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WO2009141417A1 - Procédé de fabrication d'oxyde de zinc nanoscalaire dopé par un métal alcalin, ayant une teneur variable en dopant - Google Patents

Procédé de fabrication d'oxyde de zinc nanoscalaire dopé par un métal alcalin, ayant une teneur variable en dopant Download PDF

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Publication number
WO2009141417A1
WO2009141417A1 PCT/EP2009/056209 EP2009056209W WO2009141417A1 WO 2009141417 A1 WO2009141417 A1 WO 2009141417A1 EP 2009056209 W EP2009056209 W EP 2009056209W WO 2009141417 A1 WO2009141417 A1 WO 2009141417A1
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WO
WIPO (PCT)
Prior art keywords
zinc oxide
alkali metal
zinc
doped
compound
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP2009/056209
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German (de)
English (en)
Inventor
Andrey Orlov
Matthias Driess
Yilmaz Aksu
Sebastian Polarz
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Grillo Zinkoxid GmbH
Original Assignee
Grillo Zinkoxid GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Grillo Zinkoxid GmbH filed Critical Grillo Zinkoxid GmbH
Priority to DE112009001152T priority Critical patent/DE112009001152A5/de
Publication of WO2009141417A1 publication Critical patent/WO2009141417A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/02—Oxides; Hydroxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/02—Oxides; Hydroxides
    • C01G9/03—Processes of production using dry methods, e.g. vapour phase processes
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
    • C07F3/06—Zinc compounds
    • 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
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/54—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing zinc or cadmium
    • 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
    • H10F71/00—Manufacture or treatment of devices covered by this subclass
    • H10F71/125—The active layers comprising only Group II-VI materials, e.g. CdS, ZnS or CdTe
    • H10P14/265—
    • H10P14/3426—
    • H10P14/3444—
    • H10P14/3461—
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/50—Solid solutions
    • C01P2002/52—Solid solutions containing elements as dopants
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/50—Solid solutions
    • C01P2002/52—Solid solutions containing elements as dopants
    • C01P2002/54—Solid solutions containing elements as dopants one element only
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Definitions

