WO2008062693A1 - Procédé de fabrication d'un précurseur de substance fluorescente - Google Patents

Procédé de fabrication d'un précurseur de substance fluorescente Download PDF

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Publication number
WO2008062693A1
WO2008062693A1 PCT/JP2007/072003 JP2007072003W WO2008062693A1 WO 2008062693 A1 WO2008062693 A1 WO 2008062693A1 JP 2007072003 W JP2007072003 W JP 2007072003W WO 2008062693 A1 WO2008062693 A1 WO 2008062693A1
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WIPO (PCT)
Prior art keywords
group
compound
particle size
particles
phosphor
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PCT/JP2007/072003
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English (en)
Japanese (ja)
Inventor
Jun Takai
Hideharu Iwasaki
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Kuraray Luminas Co., Ltd.
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Priority to JP2008545367A priority Critical patent/JP5300490B2/ja
Publication of WO2008062693A1 publication Critical patent/WO2008062693A1/fr

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    • 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

Definitions

  • the present invention relates to a method for producing a ⁇ - ⁇ group compound semiconductor particle useful for producing an inorganic phosphor.
  • a method for producing phosphor precursor particles having a uniform particle size by controlling the particle size distribution of aggregates (secondary particles) composed of primary particles of a ⁇ - ⁇ group compound semiconductor, and obtained by the same method The present invention relates to phosphor precursor particles.
  • II-VI group compound semiconductors for example, compound semiconductors mainly composed of zinc sulfide or the like are doped with an activating element such as manganese, copper, silver, terbium, thulium, europium, or fluorine in the crystal structure. Thereafter, when further heat treatment or the like is performed, the light emission phenomenon is exhibited by irradiation with light, electrons or the like or application of voltage. Therefore, the above compound semiconductor is useful as a host material for phosphors, and in particular, compound semiconductor particles mainly composed of zinc sulfide or the like are used in plasma displays, electret luminescent displays, field emission displays, etc. It can be a precursor for producing a phosphor used in a display device.
  • an activating element such as manganese, copper, silver, terbium, thulium, europium, or fluorine in the crystal structure.
  • the term "precursor” means a compound semiconductor doped with an activator, which is in a stage before being subjected to heat treatment or the like.
  • a compound semiconductor doped with an activator exhibits properties as a phosphor only after being subjected to heat treatment or the like. Therefore, the precursor in the previous stage to become a phosphor is strictly different from the phosphor itself. Indicates a distinction.
  • Methods for synthesizing phosphor precursors based on zinc sulfide include a method using a solid phase reaction and a method using a reaction in a liquid phase.
  • the raw material zinc sulfide particles are grown together with inorganic salts called fluxes from 800 ° C to 1300 ° C at the very first temperature to grow into micron-sized particles.
  • second calcination at 500 ° C. and 1000 ° C. to obtain phosphor particles (see Patent Documents !! to 3).
  • the solid phase synthesis method has a limit in obtaining a phosphor with higher brightness by doping the zinc sulfide matrix with an activator.
  • the concentration distribution of the activator or coactivator inside the obtained phosphor particles can be homogenized.
  • Phosphor particles are formed through two processes, nucleation and particle growth. By controlling the degree of supersaturation during particle growth, monodisperse particles with a narrow particle size distribution are used. A product can be obtained.
  • the phosphor base material and each raw material component solution containing the constituent elements of the activator or coactivator are mixed to coprecipitate the phosphor base crystal, activator or coactivator.
  • a method for producing a phosphor by precipitation is disclosed (see Patent Document 6).
  • a method for producing a II-VI compound semiconductor a method of reacting a Group 11 element-containing compound with a Group VI element-containing amide compound such as thioacetamide under hydrothermal conditions is also disclosed (Patent Document 7 and Non-Patent Document 7). (See Patent Literature 1).
  • Patent Document 1 JP-A-8-183954
  • Patent Document 2 JP-A-7-62342
  • Patent Document 3 JP-A-6-330035
  • Patent Document 4 Japanese Patent Laid-Open No. 2005-306713
  • Patent Document 5 JP-A-2005-139372
  • Patent Document 6 Japanese Unexamined Patent Application Publication No. 2005-132947
  • Patent Literature 7 Special Table 2004-520260
  • Non-Patent Document 1 J. Chem. Soc. Faraday Trans., 1 (80) 563—570 (1984) Disclosure of the Invention
