• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
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    • 专利摘要:
    growth of thin films of al2o3 for photovoltaic applications a composition comprising, for 100% of its total mass, at least 97% of an aluminum precursor of general formula: al (r1) 2 (or2) with r1 and r2 independently selected from the group consisting of methyl, ethyl, propyl, isopropyl and t-butyl; and: - from 200 ppb to 5 ppm mo (molybdenum); - from 1000 ppm to 5 ppb of fe (iron); - from 200 ppb to 5 ppm cu (copper); - from 200 ppb to 5 ppm of ta (tantalum).
    公开号:BR112013005138B1
    申请号:R112013005138-8
    申请日:2011-08-25
    公开日:2020-09-29
    发明作者:Willhelmus Mathijs Marie Kessels；Technische Universiteit Eindhoven；Gijs Dingemans；Stephen Potts；Nicolas Blasco；Christophe Lachand；Alain Madee
    申请人:L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges；Technische Universiteit Eindhoven；
    IPC主号:
    专利说明:

    The present invention relates to an aluminum source composition containing metallic impurities, useful for the deposition of thin films in photovoltaic technologies, in particular, for solar cells.
    The photovoltaic effect has been known since the late 19th century. The principle is to convert light energy into electricity. In the current ecological context, this is a promising solution for the production of clean and renewable energy. One of the reasons for the slow development of photovoltaic electricity, so far, is the lack of competitiveness compared to traditional solutions such as coal, fossil fuels or nuclear-based electricity. Thus, the contribution of solar energy as a significant component of the energy mix in the future is limited to the ability to continue the race to reduce cost per peak watt. To achieve this goal, reducing manufacturing costs and improving cell efficiency are two solutions.
    The reduction in manufacturing costs is directed, for example, with the use of thinner wafers to limit the impact of the price of silicon raw material on the total cost of the cell (in 2010, cost division is 55% for wafer - with 23% for silicon raw material, 13% for silicon growth and 18% for the wafering stage - and 45% for cell processing), and, in general, with reduced consumption of raw materials, including chemicals used during each stage of the manufacturing process. This decrease in manufacturing cost is driven by manufacturing tool suppliers (OEM - Original Equipment Manufacturers) and material suppliers.
    Improving the efficiency of the photovoltaic cell requires innovative activity that occurs in research laboratories. The work related to the passivation phenomenon carried out by academics can contribute to improving the performance of photovoltaic cells. Passivation of cell defects, for example, by hydrogen, increases the efficiency of the cell, reducing the probability of recombination of electron-hole pairs on the surface and in the volume of silicon: the smaller the number of defects in the material, the greater the probability that cargo carriers are collected. These recombinations occur on the front side of the solar cell, as well as on the rear. To prevent recombination at the rear, the deposition of a thin layer of A12O3 has been described in the literature (eg, P. Vitanov et al. "Chemical Deposition of A12O3thin films on Si substrates" Thin Solid Films, 517 (2009) , 6327-6330), as well as Hoex et al. "Silicon surface passivation by atomic layer deposited A1203" JOURNAL OF APPLIED PHYSICS 104, 044903 2008_demonstrated that very thin layers of ALD-A12O3 (nm 5-30) can provide excellent surface passivation for n-type and n-type silicon wafers -p, after annealing at 425 ° C. This layer contributes to passivation in two ways: reducing the defect density of the interface and passivating the field effect thanks to the high negative charge density on the silicon - alumina interface (G. Dingemans, R. Seguin, P.
    Engelhart, M. C. M. van de Sanden and W. M. M. Kessels; "silicon surface passivation by ultrathin A12O3 films synthesized by thermal and plasma atomic layer deposition"; Phys. Status Solid! RRL4, No. 1-2, 10-12 (2010)).
