WO2008052771A1 - Leuchtstoffe - Google Patents
Leuchtstoffe Download PDFInfo
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- WO2008052771A1 WO2008052771A1 PCT/EP2007/009470 EP2007009470W WO2008052771A1 WO 2008052771 A1 WO2008052771 A1 WO 2008052771A1 EP 2007009470 W EP2007009470 W EP 2007009470W WO 2008052771 A1 WO2008052771 A1 WO 2008052771A1
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- Prior art keywords
- activator
- network
- phosphors
- ligands
- molecular
- Prior art date
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- 239000000126 substance Substances 0.000 title abstract description 14
- 239000012190 activator Substances 0.000 claims abstract description 51
- 229910052796 boron Inorganic materials 0.000 claims abstract description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 19
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 18
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims description 34
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 16
- 238000000197 pyrolysis Methods 0.000 claims description 13
- 238000005915 ammonolysis reaction Methods 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000003446 ligand Substances 0.000 claims description 10
- 229910021529 ammonia Inorganic materials 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 8
- 229920000642 polymer Polymers 0.000 claims description 8
- 229910052693 Europium Inorganic materials 0.000 claims description 6
- 150000004820 halides Chemical class 0.000 claims description 6
- RVNZEJNWTUDQSC-JOCHJYFZSA-N (2r)-n-(6-aminohexyl)-1-tridecanoylpyrrolidine-2-carboxamide Chemical compound CCCCCCCCCCCCC(=O)N1CCC[C@@H]1C(=O)NCCCCCCN RVNZEJNWTUDQSC-JOCHJYFZSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052684 Cerium Inorganic materials 0.000 claims description 4
- 229910052788 barium Inorganic materials 0.000 claims description 3
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 2
- 229910052691 Erbium Inorganic materials 0.000 claims description 2
- 229910052689 Holmium Inorganic materials 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 2
- 229910052772 Samarium Inorganic materials 0.000 claims description 2
- 229910052771 Terbium Inorganic materials 0.000 claims description 2
- 229910052775 Thulium Inorganic materials 0.000 claims description 2
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 2
- 229910052787 antimony Inorganic materials 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910052745 lead Inorganic materials 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 abstract description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 5
- 238000010348 incorporation Methods 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 5
- 239000001301 oxygen Substances 0.000 abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 abstract description 5
- 230000003287 optical effect Effects 0.000 abstract description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 3
- 125000000129 anionic group Chemical group 0.000 abstract description 2
- 125000002091 cationic group Chemical group 0.000 abstract description 2
- 230000005284 excitation Effects 0.000 abstract description 2
- 239000011574 phosphorus Substances 0.000 abstract description 2
- 238000001228 spectrum Methods 0.000 abstract description 2
- 238000005286 illumination Methods 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 150000002739 metals Chemical class 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000007858 starting material Substances 0.000 description 4
- 238000006467 substitution reaction Methods 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000008240 homogeneous mixture Substances 0.000 description 2
- 229910052747 lanthanoid Inorganic materials 0.000 description 2
- 150000002602 lanthanoids Chemical class 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- -1 phosphorus halide Chemical class 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000004639 Schlenk technique Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005090 crystal field Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 230000005274 electronic transitions Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000012704 polymeric precursor Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7715—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing cerium
- C09K11/7726—Borates
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/583—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
- C04B35/589—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride obtained from Si-containing polymer precursors or organosilicon monomers
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- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3229—Cerium oxides or oxide-forming salts thereof
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/46—Gases other than oxygen used as reactant, e.g. nitrogen used to make a nitride phase
- C04B2235/465—Ammonia
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- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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- C04B2235/6565—Cooling rate
Definitions
- the invention relates to a new class of phosphors based on a universally dopable matrix of an amorphous, at most partially crystalline network of the elements P, Si, B, Al and N, preferably of the composition Si 3 B 3 N 7 .
- Optical excitation and emission can be varied in this system by incorporation of any cationic activators, singly or in combination, but also by incorporation of oxygen as an anionic component throughout the practically relevant range. This opens up the full spectrum of applications for phosphors, such as lighting systems or electronic screens.
- Phosphors based on oxo and / or nitrido-silicates, phosphates or aluminates as host lattice, doped with transition metals or lanthanides as activator, are described in many different variants.
- the requirements for the ready-to-use phosphors are constantly growing, especially because of the classic applications such as electron beam screens (Braunsche tube) or
- the previously provided phosphors are usually crystalline.
- the desired luminous properties are obtained by exchanging ions present in the crystalline lattice of the substances with other ions, so-called activators.
- the respective crystalline matrix must contain certain cations on defined lattice sites. These cations and their lattice sites must be such that they correspond to the chemical and structural needs of the activator and thus allow a corresponding substitution. This condition has a strong limiting effect in that a specific host structure has to be found for each activator ion. Due to an unavoidable mismatch of substituted and Aktivatoranionen also the achievable doping concentrations are limited.