  • the phosphor particles obtained by the methods disclosed in Patent Documents 4 to 7 and the like are fine primary particles having an average particle diameter of about several nanometers. These primary particles can aggregate with each other to form secondary particles having a particle size of several hundreds of micrometers, while there may be particles that remain as small particles having a particle size of several nanometers to several tens of nanometers. This gives a particle product with a broad particle size distribution. Particle products with large variations in particle size have irregular particle shapes and a large difference in sedimentation speed, which requires complicated processes such as particle recovery and washing, or a very long time. There is a problem in that it is inconvenient to handle. Therefore, it has been desired to develop a method for preparing monodispersed phosphor precursor particles having a narrow particle size distribution.
  • the present inventors made a reaction between a group II element and a raw material compound containing a group VI element in an aqueous liquid phase to which an electrolyte compound composed of a specific metal salt was added. It was found that when primary particles of a Group VI compound semiconductor were produced, the primary particles were further aggregated to form secondary particles having a uniform particle size, and the present invention was completed.
  • the present invention adds a group VI element-containing amide compound to an aqueous liquid phase containing an electrolyte compound composed of an inorganic acid salt or an organic acid salt of a typical metal and a group II element-containing compound, and ⁇ - ⁇
  • a method for producing a group II-VI phosphor precursor characterized in that particles of a group III compound semiconductor are produced.
  • the II-VI group compound semiconductor particles obtained by the present invention are not limited to the primary particles generated by the reaction with the Group II element-containing compound immediately after the addition of the Group VI element-containing amide compound. Secondary particles (aggregates) formed by aggregation in the liquid phase are also included. Therefore, another embodiment of the present invention is an aggregate of II-VI compound semiconductors represented by D.
  • the aggregate is characterized by an average particle size of 8-30 m and a standard deviation of 0.0;! -0.2.
  • II-VI compound semiconductor particles whose particle size distribution is controlled to be monodispersed can be obtained. Therefore, if the phosphor precursor particles obtained by the present invention are used, the efficiency of the steps such as the washing and recovery operation of the particles is remarkably improved, and The efficiency of the entire manufacturing process of the light body can be improved.
  • FIG. 1 Particle size distribution of phosphor precursor particles obtained in Example 1 (A)
  • FIG. 2 SEM photograph of phosphor precursor particles obtained in Example 1 (A) (upper photo: sukeno-reno 10 ⁇ 111, magnification 3000 times, lower photo: scale bar 60 ⁇ 111, magnification 60 times) )
  • FIG. 4 Particle size distribution of phosphor precursor particles obtained in Example 3
  • FIG. 5 Particle size distribution of phosphor precursor particles obtained in Example 4.
  • FIG. 6 Particle size distribution of phosphor precursor particles obtained in Example 6
  • FIG. 7 Particle size distribution of phosphor precursor particles obtained in Example 7
  • FIG. 8 Particle size distribution of phosphor precursor particles obtained in Example 8.
  • FIG. 9 Particle size distribution of phosphor precursor particles obtained in Comparative Example 1
  • FIG. 10 SEM photograph of phosphor precursor particles obtained in Comparative Example 1 (scale bar 6 am, magnification 5000 times)
  • FIG. 11 Particle size distribution of phosphor precursor particles obtained in Comparative Example 2
  • II group VI compound semiconductor used in the present application is composed of group II elements (Be, Mg, Zn, Cd, Hg) and group VI elements (O, S, Se, Te). It is a general term for binary compound semiconductors and mixed crystal semiconductors. Examples of II-VI group compound semiconductors used in the present invention include zinc sulfide, zinc selenide, cadmium sulfide, cadmium selenide, and the like. ⁇ It may be partially replaced by non-metal ions (activator or coactivator).
  • Group II element-containing compounds used in the present invention are not particularly limited, but include inorganic acid salts such as zinc chloride, zinc nitrate, zinc sulfate, cadmium chloride, cadmium nitrate, cadmium sulfate, and zinc acetate.
  • Organic acid salts such as zinc propionate, zinc oxalate, cadmium acetate, cadmium propionate, and cadmium oxalate can be used. These compounds may be used alone or in combination. This compound can be used at any concentration, but if the concentration is too high, II-VI compound semiconductors are produced.
  • the group II element-containing compound is used at a concentration of 0.01 mol / liter to 5 mol / liter, preferably 0.1 mol / liter to 2 mol / liter.
  • thioamides such as thioformamide, thioacetamide, and thiopropionamide can be used. These may be used singly or as a mixture of a plurality of types, but thioacetamide is preferably used from the viewpoints of economy and availability.
  • thioamides considering reaction efficiency and volumetric efficiency, 1.0 to 100 times, preferably 1.7 to 30 times, more preferably, relative to the number of moles of the group X element-containing compound 1. Use in an amount that gives 9 to 5 times the number of moles.
