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(12) United States Patent (10) Patent No.: US 9,580,610 B2 Koehler Et Al

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(12) United States Patent (10) Patent No.: US 9,580,610 B2 Koehler Et Al USOO958.061 OB2 (12) United States Patent (10) Patent No.: US 9,580,610 B2 Koehler et al. (45) Date of Patent: Feb. 28, 2017 (54) ALUMINIUM OXIDE PASTES AND PROCESS (52) U.S. Cl. FOR THE USE THEREOF CPC ............. C09D 7/1216 (2013.01); C09D I/00 (2013.01); C09D 5/006 (2013.01); C09D (75) Inventors: Ingo Koehler, Reinheim (DE); Oliver 7/1233 (2013.01); C23C 18/1216 (2013.01); Doll, Dietzenbach (DE); Werner C23C 18/1245 (2013.01); C23C 18/1254 Stockum, Reinheim (DE); Sebastian (2013.01); HOIL 21/2225 (2013.01) Barth, Darmstadt (DE) (58) Field of Classification Search None (73) Assignee: MERCK PATENT GMBH, Darmstadt See application file for complete search history. (DE) (*) Notice: Subject to any disclaimer, the term of this (56) References Cited patent is extended or adjusted under 35 U.S. PATENT DOCUMENTS U.S.C. 154(b) by 99 days. 2008/0090101 A1 4/2008 Klipp et al. (21) Appl. No.: 14/003,467 2009,018951.0 A1 7/2009 Kanamori et al. (Continued) (22) PCT Filed: Feb. 9, 2012 FOREIGN PATENT DOCUMENTS (86). PCT No.: PCT/EP2012/000592 CN 101679.807. A 3, 2010 S 371 (c)(1), EP 1156024 A1 11 2001 (2), (4) Date: Sep. 6, 2013 (Continued) (87) PCT Pub. No.: WO2012/119686 OTHER PUBLICATIONS PCT Pub. Date: Sep. 13, 2012 International Search Report for PCT/EP2012/000592 (Jun. 28, (65) Prior Publication Data 2013). US 2014/0000481 A1 Jan. 2, 2014 (Continued) (30) Foreign Application Priority Data Primary Examiner – Colin W Slifka (74) Attorney, Agent, or Firm — Millen White Zelano and Mar. 8, 2011 (EP) ..................................... 11 OO1921 Branigan, PC; Csaba Henter; Anthony Zelano Sep. 6, 2011 (EP) ..................................... 11 OO7205 (57) ABSTRACT (51) Int. Cl. C09D 7/12 (2006.01) The present invention relates to aluminium oxide pastes and HOIL 2L/22 (2006.01) to a process for the use of the aluminium oxide pastes for the C23C 8/2 (2006.01) formation of Al-O coatings or mixed Al-O. hybrid layers. C09D I/00 (2006.01) C09D 5/00 (2006.01) 20 Claims, 2 Drawing Sheets US 9,580,610 B2 Page 2 (56) References Cited L. Jiang et al., “Adsorption of Salicylic Acid, 5-Sulfosalicylic Acid and Tiron at the Alumina-Water Interface'. Colloids and Surfaces A: U.S. PATENT DOCUMENTS Physicochem. Eng. Aspects, vol. 211, No. 2-3 (Dec. 1, 2002) pp. 165-172. 2010/024.3221 A1 9/2010 Yamasaki et al. 2011/0076505 A1* 3/2011 Ishii .......................... C23C 8/10 P.C. Hidber et al., “Influence of the Dispersant Structure on Prop 428,472 erties of Electrostatically Stabilized Aqueous Alumina Suspen sions”, Journal of the European Ceramic Society, vol. 17. No. 2 FOREIGN PATENT DOCUMENTS (1997) pp. 239-249. N. Ozer et al., “Preparation of Amorphous Al2O3 Films by the EP 2085411 A2 8, 2009 EP 2147957 A1 1, 2010 Sol-Gel Process”, Part of the SPIE Conference on Solar Optical JP 06-19129 A T 1994 Materials XVI, SPIE vol. 3789 (Jul 1999) pp. 77-83. JP 2010-254553 A 11 2010 M. Nocun et al., “Sodium Diffusion Barrier Coatings Prepared by TW 200819506 A 5, 2008 Sol-Gel Method”. Optica Applicata, vol. 38, No. 1 (2008) pp. TW 200936,717 A 9, 2009 171-179. Chinese Office Action dated May 15, 2015 issued in corresponding OTHER PUBLICATIONS CN 201280011955.6 application (pp. 1-12). English Abstract of JPH 06-191929 A published Jul. 12, 1994. L. Montanaro et al., “Set up of a Screen-Printing Procedure for the English Abstract of JP 2010-254553 A published Nov. 11, 2010. Production of a B Alumina-Based Gas Sensor'. Journal of Electroceramics, vol. 5, No. 3 (2000) pp. 253-259. * cited by examiner U.S. Patent Feb. 28, 2017 Sheet 1 of 2 US 9,580,610 B2 383.38 : *::::::: U.S. Patent Feb. 28, 2017 Sheet 2 of 2 US 9,580,610 B2 Change in viscosity •Example 1 &Exampl 93 7 Storage time days E-3 E-4 SE-s --screen printed A223 1.0E-38 r. ::::::::: of passivated Carries density A in US 9,580,610 B2 1. 2 ALUMNIUM OXDE PASTES AND PROCESS highly promising replacement for SiO2 layers to be obtained. FOR THE USE THEREOF Besides the above-mentioned uses, in which Al-O serves either as diffusion barrier and/or Sol-gel-based doping The present invention relates to aluminium oxide pastes Source, Al2O is also Suitable, owing to the hardness of its and to a process for the use of the aluminium oxide pastes crystalline modifications, for use as mechanical protection for the formation of Al-O coatings or mixed Al-O hybrid layer. layers. Surprisingly, it has now been found that it is possible to The synthesis of Sol-gel-based layers is attaining ever synthesise and formulate paste-form mixtures based on the greater importance in industrial production owing to their Al-O sol-gel process which meet the rheological require variety of possible uses. Thus, the following functional 10 ments of the screen-printing process. Unexpectedly, the layers or Surface finishes and