CN1218084A - Preparation of fluorescent powder for dysprosium and lead dosed high voltage mercury lamp - Google Patents

Abstract

A process for preparing dysprosium-lead co-diffused fluorescent powder for high-tension mercury lamp features that ytterbium vanadophosphate is used as matrix material and dysprosium is used as activating ions, and includes high-temp calcining in air. The lead ions partially replace dysprosium ions to activate the ytterbium's cations in ytterbium vanadophosphate, so the luminous performance of fluorescent powder is greatly improved, resulting in higher light intensity.

Description

Dysprosium, the plumbous preparation method who mixes the high-pressure mercury lamp phosphor altogether

The invention belongs to dysprosium, the plumbous preparation method who mixes the high-pressure mercury lamp phosphor altogether.

High voltage mercury lamp is a kind of lighting that is widely used at present, is mainly used in the illumination in road and other place.The principle of work of this kind light fixture is that the ultraviolet ray excited fluorescent material that is applied to the glass lamp housing inboard based on 365nm that utilizes the high-pressure mercury vapor discharge to be produced produces as seen luminous.Employed fluorescent RE powder mainly is europkium-activated vanadic acid yttrium and vanadium yttrium phosphate in high voltage mercury lamp at present.English Patent Brit.1,135,304 (C1.09k), General Electric Company discloses and has been entitled as " preparation that europium activates the vanadic acid yttrium "; It is that the feedstock production europium activates vanadic acid yttrium phosphor powder that this method has been reported with yttrium oxide, europium sesquioxide and Vanadium Pentoxide in FLAKES.United States Patent (USP) U.S.3,647,706 (C1.301-4p; C09k), people such as Lagos discloses and has been entitled as " preparation that europium activates vanadium yttrium phosphate fluorescent material "; It is that raw material prepares the method that europium activates lamp phosphor in 1200-1400 ℃ of calcination that this patent has been reported with yttrium oxide, europium sesquioxide, primary ammonium phosphate and ammonium vanadate.Though above-mentioned two kinds of fluorescent material all have preferable performance, owing to will use content rareness in rare-earth mineral, expensive europium sesquioxide and make the cost of this type of fluorescent material higher.The lamp phosphor that with the dysprosium is active ions also has report.United States Patent (USP) U.S.3 for example, 501,412 (C1.252-301.4; C09k), R.Ropp discloses the patent that is entitled as " activated by dysprosium rare-earth vanadate fluorescent material "; This method is a feedstock production geseous discharge lamp phosphor with rare earth oxide and Vanadium Pentoxide in FLAKES.Japanese Patent JP 02 28,283,[90 28,283] (C1.C09K11/83), K.Nakagawa discloses the patent that is entitled as " the white luminous fluorescent material of rare earth use for discharge lamp "; The described fluorescent material of this patent consist of Y _1-xDy _xV _1-yP _yO ₄

The present invention finds by a large amount of experiment screening, partly replaces the luminescent properties that yttrium positively charged ion in the activated by dysprosium vanadium yttrium phosphate can significantly improve fluorescent material with lead ion, improves the luminous intensity of fluorescent material largely; Compare with not leaded ionic activated by dysprosium fluorescent material, the luminous intensity of plumbiferous corresponding fluorescent material can improve about 20%.Owing to used the europium sesquioxide that has replaced few amount and high price at the big inexpensive dysprosium oxide of China's amount,, also expanded new approach for the development and use of dysprosium oxide so the present invention can reduce the production cost of fluorescent material.

The objective of the invention is the mode of mixing altogether with dysprosium oxide, plumbous oxide, the high temperature sintering in air such as yttrium oxide, Vanadium Pentoxide in FLAKES and primary ammonium phosphate that is equipped with respective numbers prepares the high-pressure mercury lamp phosphor.