    Recombination also occurs in the bulky part of silicon. Therefore, for effective collection of carriers, their diffusion length (average distance covered by a load carrier before it becomes recombined) or life span must be at least equal to the thickness of the wafer (VG Litovchenko, NI Klyuis, AA Evtukh, AA Efremov, AV Sarikov, et al .; "Solar cells prepared on multicrystalline silicon subjected to new gettering and passivation treatments"; Solar Energy Materials and Solar Cells, 72 (2002), 343-351)). The injection of atomic hydrogen to passivate defects and reduce the amount of metallic impurities in the bulky part are two main solutions to increase the duration of diffusion. Various sources of contamination can be identified during the different manufacturing steps: from silicon wafer production, including silicon ingot or silicon smelting steps, to the manufacture of solar cells, where many of the chemicals are used. The harmful impact of some impurities such as copper or iron on the life span of charge carriers is known thanks to studies carried out for the semiconductor industry. Figure 1 and Figure 2 detail the conversion efficiency of solar cells based on p-type and n-type wafers, depending on the concentration of selected metal impurities.
    Figure 1 shows the effect of metal impurity concentration on the conversion efficiency of solar cells based on p-type Cz-Si.
    Figure 2 shows the effect of the concentration of metal impurities on the conversion efficiency of solar cells based on Cz-Si type-n.
    The detrimental effect of iron on a boron doped silicon wafer (p-type) is described by Zoth et al ("Silicon contamination control by lifetime measurements"; in Analytical and Diagnostic Techniques for Semiconductor Materials, Devices and Processes (eds. Kolbesen et al.), The Electrochemical Society proceedings, volume ECS PV 99-16 (1999)). During the high temperature (about 800 ° C) burning step required by most solar cell manufacturing processes, the iron atoms, also those possibly and involuntarily deposited with A12O3, will be dispersed evenly in the silicon volume, due diffusion phenomena. These atoms will be located at interstitial sites and some of them will be reversibly combined with a boron atom. The injection of a minor carrier in silicon by photoexcitation will dissociate the FeB pairs and, therefore, the interstitial iron atoms will become recombination centers that are ten times stronger than FeB.
    Iron will also form an oxide, when oxygen is present in the volume. This oxide is an additional defect in the structure and then a recombination center.
    Other metallic impurities, such as copper and nickel, will have an impact on the surface of the wafer from which they will precipitate and form recombination centers. Titanium and molybdenum will diffuse slowly in the volume and form centers of active recombination after high temperature firing.
    To conclude, experts in silicon science consider that transition metals, more precisely, iron, copper, tantalum or molybdenum, are particularly detrimental to the overall performance of solar cells (AA Istratov, C. Flink, H. Hieslmair, SA McHugo , ER Weber; "Diffusion, solubility and gettring of copper in silicon"; Materials Science and engineering B72 (2000) 99-104).
    It is easily understood that impurities can be introduced during the processing of the wafer itself or during handling. During the manufacture of solar cells, contamination can result from the inappropriate use of quality chemicals. In a CVD process, for example, these unwanted elements will be transferred in the gas phase with the main compounds and then incorporated into the layers to be deposited, more precisely, in the passivation layers.
    Based on the information above resulting from the experience of the scientific community, it is obvious that the deposition of A12O3 - for the surface of the silicon wafer based on solar cells - performed by ALD, that is, Atomic Layer Deposition, or MOCVD, that is, Metal -Organic Chemical Vapor Deposition (Agostinelli et al "very low recombination surface speeds in passivated p-type silicon wafers with a fixed negative charge dielectric"; Solar Energy Materials and Solar Cells, 90 (2006), 3438-3443), or PECVD, ie Plasma Enhanced Chemical Phase Vapor Deposition (Saint-Cast et al., very low speed surface recombination in p-type c-Si by high rate of plasma deposited aluminum oxide, Applied Physics Letters 95, 1 51502 2009), or any other vapor phase deposition technique, can induce the incorporation of impurities in the deposited layer, these impurities can be found originally in the aluminum source precursor used for these processes. deposition bones. It can be argued that impurities will be secreted in the passive alumina layer, but this consideration does not take into account that each metallic impurity has a specific diffusion factor and that this phenomenon diffuses from the alumina layer to the volume of silicon increases with temperature. Therefore, the more contaminated the passivation layer, the more contaminated the silicon is due to improved diffusion during mandatory annealing or other high temperature steps (see Figure 3).