  • the liquid phase medium used in the present invention is typically water. Unless the solubility of the additive (electrolyte) described later is significantly reduced, a polar organic compound (for example, methanol, ethanol, etc.) In addition to alcohol!
  • a polar organic compound for example, methanol, ethanol, etc.
  • a mother substance produced by adding a compound containing an activator or a coactivator element capable of becoming a luminescence center in an aqueous liquid phase together with a group II element-containing compound and a group VI element-containing amide.
  • the element crystal can be doped with ions of the element.
  • Elements that can be used as the emission center include transition metals such as manganese, copper, silver, gold, and iridium, halogens such as chlorine, iodine, and bromine, cerium, iridium, praseodymium, neodymium, samarium, europium, gadolinium, tenolebium, Rare earths such as dysprosium, honorium, enorebium, sillium, ytterbium. If necessary, examples include aluminum, gallium, indium, and halogens such as fluorine, chlorine, bromine and iodine which act as donors for the transition metals and rare earths that are acceptors.
  • transition metals such as manganese, copper, silver, gold, and iridium
  • halogens such as chlorine, iodine, and bromine
  • halides such as chloride, bromide and iodide
  • organic acid salts such as formic acid, acetic acid and propionic acid
  • complex salts such as acetylylacetonate and the like.
  • a coordinating compound such as pyridine and phosphine can be present together.
  • the amount used is usually a force ranging from 0.0001 parts by weight to 20 parts by weight as ions to be introduced with respect to 100 parts by weight of the ⁇ - ⁇ group compound semiconductor to be produced. In consideration of economy, the range is from 0.0002 to 10 parts by weight.
  • particles of a ⁇ - ⁇ group phosphor are generated by the reaction of the group II or group VI element-containing compound.
  • the primary particles of the phosphor particles are fine particles having a particle size of several nm to 30 nm, but further aggregate in the aqueous liquid phase in which the electrolyte compound is dissolved to form secondary particles of an appropriate size.
  • the particle size distribution of the secondary particles obtained by the present invention shows narrow monodispersity.
  • the average particle size of the agglomerates usually obtained is usually less than 30, im and the standard deviation is less than 0.2.
  • the average particle size of the agglomerates is 8-30 m and the standard deviation is 0.0;! -0.2.
  • particle size used herein means an average particle size obtained by determining the center particle size D50 from the particle size distribution curve unless otherwise specified.
  • the additive (flocculating agent) that can further agglomerate the primary particles generated in the aqueous liquid phase is not particularly limited as long as it is an electrolyte compound that can be dissolved in the aqueous liquid phase. It is preferable not to be mixed in the II-VI phosphor precursor. This is because if the ions generated when the electrolyte is dissolved in the liquid phase are mixed into the phosphor precursor, the performance as a phosphor deteriorates and the brightness decreases.
  • examples of the additive preferably used in the present invention include inorganic acids or organic acid salts of typical metals, and more preferable are inorganic acid salts or organic acid salts of alkaline earth metals.
  • Examples of the typical metal include metal elements such as magnesium, calcium, and sodium, and particularly preferable metals are magnesium and calcium.
  • additive compounds containing these metals the ability to use halides such as hydroxides, sulfates, nitrates, chlorides and bromides, and organic acid salts such as formic acid, acetic acid and propionic acid, especially water
  • halides such as hydroxides, sulfates, nitrates, chlorides and bromides
  • organic acid salts such as formic acid, acetic acid and propionic acid, especially water
  • oxides and sulfates is preferred.
  • the present invention can be carried out by adding the above compound in an arbitrary amount together with the Group II element-containing compound to the liquid phase in advance, and further adding a Group VI element-containing amide compound.
  • the addition amount of the additive compound is usually in the range of 0.0001 to 20 parts by weight with respect to 100 parts by weight of the IHV group compound semiconductor to be produced, but is preferable from the viewpoint of the agglomeration effect and economy. Is in the range of 0.0002 to 10 parts by weight. Also generate From the standpoint of controlling the particle size distribution of the aggregates to avoid mixing into the product, the preferred addition amount is 0.5 to 40 mol% based on the molar amount of the Group II-containing compound used. a range, particularly preferably in the range of 0.8 to 30 mole 0/0.
  • the II-VI group phosphor precursor can be produced by a batch method or a continuous method.
  • the temperature of the liquid phase is not particularly limited as long as the progress of the reaction and the agglomeration effect of the particles are not impaired, but varies depending on the type and amount (concentration) of components contained in the liquid phase. obtain.