- Impurities have very unfavorable effects, especially with optical materials. In the case of phosphors, they impair their efficiency, because they reduce the optical transmission and at the same time promote radiationless decay.
- An object of the present invention was to overcome the described disadvantages of the prior art.
- a thermally and chemically resistant matrix should be provided, in which universally arbitrary activators can be introduced.
- the production route should allow a high purity of the product.
- phosphors based on an amorphous or partially crystalline network comprising nitrogen (N) and at least two elements selected from P, Si, B and Al, and wherein at least one activator is incorporated in the network.
- the phosphors according to the invention are distinguished, in particular, by the fact that they are not substances based on a crystalline structure but rather substances based on an amorphous or partially crystalline network.
- the base materials used according to the invention for forming the phosphor have networks which are in particular X-ray amorphous, that is to say they do not have crystallites with a diameter of ⁇ 300 nm, in particular no crystallites with a diameter ⁇ 200 nm, and even more preferably no crystallites with one Diameter ⁇ 100 nm.
- the base material of the phosphors according to the invention therefore does not have any long-range lattice symmetry.
- the network of the base material at least one activator is further incorporated in the phosphors according to the invention.
- the activators are additionally incorporated.
- the base material of the phosphors according to the invention comprises at least two elements selected from P, Si, B 1 Al and independently thereof always N.
- the network consists of the elements P, Si, B 1 Al and N. or the respective subsystems P, Si, B and N, P, Si, Al and N, Si, B, Al and N, P, B, Al and N, P, Si and N, P, B and N 1 P, Al and N, Si, B and N, Si, Al and N or B, Al and N.
- suitable activators are incorporated or incorporated.
- any metal ions can be introduced into the inorganic amorphous or partially crystalline network as activators.
- Preferred activator elements are Ba 1 Zn, Mn, Eu, Ce, Pr 1 Nd, Sm, Tb, Dy, Ho, Er, Tm, Yb, Sn, Sb, Pb or Bi.
- the activators are Mn 2+ , Zn 2+ , Ba 2+ , Ce 3+ , Nd 3+ , Eu 2+ , Eu 3+ , Gd 3+ , Tb 3+ , Sn 2+ , Sb 3+ , Pb 2+ or Bi 3+ .
- the amount of activators in the phosphor is preferably ⁇ 0.1% by weight, in particular ⁇ 0.5% by weight and preferably up to 14% by weight, in particular up to 5% by weight.
- the activators may also have a sensitizer function.
- the incorporation of suitable activators into an amorphous three-dimensional network of the composition Si / B / N is particularly preferred.
- This host material has no periodic lattice symmetry.
- the base material structure is preferably nitridic in nature, which may optionally be doped oxide.
- the invention further relates to a process for the preparation of phosphors as defined above, comprising the steps of (i) providing one or more molecular precursors, (ii) processing the one or more molecular precursor to a preceramic material; and (iii) pyrolysis of the preceramic material to form an amorphous or partially crystalline network characterized in that an activator is added in at least one of steps (i), (ii) or (iii) becomes.
- the base material is accessible only through molecular or polymeric precursors, which are processed into a preceramic material which is then converted to the final ceramic state by pyrolysis.
- one or more molecular precursors are first provided.
- the molecular precursors contain the elements of the
- Base material ie in particular at least two elements selected from P, Si, B and AI.
- concentrations of P, Si, B, Al are in each case set between 0 and 100 atom%, preferably between 10 and 80 atom%.
- the molecular precursors are halides, preferably chlorides.
- molecular precursors in particular a mixture of molecular precursors, which are then subjected to co-ammonolysis.
- Mixtures of molecular precursors can be obtained, for example, by mixing a silazane and a boron and / or phosphorus halide.
- a molecular precursor used which is a one-component precursor.
- a one-component precursor already contains all elements of the product.
- the starting point for the preparation is particularly preferably the molecular compound CI 3 Si (NH) BCI 2 (TADB) which already contains the Si-NB linkage desired in the end product.
- More preferred molecular component precursors are CI 4 P (N) (BCI 2) SiCl 3, Cl 3 PNSiCI 3, (CI 3 Si) 2 NBCI 2, CI 3 SiN (BCI 2) 2, (H 3 Si) 2 NBCI 2, CI 3 Si (NH) (BCI) (NH) SiCl 3 , CI 3 Si (NH) (AICI) (NH) SiCl 3 , [(CI 3 Si) (NH) (BNHJ] 3 , (CI 3 Si (NH ) AICIz) 2 or [CI 3 PN (PCIZ) 2 N] + [AICI 4 ] -.
- the precursor material is then processed into a preceramic material in step (ii).