    Table 1 details the typical concentrations of upper impurity limits and the requirements for an aluminum precursor to be used in the electronics industry (eg, MOCVD of epitaxial AlGaAs, AlGaN and InAlGaP films for product applications, such as high-power LEDs. brightness and lasers, and more recently aluminum oxide ALD, which is the dielectric layer of choice in DRAM devices). This aluminum precursor is a precursor of formula Al (Ri) 2 (OR2) with Ri and R2 independently selected from the group consisting of methyl, ethyl, propyl, isopropyl and t-butyl. These limits are based on chemical process guidelines. These guidelines provide information on general contamination and appropriate metal to assist end users and chemical manufacturers. If the amount of one of the impurities is greater than the present limit, the precursor does not meet the requirements for use in the manufacture of a semiconductor. The degree, as defined in table 1 is called "semiconductor degree" in the present description.
    Table 1: Typical concentration of impurities in semiconductor grade aluminum precursor of the invention
    The data in Table 1 and the discussion above encourages a solar cell manufacturer to use the "semiconductor grade" to avoid any risk of contamination and, therefore, any possible degradation of the efficiency of the cells. A use of "non-semiconductor grade" precursor for deposition of the A12O3 surface passivation layer can be a non-negligible source of contamination with strong life-threatening "killers" such as iron or copper.
    A12O3 is used in the semiconductor industry for a variety of applications, such as electrical insulation and passivation. For these applications, the "semiconductor grade" aluminum precursor is commonly used to avoid metallic impurities that potentially generate undesirable phenomena, such as leakage currents.
    However, the inventors of the present invention surprisingly show that the use of a non-semiconductor grade aluminum precursor can be used for the deposition of a surface passivation layer in the manufacture of crystalline silicon wafer-based solar cells in such a way that the use of non-semiconductor grade chemicals does not induce any observable deterioration in cell performance (assessed, for example, by measuring the carrier's lifetime). Another application of the non-semiconductor grade may be the deposition of A12O3 for the encapsulation of photovoltaic devices.
    The present invention relates to a composition comprising, for 100% of its total mass, at least 97% of an aluminum precursor of general formula: A1 (R1) 2 (OR2) with Ri and R2 independently selected from the group consisting of methyl, ethyl, propyl, isopropyl and t-butyl, and: - From 200 ppb to 5 ppm Mo (molybdenum); - From 1000 ppb to 5 ppm of Fe (Iron); - From 200 ppb to 5 ppm Cu (Copper); From 200 ppb to 5 ppm of Ta (Tantalum).
    According to an embodiment of the invention, the composition also comprises: - From 5000 ppb to 10 ppm Ni (Nickel); - From 2000 ppb to 10 ppm Zn (Zinc); - From 5000 ppb to 10 ppm W (Tungsten).
    According to another embodiment of the invention, said aluminum precursor is Al (Me) 2 (OiPr).
    According to another embodiment of the invention, the composition comprises other metallic impurities, such as B (Boron), Ca (Calcium), K (Potassium), Cr (Chromium), Na (Sodium), Nb (Niobium), Ti (Titanium ), Mn (Manganese), Co (Cobalt), Sn (Tin) in an amount between 0 and 20 ppm of each.
    According to another embodiment, the invention relates to the use of a composition as above for a method of depositing thin films by ALD, PEALD, CVD, PECVD or MOCVD.
    According to one embodiment, the invention relates to use as defined above, wherein the deposition method is an ALD method.
    According to one embodiment, the invention relates to use as defined above, wherein the thin film is an AljOi film.
    According to one embodiment, the invention relates to the use as defined above, for growing A12O3 for photovoltaic applications.
    According to one embodiment, the invention relates to the use as defined above, wherein the composition defined above, comprises from 97% to 99.4% of said aluminum precursor.
    According to another embodiment, the invention relates to an A12O3 film obtained by use as defined above.
    According to one embodiment, the invention relates to the use of film, as defined above, for the passivation of photovoltaic devices, in particular, for solar cells.
    According to one embodiment, the invention relates to the use as defined above, for the encapsulation of photovoltaic devices, in particular, for solar cells.
