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Filler, glass composition, and method for producing hexagonal phosphate

A technology of crystalline phosphate and manufacturing method, which is applied in the direction of phosphorus compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problem of large thermal expansion coefficient, insufficient reduction of thermal expansion coefficient of packaging materials, and damage to the fluidity of packaging material compositions. Packaging materials Solve problems such as melt fluidity and achieve excellent processability and low thermal expansion

Inactive Publication Date: 2015-04-22
TOAGOSEI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] The lead-free low-melting point glass that has been widely used recently has a larger thermal expansion coefficient than the conventional lead-containing glass, so the known low-thermal expansion fillers described in Patent Documents 1 to 3 have insufficient effects, even if a large amount of filler is added. , also has the following problems: the thermal expansion coefficient of the encapsulation material cannot be sufficiently reduced, or the fluidity of the encapsulation material composition and the melt fluidity of the encapsulation material are impaired

Method used

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  • Filler, glass composition, and method for producing hexagonal phosphate
  • Filler, glass composition, and method for producing hexagonal phosphate
  • Filler, glass composition, and method for producing hexagonal phosphate

Examples

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Embodiment

[0106] Hereinafter, although an Example demonstrates this invention, this invention is not limited to an Example. Chemical formula The synthesized hexagonal phosphate is dissolved in hydrofluoric acid and nitric acid, and the content of metal and P component contained is measured by ICP emission analysis method to calculate the chemical formula. The other species were analyzed and calculated in the same manner, and those containing crystal water were analyzed by Tg-DTA to measure the water content to determine the chemical formula, and the chemical purity related to the determined chemical formula was calculated. The generation of hexagonal crystal phase was confirmed by powder X-ray diffraction, and the crystal purity was judged according to the standard X-ray diffraction pattern, and the product of chemical purity and crystal purity was regarded as purity. The average diameter and the maximum particle diameter were measured using a laser diffraction particle size distributio...

Embodiment 2

[0115] ○Synthesis of hexagonal phosphate B

[0116] Mix 904g of α layered zirconium phosphate (Zr(HPO) with an average diameter of 2 μm with a 20L Henschel mixer 4 ) 2 ·H 2 O) NS-10TZ manufactured by Toya Synthesis and 147g of zirconium oxyhydroxide (ZrO(OH) 2 ·H 2 O), 70g of magnesium hydroxide (Mg(OH) 2 ) reagent for 5 minutes. 2 L of water was added thereto to form a slurry, which was placed in an enamel container having a square shape of 30 cm and a depth of 10 cm, and dried at 150° C. for 24 hours.

[0117] The dried block was placed in a sagger made of alumina, and sintered at 900° C. (heating time 6 hours) for 6 hours in an electric furnace. The sintered block is pulverized with a ball mill, and further pulverized into primary particles with a jet mill to obtain hexagonal phosphate B. Powder X-ray diffraction measurement was performed in the same manner as in Example 1, and it was confirmed that there were no other crystalline impurities other than hexagonal crys...

Embodiment 3

[0119] ○Synthesis of hexagonal phosphate C

[0120] Mix 904g of α layered zirconium phosphate (Zr(HPO) with an average diameter of 2 μm with a 20L Henschel mixer 4 ) 2 ·H 2 O) NS-10TZ produced by Toya Synthesis and 165g of niobic acid (including Nb 2 o 5 :H 2 O, as Nb 2 o 5 The purity is 80% by weight), the calcium hydroxide reagent of 90g 5 minutes. 2 L of water was added thereto to form a slurry, which was placed in an enamel container having a square shape of 30 cm and a depth of 10 cm, and dried at 150° C. for 24 hours.

[0121] The dried block was placed in a sagger made of alumina, and sintered for 6 hours at 1200° C. (heating time 6 hours) in an electric furnace. The sintered block is pulverized with a ball mill, and further pulverized into primary particles with a jet mill to obtain hexagonal phosphate C. Powder X-ray diffraction measurement was performed in the same manner as in Example 1, and it was confirmed that there were no other crystalline impurities o...

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Abstract

The purpose of the present invention is to provide: a filler which does not contain an alkali metal in the composition, and a small amount of which is capable of greatly decreasing the thermal expansion coefficient of a glass composition if added thereinto; a glass composition which uses this filler; and a production method wherein a hexagonal phosphate, which does not contain an alkali metal in the composition and is suitable for use as the above-mentioned filler, can be produced by a simple and industrially advantageous process. A filler of the present invention is characterized by being composed of particles of a hexagonal phosphate represented by formula (1) and having a volume-based median diameter within the range of from 0.05 mum to 10 mum (inclusive) as determined using a laser diffraction particle size distribution measuring instrument. A method for producing a hexagonal phosphate of the present invention is characterized by comprising: a step for obtaining a mixture by blending a layered tetravalent metal phosphate, a compound of at least one divalent metal that is selected from the group consisting of alkaline earth metals, Zn, Cu, Ni and Mn, and an m-valent metal compound; and a step for obtaining a hexagonal phosphate represented by formula (1) by firing the mixture. AxByCz(PO4)3.nH2O (1)

Description

technical field [0001] The present invention relates to fillers composed of hexagonal phosphate particles and glass compositions comprising the same. Since the composition containing the filler of the present invention has a low coefficient of thermal expansion, it can be used as a packaging material for electronic components such as cathode ray tubes, plasma display panels (PDP), fluorescent display tubes, and organic EL. [0002] Also, the present invention relates to a method for producing hexagonal phosphate using tetravalent metal layered phosphate as a raw material. The hexagonal phosphate obtained by this production method can be used as a filler for compositions such as glass and resin, so that the thermal expansion coefficient of the cured product can be reduced, so it can be mainly used in cathode ray tubes and plasma display panels (PDP). , Fluorescent display tubes, organic EL and other packaging materials for electronic components. Background technique [0003...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C8/24C01B25/45
CPCC03C8/24C01B25/45C03C14/004C08K3/32C08K2003/325C08K2003/328C08K2003/327
Inventor 橘美树大野康晴
Owner TOAGOSEI CO LTD