- a soluble or meltable or an insoluble and infusible amorphous intermediate is obtained by ammonolysis.
- the intermediate is then pyrolyzed, preferably in the stream of ammonia or nitrogen.
- an activator is added in at least one of the steps (i), (ii) or (iii).
- the activators are preferably introduced via the two different routes described below.
- TADB molecular precursor
- the solution of the metals in ammonia can also be converted into precursors, e.g. TADB be dripped.
- the resulting polymeric imidamide contains, besides the base material elements, e.g. in addition to silicon and boron, the or the activator elements homogeneously distributed.
- Activators that do not dissolve in liquid ammonia in elemental form can be incorporated as complex molecular compounds become.
- the ligands used should preferably contain only system-inherent elements such as halide (chloride), hydrogen, silicon or boron. All other elements would not be removed or only with additional effort from the final product.
- Particularly suitable and systems are compatible [3 Si (N) SiCl 3 Cl] ", and chloride as ligands of metal complexes for example. Since all form binary chlorides as activators candidate metals from which the desired complexes by reaction with Li [CI 3 Si (N) SiCl 3] can be represented, this access is universal.
- the preceramic intermediate material which is in particular a preceramic imidamide, is prepared by ammonolysis of molecular precursors containing P, Si, B and / or Al and of activators.
- the activators are preferably present as halides or as complex compounds or as metals dissolved in ammonia.
- the activators and the molecular precursors may be dissolved in each other or together in a solvent.
- the one-component molecular precursor preferably comprises two or more of the elements P, Si, B and Al.
- the starting materials are preferably selected so that elements of the ligands of the complexed activator and elements of the molecular precursors with the exception of the system-immanent elements of the preceramic polymer, in particular with the exception of nitrogen in the course of the ammonolysis and the subsequent pyrolysis, can be completely expelled.
- Particularly preferred are the following variants of the preparation.
- the molecular precursor is dripped in pure form or dissolved in liquid ammonia, the ammonia containing dissolved activators, such as europium or barium.
- the molecular precursor are dripped together with one or more activator elements as halides, as a mixture or dissolved together for ammonolysis in liquid ammonia.
- the molecular precursor is added dropwise together with one or more activator elements as a complex compound as a mixture or dissolved together for ammonolysis in liquid ammonia.
- the molecular precursor and in each case a halide of the activator or the activator elements in a homogeneous mixture or dissolved together with gaseous ammonia is ammonolyzed. It is further preferred to ammonolyse the molecular precursor and in each case a complex compound of the activator or elements in a homogeneous mixture or dissolved together with gaseous ammonia.
- pyrolysis takes place according to the invention, forming an amorphous or partially crystalline network.
- the preceramic amide obtained as an intermediate is converted at temperatures between 600 0 C and 1500 0 C, preferably between 1000 0 C and 1300 0 C, in the final product.
- the pyrolysis preferably takes place in an atmosphere comprising nitrogen, argon, ammonia or mixtures thereof.
- Fine tuning of the ligand field and thus of the electronic transitions on the activator element is achieved by partial substitution of nitride by oxide. This can be achieved, for example, quite simply by exposing the preceramic polymer to a gas atmosphere which is loaded with a defined amount of water vapor.
- the controlled hydrolysis of the preceramic imidamide preferably produces an end product after pyrolysis which is up to 20 wt .-%, preferably up to 10 wt .-%, in particular up to 6 wt .-% oxygen, preferably up to 4 wt .-% oxygen.
- two or more activators are possible according to the invention.
- the two routes presented above will be labeled individually or in combination.
- two or more metals suitable as activators may be dissolved in liquid ammonia or incorporated as complex compounds in solution with TADB or both in liquid ammonia and in solution with TADB.
- the application of the phosphors can according to the prior art, for. B. dispersed in a resin.
- the sinterability of the polymeric preceramic precursor can be exploited in the new system presented here.
- the preceramic polymer is slurried or dusted onto the surface to be coated and then baked.
- the new phosphors are thermally stable up to at least 1,200 ° C, far higher than required for use in LEDs (max. 200 0 C). By chemical analysis (digestion, ICP-OES) no impurities are detectable, with a detection limit of 0.5 ppm.
- the new phosphors are particularly suitable for use in lighting systems, LEDs or electronic screens.
- the then almost salt-free polymer was first heated in a heated at 600 0 C BN crucible in an NH 3 stream at 900 0 C, then heated in an N 2 stream to 1200 0 C (heating rate 10 ° C / min) and cooled after a holding time of 3 h at the same rate.
- the product is X-ray amorphous.
- Chemical analysis (ICP-OES) showed a content of 1.2% by weight of Eu.