  • the temperature of the liquid phase is adjusted to be in the range of 20 ° C to 120 ° C.
  • Liquid phase temperature control can be performed from outside the reaction vessel using a conventional temperature-controllable heating device, even if a temperature-controllable heating device is installed in the liquid phase. Good.
  • the method of the present invention is preferably carried out in the range of 60 ° C to 100 ° C, more preferably 65 ° C to 90 ° C.
  • the time required for carrying out the method of the present invention is appropriately determined by those skilled in the art by observing the progress of the reaction and the degree of formation of aggregated particles according to the conditions such as the scale of the implementation. Forces that can be selected Usually;! To 20 hours, preferably 3 to; the reaction can be carried out in 10 hours
  • the particle size distribution of the particle product is SALD— The distribution was evaluated by measuring with a laser diffraction scattering method using the 2100, and determining the median diameter D using the SALD-2100 analytical software attached to the instrument.
  • Example 1 Production of zinc sulfide particles
  • Example 1 (A) the same procedure as in Example 1 (A) was followed except that the amount of magnesium sulfate used was 3. Og (25 mmol, corresponding to 20 mol% of the molar amount of zinc nitrate). 19.9 g of zinc sulfide was obtained (yield 98%). The average particle size was 24.3 m.
  • Example 1 In Example 1 (A), the same procedure as in Example 1 (A), except that the amount of magnesium sulfate used was 0.3 g (2.5 mmol, corresponding to 2 mol% relative to zinc nitrate). According to the above, 11.3 g of zinc sulfide was obtained (yield 93%). The average particle size was 8.2 m. [0032]
  • Example 4 the same procedure as in Example 1 (A), except that the amount of magnesium sulfate used was 0.3 g (2.5 mmol, corresponding to 2 mol% relative to zinc nitrate). According to the above, 11.3 g of zinc sulfide was obtained (yield 93%). The average particle size was 8.2 m.
  • Example 1 (A) except that magnesium sulfate was changed to magnesium chloride hexahydrate 2.54 g (12.5 mmol, corresponding to 10 mol% of the molar amount of zinc nitrate), Example 1 (A) and In the same manner, 10.9 g of zinc sulfide was obtained (yield 89%). The average particle size was 18. 8 111.
  • Example 5 Production of manganese-doped zinc sulfide particles
  • Example 7 Production of copper gallium-doped zinc sulfide particles
  • Example 8 Production of silver gallium-doped zinc sulfide particles
  • Example 1 (A) was carried out in the same manner as in Example 1 (A) except that magnesium sulfate was not used, to obtain 11.8 g (yield 97%) of zinc sulfide.
  • the average particle size was 39.7 111.
  • Figure 9 shows the particle size distribution curve obtained for the particle product, and Figure 10 shows the SEM observation photograph.
  • the particle size distribution and standard deviation in Table 1 were determined based on the particle size distribution curves obtained in Examples and Comparative Examples. There is no significant difference in product yield between the examples and comparative examples, but the particle size distribution and standard deviation between the examples (1-8) and the comparative examples (1, 2). There are significant differences.
  • the average particle size of the particles obtained in the examples falls within the range of 8 to 30 111, which is not much larger than the extremely large value or extremely small value as obtained in the comparative example.
  • the standard deviation is less than 0.2, and it can be seen that there is little variation in the particle size of the generated particles. This difference in particle size distribution becomes more apparent from the shape of the particle size distribution curves in FIGS. In particular, from FIGS. 1 and 3 to 8, which correspond to the results of the examples of the present invention, the force S is used to confirm the monodispersity of the particle diameters of the particles obtained in the examples of the present invention.
  • the particle product is a combination of fine particles aggregated with each other! One larger particle is formed, the particle size is apparently uniform, and it can be seen that there is no significant difference in the external shape of each particle.
  • the SEM photograph of the particle product obtained from Comparative Example 1 (Fig. 10) According to the above, there are irregular shapes having irregular shapes, and the formation of apparently uniform particles as in Example 1 (A) has occurred! /, N! /, Force S confirmation it can.
  • the present invention provides a method for producing a monodispersed particle product having a narrow particle size distribution for II-VI group compound semiconductors, which are precursor compounds of inorganic phosphors. According to the production method of the present invention, it is possible to efficiently produce inorganic phosphor precursor particles that are easy to handle / in industrial processes. Furthermore, since the method of the present invention is a production method based on a liquid phase synthesis method, it is possible to uniformly introduce an activator or a coactivator element that can be a luminescence center into a base material compound. Useful for the production of phosphors with high brightness