modifications can be built up paste-form mixtures can be applied Surprisingly easily to or carried out by means of Sol-gel technology: silicon wafer Surfaces in the screen-printing process, where antireflection coatings, for example for optical compo they have high structure fidelity. nents and the like For use, in particular in the Solar sector, Sol-gel-based corrosion-protection coatings, for example of Steels and 15 layers have to meet particular requirements, and thus so too the like do the pastes based on them, meaning that these requirement Scratch-protection coatings S also have to be taken into account in the formulation of Surface seals compositions for the production of Such layers. hydrophobisation or hydrophilisation of surfaces On the one hand, Suitable solvents having properties synthesis of membranes and membrane materials which are advantageous for the use. Such as, for example, no synthesis of Support materials for catalytic applications to low toxicity, adequate surface wetting, etc., should be precursors of sinter ceramics and sinter-ceramic compo selected. Furthermore, corrosive anions (Cl or NO, etc.) nents should not be present in the pastes, since they would greatly dielectric layers for electronic and microelectronic com limit the possible uses of the pastes. Corresponding pastes ponents having the following special applications, 25 could, for example, corrode the printing and deposition where the formation of one of the desired functional equipment used, but also later undesirably promote corro ities may be, but does not have to be, linked to specific sion of solder contacts when connecting up Solar cells which heat treatment, such as, for example, in a stream of O, are provided with Such layers, which would consequently N, O/N and/or forming gas: result in limited long-term stability of crystalline silicon spin-on-glass ("SoG) in the manufacture of integrated 30 Solar cells. circuits For the production of screen-printable pastes, the litera dielectric buffer layers between individual metallisa ture only discloses syntheses using rheological additives or tion planes in the manufacture of integrated circuits grinding of metal oxides precipitated by the sol-gel process (“porous MSQ) with Subsequent Suspension of these oxides. However, this printable dielectric layers for printed circuits, printable 35 type of paste production with post-treatment or admixture of electronics in general and printable organic electron rheological additives usually comprises contamination of ics in particular the actual active Substances. diffusion-barrier layers (cf. MERCK SolarFesist patent) Zhou et al. have investigated, for example, the synthesis for semiconductors in general of a CuZnSnS paste. Elemental copper, Zinc, tin and Sulfur for silicon in particular and especially for silicon wafers 40 were ground in a ball mill with addition of ethanol. After and in particular for those for the production of Subsequent drying, these were Suspended in isopropanol and crystalline silicon Solar cells mixed with a 10% ethylcellulose mixture in isopropanol. matrices for the binding of dopants (for example B. Ga, P. This mixture was ground again in a ball mill with addition AS, etc.) for the specific full-area and/or local doping of of terpineol, and the alcohol was removed in vacuo. The semiconductors in general 45 resultant viscous mass was employed for screen printing, silicon in particular and especially for silicon wafers and the layers obtained were investigated. {1 Z. Zhou, Y. and in particular for those for the production of Wang, D. Xu, Y. Zhang, Solar Energy Materials and Solar crystalline silicon Solar cells Cells, in press, (2010)} electronic passivation of semiconductor Surfaces in gen Hansch et al. in turn investigated the synthesis of a eral and of silicon Surfaces in particular, which results 50 screen-printable YO/ZrO mixed oxide. A YO/ZrO sol in a considerable reduction in the Surface recombina was obtained by mixing Zirconium n-propoxide stabilised by tion speed. means of acetylacetone and carboxylic acid (acetic acid, This list only represents a selection of the various possible propionic acid, caproic acid, nonanoic acid) in isopropanol applications. and an aqueous yttrium nitrate solution. In order to obtain a Most sol-gel processes known from the literature are 55 screen-printable paste, a calcined YO/ZrO powder was based on the use of silicon and alkoxides thereof (siloxanes), added to this sol (sol/powder 20/80-40/60 wt.%), and this the specific hydrolysis and condensation of which enables mixture was Subsequently ground by means of a ball mill for networks having various properties and coatings which can homogenisation. In the same way, pastes were prepared with be derived therefrom to be synthesised very easily, and addition of organic additives (terpineol or ethylcellulose), Smooth or porous films, or films in which particles are 60 but a paste was also prepared only from the calcined oxide.
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