The present invention at high temperature prepares the vanadium yttrium phosphate matrix compounds according to the principle of high temperature solid state reaction; The method that adopts positively charged ion to replace is introduced the case of ruthenium ion in the vanadium yttrium phosphate matrix by solid state reaction with dysprosium and lead ion under the condition of high temperature, thereby prepares dysprosium, lead is mixed fluorescent material altogether.The ultraviolet ray based on 365nm that high-pressure mercury vapor discharge is produced is at first absorbed by the anionic group in the material, and then the mode of intensity of activation by the non-radiative energy transmission is transported to the dysprosium ion that occupies the ruthenium ion case and makes it be in excited state and produce white luminous.

The present invention presses following mixed with yttrium oxide, dysprosium oxide, plumbous oxide, Vanadium Pentoxide in FLAKES and primary ammonium phosphate:

Y _1-x-y(VO ₄) _1-a(PO ₄) _a∶Dy _x,Pb _y

Wherein: 0.005≤x≤0.02,0.005≤y≤0.02,0.10≤a≤0.80 mixture mixes the back in 400 ℃ of calcinations 4 hours in air through grinding, take out after the grinding again in 1200-1400 ℃ in air calcination 4-8 hour.Product is white powder fluorescent material after grinding, wash, drying.

Embodiment provided by the invention is as follows:

1. with 55.32 gram yttrium oxide, 22.74 gram Vanadium Pentoxide in FLAKESs, 28.76 gram primary ammonium phosphates, 0.93 gram dysprosium oxide and 1.12 gram plumbous oxide mixings, porphyrize; Mixture was in 400 ℃ of calcinations 4 hours; Take out behind the porphyrize again in 1300 ℃ of calcinations 8 hours; The product porphyrize after washing, oven dry promptly get and consist of Y _0.98(VO ₄) _0.50(PO ₄) _0.50: Dy _0.01, Pb _0.01White fluorescent powder.Coated the inside and outside town of 250W high voltage mercury lamp with this fluorescent material, luminous efficiency is respectively 19.17lm/w and 48.80lm/w.

2. with 1.117 gram yttrium oxide, 0.728 gram Vanadium Pentoxide in FLAKES, 0.230 gram primary ammonium phosphate, 0.009 gram dysprosium oxide and 0.011 gram plumbous oxide mixing, porphyrize; Mixture was in 400 ℃ of calcinations 4 hours; Take out behind the porphyrize again in 1200 ℃ of calcinations 6 hours; The product porphyrize after washing, oven dry promptly get and consist of Y _0.99(VO ₄) _0.80(PO ₄) _0.20: Dy _0.005, Pb _0.005White fluorescent powder.This fluorescent material all produces strong white luminous under the exciting of 365nm and 254nm mercury line.

3. with 1.095 gram yttrium oxide, 0.181 gram Vanadium Pentoxide in FLAKES, 0.923 gram primary ammonium phosphate, 0.028 gram dysprosium oxide and 0.034 gram plumbous oxide mixing, porphyrize; Mixture was in 400 ℃ of calcinations 4 hours; Take out behind the porphyrize again in 1400 ℃ of calcinations 4 hours; The product porphyrize after washing, oven dry promptly get and consist of Y _0.97(VO ₄) _0.20(PO ₄) _0.80: Dy _0.015, Pb _0.015White fluorescent powder.This fluorescent material all produces strong white luminous under the exciting of 365nm and 254nm mercury line.

Claims (1)

1. a dysprosium, the plumbous preparation method who mixes the high-pressure mercury lamp phosphor altogether is characterized in that yttrium oxide, dysprosium oxide, plumbous oxide, Vanadium Pentoxide in FLAKES and primary ammonium phosphate by following mixed:

Y _1-x-y(VO ₄) _1-a(PO ₄) _a∶Dy _x,Pb _y

Wherein: 0.005≤x≤0.02,0.005≤y≤0.02,0.10≤a≤0.80 mixture mixes the back in 400 ℃ of calcinations 4 hours in air through grinding, take out after the grinding again in 1200-1400 ℃ in air calcination 4-8 hour.Product is white powder fluorescent material after grinding, wash, drying.