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Luminescent Compositions (AREA)

Abstract

L'invention concerne un procédé de fabrication d'un précurseur d'une substance fluorescente d'un élément des groupes II-VI, caractérisé par l'ajout d'un composé amide contenant un élément du groupe VI à une phase liquide aqueuse contenant un composé d'électrolyte comprenant un sel d'acide inorganique ou un sel d'acide organique d'un métal typique et contenant un composé d'un élément du groupe II afin d'obtenir des particules d'un semi-conducteur d'un composé d'un élément des groupes II-VI. Le procédé permet de fabriquer un précurseur d'un semi-conducteur d'un composé d'un élément des groupes II-VI sous forme d'un produit de réaction particulaire monodispersé dont le diamètre de particule présente une inhomogénéité réduite. Le produit particulaire est constitué d'agrégats ayant un diamètre de particule moyen en termes de D50 de 8 à 30 µm et un écart type de 0,01 à 0,2.
PCT/JP2007/072003 2006-11-21 2007-11-13 Procédé de fabrication d'un précurseur de substance fluorescente WO2008062693A1 (fr)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008133289A1 (fr) * 2007-04-25 2008-11-06 Kuraray Luminas Co., Ltd. Phosphore bleu
EP2600395A4 (fr) * 2010-07-26 2016-05-25 Nissan Chemical Ind Ltd Composition de précurseur pour la formation d'une couche semi-conductrice d'oxyde métallique amorphe, couche semi-conductrice d'oxyde métallique amorphe, leur procédé de production et dispositif à semi-conducteur

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5382683A (en) * 1976-12-28 1978-07-21 Matsushita Electric Ind Co Ltd Production of fluorescent substance
JPH06299150A (ja) * 1993-04-20 1994-10-25 Matsushita Electric Ind Co Ltd 蛍光体及びその製造方法
JPH0790262A (ja) * 1993-09-27 1995-04-04 Nec Kansai Ltd 電界発光素子用蛍光体の製造方法
JPH0913029A (ja) * 1995-06-28 1997-01-14 Toshiba Corp 硫化亜鉛蛍光体
JP2006008806A (ja) * 2004-06-24 2006-01-12 Fuji Photo Film Co Ltd 蛍光体前駆体、エレクトロルミネッセンス蛍光体、それらの製造方法及び分散型エレクトロルミネッセンス素子

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5382683A (en) * 1976-12-28 1978-07-21 Matsushita Electric Ind Co Ltd Production of fluorescent substance
JPH06299150A (ja) * 1993-04-20 1994-10-25 Matsushita Electric Ind Co Ltd 蛍光体及びその製造方法
JPH0790262A (ja) * 1993-09-27 1995-04-04 Nec Kansai Ltd 電界発光素子用蛍光体の製造方法
JPH0913029A (ja) * 1995-06-28 1997-01-14 Toshiba Corp 硫化亜鉛蛍光体
JP2006008806A (ja) * 2004-06-24 2006-01-12 Fuji Photo Film Co Ltd 蛍光体前駆体、エレクトロルミネッセンス蛍光体、それらの製造方法及び分散型エレクトロルミネッセンス素子

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008133289A1 (fr) * 2007-04-25 2008-11-06 Kuraray Luminas Co., Ltd. Phosphore bleu
JP5583403B2 (ja) * 2007-04-25 2014-09-03 株式会社クラレ 青色蛍光体
EP2600395A4 (fr) * 2010-07-26 2016-05-25 Nissan Chemical Ind Ltd Composition de précurseur pour la formation d'une couche semi-conductrice d'oxyde métallique amorphe, couche semi-conductrice d'oxyde métallique amorphe, leur procédé de production et dispositif à semi-conducteur
US10756190B2 (en) 2010-07-26 2020-08-25 Nissan Chemical Industries, Ltd. Precursor composition for forming amorphous metal oxide semiconductor layer, amorphous metal oxide semiconductor layer, method for producing same, and semiconductor device

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JP5300490B2 (ja) 2013-09-25
TW200835775A (en) 2008-09-01

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