- the residual, almost salt free polymer was dissolved in a heated at 600 0 C BN crucible 3 stream at 900 0 C initially heated in a NH, then in a stream of N 2 to 1200 0 C heated (heating rate 10 ° C / min) and cooled after a holding time of 3 hours at the same rate.
- the product is X-ray amorphous and contains by chemical analysis (ICP-OES) a proportion of 0.5 wt.% Ce and 0.7 wt.% Eu.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Structural Engineering (AREA)
- Luminescent Compositions (AREA)
Abstract
Description
Claims
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CN2007800403180A CN101595200B (zh) | 2006-11-02 | 2007-10-31 | 发光物质 |
EP07819502A EP2092042A1 (de) | 2006-11-02 | 2007-10-31 | Leuchtstoffe |
US12/513,449 US8357313B2 (en) | 2006-11-02 | 2007-10-31 | Luminescent substances |
JP2009535023A JP5447836B2 (ja) | 2006-11-02 | 2007-10-31 | 発光物質 |
KR1020097011343A KR101289762B1 (ko) | 2006-11-02 | 2007-10-31 | 발광체 |
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DE102006051757A DE102006051757A1 (de) | 2006-11-02 | 2006-11-02 | Leuchtstoffe |
DE102006051757.1 | 2006-11-02 |
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WO2008052771A1 true WO2008052771A1 (de) | 2008-05-08 |
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US (1) | US8357313B2 (de) |
EP (1) | EP2092042A1 (de) |
JP (1) | JP5447836B2 (de) |
KR (1) | KR101289762B1 (de) |
CN (1) | CN101595200B (de) |
DE (1) | DE102006051757A1 (de) |
WO (1) | WO2008052771A1 (de) |
Cited By (1)
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CN102159665A (zh) * | 2008-09-15 | 2011-08-17 | 马普科技促进协会 | 氮化物基荧光体的制备 |
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DE102006051756A1 (de) * | 2006-11-02 | 2008-05-08 | MAX-PLANCK-Gesellschaft zur Förderung der Wissenschaften e.V. | Lichtquelle |
US9266558B2 (en) | 2010-09-15 | 2016-02-23 | GM Global Technology Operations LLC | Methods, systems and apparatus for steering wheel vibration reduction in electric power steering systems |
US9440674B2 (en) | 2010-09-15 | 2016-09-13 | GM Global Technology Operations LLC | Methods, systems and apparatus for steering wheel vibration reduction in electric power steering systems |
KR20120061343A (ko) * | 2010-12-03 | 2012-06-13 | 삼성엘이디 주식회사 | 형광체 제조방법 및 발광 장치 |
CN102533251B (zh) * | 2010-12-24 | 2015-09-30 | 陈文通 | 一种含钐和锌荧光材料及其制备方法 |
CN115480351A (zh) * | 2022-09-15 | 2022-12-16 | 四川天邑康和通信股份有限公司 | 一种室内隐形光缆及其制备方法 |
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WO2005049763A1 (en) * | 2003-11-19 | 2005-06-02 | Matsushita Electric Industrial Co., Ltd. | Method for producing nitridosilicate-based compound, nitridosilicate phosphor, and light-emitting apparatus using the nitridosilicate phosphor |
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DE4107108A1 (de) * | 1991-03-06 | 1992-09-10 | Bayer Ag | Siliciumbornitridkeramik und vorlaeuferverbindungen, verfahren zu deren herstellung sowie deren verwendung |
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2006
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- 2007-10-31 EP EP07819502A patent/EP2092042A1/de not_active Withdrawn
- 2007-10-31 WO PCT/EP2007/009470 patent/WO2008052771A1/de active Application Filing
- 2007-10-31 JP JP2009535023A patent/JP5447836B2/ja not_active Expired - Fee Related
- 2007-10-31 KR KR1020097011343A patent/KR101289762B1/ko not_active IP Right Cessation
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CN102159665A (zh) * | 2008-09-15 | 2011-08-17 | 马普科技促进协会 | 氮化物基荧光体的制备 |
JP2012503034A (ja) * | 2008-09-15 | 2012-02-02 | マックス−プランク−ゲゼルシャフト・ツア・フェルデルング・デア・ヴィッセンシャフテン・エー・ファオ | 窒化物ベースの蛍光体の製造 |
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KR20090082265A (ko) | 2009-07-29 |
US20100012897A1 (en) | 2010-01-21 |
JP5447836B2 (ja) | 2014-03-19 |
EP2092042A1 (de) | 2009-08-26 |
DE102006051757A1 (de) | 2008-05-08 |
US8357313B2 (en) | 2013-01-22 |
WO2008052771A8 (de) | 2009-07-30 |
KR101289762B1 (ko) | 2013-07-26 |
JP2010508411A (ja) | 2010-03-18 |
CN101595200B (zh) | 2013-01-02 |
CN101595200A (zh) | 2009-12-02 |
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