    From the fundamentals of the present invention, the inventors understood that a "semiconductor grade" aluminum precursor was mandatory for specific applications, but they concluded that, surprisingly, a "non-semiconductor grade" aluminum precursor, as defined in the present The invention can be used for the purpose of depositing a layer of surface passivation alumina for photovoltaic solar cells based on crystalline silicon wafer. In fact, the following detailed examples show that, contrary to what was expected, the use of "non-semiconductor grade" aluminum precursor (chemical with increased tolerance to the amount of impurities in relation to the "semiconductor grade") is a technical solution to achieve the performance of the expectations of photovoltaic solar cells. In addition, for any photovoltaic devices, encapsulation issues can be addressed by Atomic Layer Deposition or any other appropriate A12O3 vapor phase deposition technique deposited with a "non-semiconductor" grade precursor.
    This chemical with such a degree has the advantages of allowing the deposition of A12O3 layers for passivation by ALD, MOCVD, PECVD, or any other derived deposition methods without observable degradation of solar cell performance (assessed with minor lifetime measurements) carrier). In addition, for encapsulation purposes, ALD or any other derived deposition methods can be considered for the manufacture of an A12O3 film from such "non-semiconductor grade" chemicals.
    This new use of intermediate grade precursor is not only limited to the deposition of a surface passivation layer for solar photovoltaic cells and based on crystalline silicon wafer, but its advantage could be applied to other manufacturing steps in the photovoltaic industry as in the process encapsulation. Thus, these lower grade aluminum precursors can be used in several other fields of application.
    The deposition of an A12O3 thin film requires several steps: a. Vaporize the A1 (R1) 2 (OR2) source to form an aluminum source gas phase. B. Introduce several precursors in the vapor phase in a deposition device, in which said precursors include said vaporized source of Al (Ri) 2 (OR;>), and oxygen source, for example, selected from oxygen, dioxide carbon or nitrogen dioxide plasma, ozone, water.
    In one embodiment of the invention, vaporization of the new "non-semiconductor grade" precursor can be carried out by introducing a gas into a container containing said A1 (R1) 2 (OR2) "non-semiconductor grade" source. The container is preferably heated to a temperature that allows the said source to vaporize with a sufficient vapor pressure. The gas carrier can be selected from Ar, He, H2, N2 or mixtures thereof. The container can, for example, be heated to temperatures in the range of 15 ° C to 170 ° C. The temperature can be adjusted to control the amount of precursor in the gas phase.
    In another embodiment of the invention, said source of "non-semiconductor grade" of A1 (RI) 2 (OR2) is fed in a liquid state to a vaporizer, where it evaporates.
    In one embodiment of the invention, the pressure in said container is in the range of 133 mPa to 133.102 Pa.
    Said vaporized metal source is introduced into a reaction chamber, where it is contacted with a substrate of solar cells. The substrate can be coated with a material selected from the group of Si, SiO2, SiN, SiON, and other substrates and films containing silicon and other films containing metal. The substrate can be heated to a sufficient temperature to obtain the desired film at a sufficient growth rate and with the desired physical state and composition. The typical temperature ranges from an ambient temperature of 600 ° C and preferably from 150 ° C to 600 ° C. Preferably, the temperature is less than or equal to 450 ° C. The pressure in the reaction chamber is controlled to obtain the desired metal-containing film at sufficient growth rate. The typical pressure ranges from 133 mPa to 133.102 Pa or higher.
    In one embodiment of the invention, said A1 (RI) 2 (OR2) "non-semiconductor grade" source described above is mixed with one or more species of reagents before the reaction chamber.
    In one embodiment of the invention, said "non-semiconductor grade" source of AltRjpíORj) described above is mixed with one or more species of reagents in the reaction chamber.
    In another embodiment of the invention, said A1 (RX) 2 (OR2) non-semiconductor grade source and the reactive species are introduced sequentially into the reaction chamber. The A1 (RI.) 2 (OR2) "non-semiconductor grade" source and the reactive species can be introduced simultaneously (chemical vapor deposition), sequentially (atomic layer deposition) or different combinations (an example is the introduction of reagent species (an example could be oxygen) continuously and introduce a "non-semiconductor grade" source of A1 (RI) 2 (OR2) per pulse (pulsed chemical vapor deposition).