  • the invention relates to a process for the production of alkali-metal-doped nanoscale zinc oxide, zinc oxide prepared by this process and its use, and to a process for producing films of alkali metal-doped nanoscale zinc oxide, films produced by this process and their use.
  • Zinc oxide is used for a variety of purposes, such.
  • As a white pigment as a catalyst, as part of antibacterial skin protection creams and as an activator for the rubber vulcanization.
  • nanoscale zinc oxide is used as a UV-absorbing pigment.
  • ZnO zinc oxide
  • This has a band gap of 3.37 eV [2] and a high exciton-binding energy of 60 meV, which allows use as a laser [3] .
  • ZnO is a characteristic n-type semiconductor with piezoelectronic and electromechanical coupling properties [4] .
  • ZnO has been used in UV LEDs (light-emitting diodes), in photovoltaic solar cells, in UV photodetectors, in varistors, in sensors, and even in heterogeneous catalysis [5,8] .
  • lithium is able to easily occupy intermediate positions in the crystal lattice (Li 1 ) and behaves as a low donor [9/10] .
  • doping with lithium often leads to the formation of semi-insulating, n-semiconducting zinc oxide materials [5] .
  • K. Merz et al., Dalton Trans., 2003, 3365-3369 discloses a heterobubane molecule containing a potassium atom.
  • GB-A-1, 181, 580 discloses a lithium-doped zinc oxide having a lithium content at 0.0068% by weight, based on zinc oxide.
  • Li centers tend to be on interstitial sites. Interlattice-site Li centers lead to strong N-doping, which is in contrast to the desired P-type doping. Successful P-doping can only be achieved if the Li centers are specifically located on the lattice sites of the Zn (replacement of Zn 2+ by Li + ).
  • nanoscale zinc oxide which has a variably adjustable doping content.
  • a doping with alkali metals such as Li would allow the production of a p-doped semiconductor.
  • a technical problem underlying the invention is to provide a method for the production of alkali metal-doped nanoscale zinc oxide, which has a homogeneous and stable p-type doping, and the creation of ZnO with homogeneous and stable p-type doping.
  • the invention accordingly provides a process for the preparation of alkali metal-doped zinc oxide, characterized in that
  • a zinc-alkali metal-organic compound is dissolved in an organic solvent, in particular a dry organic solvent, b) a further organometallic zinc compound is added, c) the organic solvent is removed, d) the residue is from 200 ° C. to 1000 ° C. C is heated, and e) the resulting zinc oxide is cooled.
  • a dry solvent is understood as meaning a solvent which is nearly, in particular completely anhydrous.
  • the process according to the invention makes it possible to produce Li-containing ZnO in which the Li centers occupy the lattice positions of the zinc. It is therefore to a new form of Li-containing ZnO materials over those already described in the literature.
  • the organic solvent is removed in vacuo at, for example, 0.001 to 0.1 bar, in particular 0.01 to 0.05 bar.
  • the residue to 300 0 C to 1000 0 C, in particular 500 0 C to 900 0 C, 600 ° to 800 0 C or 700 0 C to 800 0 C and heated.
  • the residue is heated to 750 0 C.
  • the residue is heated for at least 15 minutes, 30 minutes, 1 hour, 2 hours or 3 hours and at most 48, 36, 24, 12, 6 or 4 hours.
  • the length of the heating time influences the particle size. By sintering, the particle size increases with prolonged heating.
  • step d) is carried out in an atmosphere having at least 80% by volume, in particular at least 90% by volume, 95% by volume, 99% by volume or approximately 100% by volume of oxygen ,
  • This oxygen atmosphere causes the complete conversion of the organic components into CO 2 and H 2 O. Disturbing carbon impurities are thereby separated.
  • the residue is heated in a tube furnace.
  • a tube furnace This is a furnace with a circular opening and a cylindrical, jacketed heating zone into which a quartz tube is inserted. Gas is supplied through the quartz tube.
  • a polar solvent is used as the organic solvent, in particular tetrahydrofuran.
  • a polar solvent has an electric dipole moment and consequently at least one center with a high and at least one center with a comparatively low electron density.
  • zinc oxide is obtained with a doping content of 0.001 to 12%, in particular from 0.01 to 12%, 0.1 to 9%, 0.1 to 6% or 0.1 to 3% (relative on atomic%).
  • the zinc oxide is doped with lithium.
  • nanoscale zinc oxide is obtained.
  • This is understood to mean nanoscale zinc oxide with an average particle size between 1 and 1000 nm.
  • zinc oxide having an average grain size between 1 and 200 nm, 1 and 100 nm, between 20 and 100, or between 30 and 100 nm is obtained.
  • zinc oxide having an average particle size of from 0.01 to 10 ⁇ m, in particular from 0.1 to 1 ⁇ m is obtained.
  • zinc oxide particles having an average grain size of more than 1 ⁇ m can also be produced.
  • the zinc-alkali metal-organic compound and the organic or organometallic zinc compound are cubanes, in particular heterocubanes.
  • Cubane are cage-like molecules of eight atoms arranged in the form of a cube. Inside the cubane, however, there is no cavity.
  • the zinc-alkali metal-organic compound is a monolithium-alkylzincalkoxide having the following structural formula, wherein thf is tetrahydrofuran and R and R 'are identical or different alkyl radicals:
  • the zinc-alkali metal-organic compound is a monolithium-alkylzincalkoxide having the above structural formula, where R is a linear alkyl radical, in particular a methyl or ethyl radical, and R 'is a nonlinear alkyl radical, in particular a Isopropyl or tertiary butyl radical.
  • the further organic or organometallic zinc compound is an alkyl zinc alkoxide.
  • the zinc-alkali metal-organic compound has the formula [(CHs) 3 Zn 3 Li (THF) (OC (CH 3) S) 4] and the organometallic zinc compound has the formula [CH 3 Zn0C ( CH 3 ) 3 ] 4 .
