い、前記120cmが、前記撹拌器の前後移動の方向に測定されるものであることを特徴とする、請求項1〜10のいずれか一項に記載の方法。
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PCT/FR2011/052363 WO2012052657A2 (fr) | 2010-10-18 | 2011-10-10 | Contrôle de la stoechiométrie de couches i-iii-vi pour des applications photovoltaïques à partir de conditions d'électrolyse perfectionnées. |
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