    In one embodiment of the invention, the reactive species are decomposed to radicals in a plasma system before entering the reaction chamber.
    In one embodiment of the invention, said reactive species include an oxygen source that is selected from oxygen (O2), radicals containing oxygen (for example, 0 or OH), for example, generated by an oxygen (O2), dioxide of carbon (CO2) or nitrogen dioxide (NO2) from plasma, ozone (O3), moisture (H20) and H2O2.
    In one embodiment of the invention, said A1 (R!) 2 (OR2) "non-semiconductor grade" source is used for atomic layer deposition of A12O3 films. The referred aluminum source and the reactive species are introduced sequentially in the reaction chamber (deposition of the atomic layer). The reactor pressure is selected in the range of 133 mPa to 133.102 Pa. Preferably, the reactor pressure is between 133 Pa and 1330 Pa. A purge gas can be introduced between the metal source pulse and the reactive species pulse . The purge gas can be selected from the group consisting of N2, Ar, He. The aluminum source, the purge gas and the pulse duration of the reactive species are between 1 ms and 10 seconds. The pulse duration is preferably about 10 ms.
    Now, the present invention will be explained with reference to examples. 1) A12O3 thin film deposited by thermal ALD from an Al grade source (RJ 2 (0R2) according to the present invention.
    The degree of Al (Me) 2 (OiPr) (DMAI), according to the present invention, is stored in a container. The container is kept at a temperature of 60 ° C. DMAI steam is entrained, but nitrogen is optionally used as a carrier gas with a flow of, for example, 50 sccm. The silicon substrate is heated to 200 ° C. Water is used as a source of oxygen. The aluminum precursor is sequentially introduced into the reaction chamber with water. During the first stage, an Al (Me) 2 (OiPr) pulse is introduced for 50 ms to 500 ms, followed by an optional 3.5 s argon purge. A pulse of water is then introduced into the reaction chamber for 20 ms, followed by 3.5 s of an optional argon purge. This first sequence is then repeated 1000 times. An A12O3 film meeting the requirements for electrical properties (load life of the silicon substrate carrier) for photovoltaic applications is obtained. This good result shows that the use of a "non-semiconductor grade" is possible for the deposition of an A13O3 layer with proficient passivation properties.
    2) A12O3 thin film deposited by ALD plasma from an A1 (R1) 2 (OR2) grade source according to the present invention. The degree of Al (Me) 2 (OiPr) (DMAI), according to the present invention, is stored in a container. The container is kept at a temperature of 60 ° C. DMAI steam is entrained, but nitrogen is optionally used as a carrier gas with a flow of, for example, 50 sccm. Oxygen gas (50 scan) and argon gas (50 sccm) are introduced continuously into the chamber. The silicon substrate is heated to 200 ° C. Oxygen plasma is used as an oxygen source. The aluminum precursor is sequentially introduced into the reaction chamber. During the first stage, an Al (Me) 2 (OiPr) pulse is introduced for 50 ms to 500 ms, followed by an optional 3.5 s argon purge. A plasma is generated for 3 s to generate the oxygen plasma followed by 3.5 s of an optional argon purge. This first sequence is then repeated 1000 times. An A12O3 film meeting the requirements for electrical properties (load life of the silicon substrate carrier) for photovoltaic applications is obtained. This good result shows that the use of a "non-semiconductor grade" is possible for the deposition of an A12O3 layer with proficient passivation properties.
    3) Deposition tests were performed with a "semiconductor grade" (the highest grade available, see Table 1 for some typical levels of impurities) and a "non-semiconductor grade" (see Table 2) Samples of Al (Me) 2 (OiPr). The recombination speeds resulting from minority carriers (before and after a 400 ° C annealing step) are given (see Figure 4) for the 20 nm thick A12O3 layer deposited by thermal ALD and plasma ALD using a "semiconductor degree" (highest degree of purity) and a "non-semiconductor degree" according to the present invention. Figure 4 shows that the results of the A12O3 layer deposited from Al (Me) 2 (OiPr) by "non-semiconductor grade" according to the present invention are equivalent to the results of the A12O3 layer deposited from Al (Me) ) 2 (OiPr) for the "semiconductor grade".