  • Another object of the invention is an alkali metal-doped zinc oxide, in which the alkali atoms, in particular the lithium atoms are as far as possible at the lattice sites of the crystal framework and which is obtainable by the inventive method.
  • the zinc oxide is homogeneously doped with lithium. This means that the concentration of lithium atoms in the zinc oxide of a batch is constant.
  • Another object of the invention is the use of the inventive p-doped nanoscale zinc oxide for the production of Semiconductors, in particular for the production of light-emitting diodes (LEDs), for the production of gas sensors, solar cells or chemical catalysts.
  • LEDs light-emitting diodes
  • An additional subject of the invention relates to a process for producing films of alkali-metal-doped nanoscale zinc oxide, characterized in that
  • a zinc-alkali metal-organic compound is dissolved in an organic solvent, in particular in a dry organic solvent, b) a further organometallic zinc compound is added, c) an inorganic platelet, in particular a quartz platelet, is coated with this solution, the Coating has a thickness of 1 nm to 10 mm, in particular 10 to 1000 nm or 50 to 500 nm, d) the coated platelet is heated within the temperature and time ranges according to at least one of claims 1-3, and e) the resulting film is then cooled.
  • the abovementioned embodiments are likewise possible.
  • the platelets are coated under inert gas conditions (eg in a glovebox) and, in particular, immersed in the solution.
  • inert gas can be z.
  • nitrogen argon or helium can be used.
  • the coated platelets are transferred to a tube furnace in step d) and heated at the conditions described above or in example 2.
  • the thickness of the coating is 100 nm to 20 mm, in particular 200 nm to 15 mm, 400 nm to 10 mm, 500 nm to 5 mm, or 500 nm to 2 mm.
  • the inorganic platelet is a metallic or mineral platelet.
  • the platelet may contain one or more modifications of the carbon, such as carbon.
  • graphite or diamond include.
  • Another object of the invention is a film of alkali metal-doped nanoscale zinc oxide, characterized in that it is obtainable by the method according to the invention.
  • An additional object relates to the use of the film for the production of solar cells, in particular in conjunction with n-semiconducting ZnO.
  • FIG. 1 Structural formula of compound 2
  • FIG. 2 PXRD spectrum of pure compounds 1 and 2 as references, and of a mixture of 1 and 2 (3: 1)
  • FIG. 3 PXRD data of samples 1-6
  • FIG. 4 SEM images in topography mode (left) and backward scattered light electron mode (right) for various lithium-doped ZnO samples
  • Figure 5 FT-IR spectrum of a sample prepared from 3 parts of compound 1 and 1 part of compound 2 (black curve) and a sample prepared from pure compound 2 (gray curve)
  • Figure 6 Li solid phase NMR spectra of various samples Examples
  • Table 1 Mixtures of precursors 1 and 2 for the preparation of lithium-doped nanoscale zinc oxide powders.
  • the mixture of precursors was prepared as described in Example 2.
  • the mixture of precursors 1 and 2 was redissolved in THF and adjusted to a certain concentration. Clean quartz slides were immersed in the precursor mixture under inert gas conditions (in a glove box). The thus coated platelets were then transferred to a tube furnace and heated under the conditions described in Example 2.
  • Precursor compounds 1 and 2 and a mixture of both (3: 1 by mole) were analyzed by powder X-ray diffraction (PXRD).
  • FIG. 1 shows that the mixture is not a physical mixture of two phases of compounds 1 and 2, but that a solid solution is present.
  • the 3/1 mixture would show no new reflexes but only a superposition of the two phases.
  • Example 5
  • the prepared powders were examined in a variety of ways (e.g., PXRD, FT-IR, Li solid phase NMR, electron scanning microscopy (SEM), transmission electron microscopy, UV / Vis, photoluminescence, Raman spectroscopy, and elemental analysis).
  • ways e.g., PXRD, FT-IR, Li solid phase NMR, electron scanning microscopy (SEM), transmission electron microscopy, UV / Vis, photoluminescence, Raman spectroscopy, and elemental analysis).
  • the PXRD data are shown in FIG. 3 and Table 2. Only the typical reflections of ZnO are visible, which proves that there is only one crystalline phase. Impurities are undetectable, indicating that lithium does not form a separate phase, but is integrated into the ZnO crystal lattice and thus the Li atoms are largely located at the positions of the Zn atoms in the crystal framework. All PXRD data were adjusted according to the Warren-Averbach method to derive cell parameters a and c, particle size D and strain e (see Table 2).
  • Table 2 Compared to the data from single-crystal X-ray analysis of zinc oxide, there is a significant increase in cell parameters a and c as a result of doping with lithium. Although the ionic radius of lithium (59 pm) is practically the same as that of zinc (60 pm), this increase can be explained by a partial charge of the unit cell due to the lack of charge compensation of the O 2 " ions Notable change in the PXRD data: Each reflex splits into two partial reflections, indicating a more drastic change in the ZnO crystal structure. The SEM measurements confirm the information obtained from the PXRD measurements. Small crystals of Li x Zni -x ( ⁇ 50 - 90 nm in diameter) form strongly agglomerated powders.
  • the presence of lithium in the prepared samples can be clearly detected by solid-state solid-state NMR spectroscopy.
  • the relative intensity of the signal ⁇ 2 increases with increasing Li doping.
  • the signal ⁇ i is a measure of the exchange of zinc ions by lithium ions at the corner position of the crystal framework, whereas the ⁇ 2 signal indicates lithium ions in intermediate positions.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