    Table 2: Typical concentration of impurities in non-semiconductor grade Al (Me) 2 (OiPr) precursor.
    Table 3: Typical concentration of impurities in non-semiconductor grade Al (Me) 2 (OiPr) precursor
    Taking into account the fundamentals of the invention, the conclusion of these tests is very surprising and opens a new possibility for the manufacture of photovoltaic solar cells based on crystalline silicon wafer thanks to the innovative solution of Al (Me) 2 (OiPr) of "non-degree" semiconductor "for deposition of alumina surface passivation. Also for any photovoltaic devices, encapsulation issues can be addressed by A12O3 Atomic Layer Deposition deposited with Al (Ri) 2 (OR2) "non-semiconductor grade". It has been shown that the deposition of A12O3 by for passivation can be performed from an A1 (RI) 2 (OR2) "grade 5 non-semiconductor", such as Al (Me) 2 (OiPr) (DMAI), as a source of aluminum, with no visible degradation of the performance of photovoltaic solar cells based on crystalline silicon wafer; and, more precisely, without impairing the passivation capacity of the surface alumina layer.
    权利要求:
    Claims (7)
    [0001]
    1. Use of a composition comprising, for 100% of its total mass, at least 97% of an aluminum precursor of formula: A1 (RI) 2 (OR2) with Ri and R2 independently selected from the group consisting of methyl, ethyl , propyl, isopropyl and t-butyl, and: - From 200 ppb to 5 ppm Mo (Molybdenum); - From 1000 ppb to 5 ppm of Fe (Iron); - From 200 ppb to 5 ppm Cu (Copper); - From 200 ppb to 5 ppm of Ta (Tantalum); characterized for being for the growth of the A12O3 film for photovoltaic solar cells based on crystalline silicon wafer.
    [0002]
    2. Use, according to claim 1, characterized by the fact that the composition also comprises: - From 5000 ppb to 10 ppm Ni (Nickel); - From 2000 ppb to 10 ppm Zn (Zinc); - From 5000 ppb to 10 ppm W (Tungsten).
    [0003]
    3. Use, according to claim 1 or 2, characterized by the fact that said aluminum precursor is Al (Me) 2 (OiPr).
    [0004]
    4. Use according to claim 1 or 2, characterized by the fact that said composition comprises other metallic impurities, such as B (Boron), Ca (Calcium), K (Potassium), Cr (Chromium), Na ( Sodium), Nb (Niobium), Ti (Titanium), Mn (Manganese), Co (Cobalt), Sn (Tin) in an amount between 0 and 20 ppm of each of them.
    [0005]
    Use according to any one of claims 1 to 4, characterized in that it is for a method of depositing thin film by ALD, PEALD, CVD, PECVD or MOCVD.
    [0006]
    6. Use, according to claim 5, characterized by the fact that the deposition method is an ALD method.
    [0007]
    Use according to any one of claims 51 to 6, characterized in that the composition comprises from 97% to 99.4% of said aluminum precursor.
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    法律状态:
    2018-05-08| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|
    2019-05-07| B06T| Formal requirements before examination [chapter 6.20 patent gazette]|
    2019-12-24| B06A| Notification to applicant to reply to the report for non-patentability or inadequacy of the application [chapter 6.1 patent gazette]|
    2020-05-05| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|
    2020-09-29| B16A| Patent or certificate of addition of invention granted|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 25/08/2011, OBSERVADAS AS CONDICOES LEGAIS. |
    2021-05-25| B16C| Correction of notification of the grant|Free format text: REFERENTE AO DESPACHO 16.1 PUBLICADO NA RPI 2595, QUANTO AOS NOMES DE TITULAR E INVENTORES |
    优先权:
    申请号 | 申请日 | 专利标题
    EP13059549|2010-09-03|
    EP10305954.9A|EP2426233B1|2010-09-03|2010-09-03|Use of dialkyl monoalkoxy aluminum for the growth of Al2O3 thin films for photovoltaic applications|
    PCT/EP2011/064656|WO2012028534A1|2010-09-03|2011-08-25|Growth of ai2o3 thin films for photovoltaic applications|
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