L'invention porte sur un procédé de fabrication d'oxyde de zinc dopé par un métal alcalin, caractérisé en ce que a) on dissout un composé organique du zinc-métal alcalin dans un solvant organique, en particulier dans un solvant organique sec, b) on ajoute un autre composé organométallique de zinc, c) on élimine le solvant organique, d) on porte le résidu à une température de 200 à 1 000°C, et e) on refroidit l'oxyde de zinc ainsi obtenu.
PCT/EP2009/056209 2008-05-21 2009-05-22 Procédé de fabrication d'oxyde de zinc nanoscalaire dopé par un métal alcalin, ayant une teneur variable en dopant Ceased WO2009141417A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DE112009001152T DE112009001152A5 (de) 2008-05-21 2009-05-22 Verfahren zur Herstellung von alkalimetall-dotiertem nanoskaligem Zinkoxid mit variablem Dotierungsgehalt

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP08156675.4 2008-05-21
EP08156675 2008-05-21

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WO2009141417A1 true WO2009141417A1 (fr) 2009-11-26

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107583461A (zh) * 2017-10-18 2018-01-16 上海纳旭实业有限公司 钛锰共掺杂纳米氧化锌的制备方法及其产品和应用
EP3365119B1 (fr) 2015-10-23 2020-01-01 Danieli & C. Officine Meccaniche S.p.A. Laminoir à cages multiples pour des corps en forme de tige comprenant trois cages à rouleaux motorisés

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1181580A (en) * 1966-08-05 1970-02-18 Agfa Gevaert Ag Process for Doping Zinc Oxide.

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1181580A (en) * 1966-08-05 1970-02-18 Agfa Gevaert Ag Process for Doping Zinc Oxide.

Non-Patent Citations (8)

* Cited by examiner, † Cited by third party
Title
DATABASE CA [online] CHEMICAL ABSTRACTS SERVICE, COLUMBUS, OHIO, US; ISLAM, EHTESANUL ET AL: "Li-concentration dependence of micro-Raman spectra in ferroelectric-semiconductor Zn1-xLixO", XP002500117, retrieved from STN Database accession no. 137:224982 *
DATABASE CA [online] CHEMICAL ABSTRACTS SERVICE, COLUMBUS, OHIO, US; ISLAM, EHTESANUL ET AL: "Micro-Raman scattering study of ferroelectric-semiconductor Zn1-xLixO", XP002500118, retrieved from STN Database accession no. 136:174678 *
FERROELECTRICS , 261(1-4), 251-256 CODEN: FEROA8; ISSN: 0015-0193, 2001 *
JOURNAL OF THE PHYSICAL SOCIETY OF JAPAN , 71(6), 1594-1597 CODEN: JUPSAU; ISSN: 0031-9015, 2002 *
KLAUS MERZ, STEFAN BLOCK, ROBERT SCHOENEN AND MATTHIAS DRIESS: "Facile synthesis and structural variation of novel heterobimetallic alkali metal-zinc-alkoxide and -siloxide clusters", DALTON TRANS., vol. 2003, 2003, pages 3365 - 3369, XP002497839 *
V. ISCHENKO, S. POLARZ, D. GROTE, V. STAVARACHE, K. FINK, M. DRIESS, ADVANCED FUNCTIONAL MATERIALS, vol. 15, no. 12, 2005, pages 1945 - 1954, XP002500114 *
X.S. WANG, Z.C. WU, J.F. WEBB AND Z.G. LIU: "Ferroelectric and dielectric properties of Li-doped ZnO thin films prepared by pulsed laser deposition", APPLIED PHYSICS A: MATERIALS SCIENCE & PROCESSING, vol. 77, no. 3-4, 2003, pages 561 - 565, XP002500116 *
X.W. ZHU, Y.Q. LIA, Y. LUA, L.C. LIUA AND Y.B. XIAA, MATERIALS CHEMISTRY AND PHYSICS, vol. 102, no. 1, 2007, pages 75 - 79, XP002500115 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3365119B1 (fr) 2015-10-23 2020-01-01 Danieli & C. Officine Meccaniche S.p.A. Laminoir à cages multiples pour des corps en forme de tige comprenant trois cages à rouleaux motorisés
CN107583461A (zh) * 2017-10-18 2018-01-16 上海纳旭实业有限公司 钛锰共掺杂纳米氧化锌的制备方法及其产品和应用

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