CN1206314C - Acumulating self-luminescence material with long afterglow and its preparing method - Google Patents

Abstract

The present invention relates to an energy-accumulating self-luminescence material with long afterglow and a preparation method thereof. The raw material of the present invention comprises base materials, a dominant activator and selective activators, wherein the molar composition of the base materials is 0.9 to 1.2 of aluminum hydroxide, 1.0 to 2.2 of strontium carbonate, 0.8 to 1.2 of boric acid, 0.045 to 0.055 of diammonium hydrogen phosphate and 0.18 to 0.5 of calcium carbonate, the molar composition of the dominant activator is 0.01 to 0.012 of europium oxide, and the molar composition of the selective activators is 0.0045 to 0.011 of dysprosium oxide, 0.01 to 0.012 of lanthanum oxide and 0.0045 to 0.0055 of neodymium oxide. The present invention has the preparation method that the europium oxide and the strontium carbonate are added in a nitrite acid solution for sufficient dissolving, the solution is compounded to weakly alkaline, and sediment is separated, filtered and dried. The boric acid, the diammonium hydrogen phosphate, the aluminium hydroxide and the calcium carbonate are added and ground for 1 to 2 hours. The powder is moved to a crucible, is covered by sufficient carbon powder and is calcined for 0.5 to 3.5 hours at 1250 to 1500 DEG C. After cooled, finished products are prepared according to requirements. The present invention has the advantages of short excitation time, long afterglow time, complete color, no radioactivity, simple production technique, no environmental pollution and low cost.

Description

Long-afterglow energy-accumulating self-luminescent material and preparation method thereof

Technical field

The invention belongs to luminescent material, particularly a kind of long-afterglow energy-accumulating self-luminescent material and preparation method thereof.

Background technology

Traditional energy-storing self-luminescent material mainly is an all-sulphide phosphor, because the time of persistence of this class luminescent material is short, radioactivity is arranged, and poor stability will carry out coating and handle during use, and its application region is limited.Thereafter high temperature solid-state hydrogen of Cai Yonging or ammonia reduction reaction must at high temperature be carried out, and have the working condition harshness, and complex process is invested problems such as bigger, and product stability is poor.

Summary of the invention

Purpose of the present invention is intended to solve the deficiencies in the prior art, it mainly is improvement to traditional processing technology, by generating new crystalline texture body, and prepare a kind of "dead", the accumulation of energy time is short, brightness is high, time of persistence is long luminescent material, and technology is simple, production safety.

Basic foundation of the present invention is: aluminium hydroxide can generate α type and γ type alumina mixture through heat, and through adding the europium thing, dysprosium thing, neodymium compound, lanthanide etc. are base-material with Strontium carbonate powder, lime carbonate as activator again, form xln jointly.And the adding of boride, make its (because boron and aluminum ions radius different produce distortion) produce can trapped electron crystalline structure " trap ", by " trap " to electronics " capturing " and progressively discharge, cause electronic level by senior to rudimentary decay, show with the form that discharges photon.Thereby the high brightness of luminescent material, the effect of steady persistence have been realized.The mole of its raw material consists of: base-material: aluminium hydroxide 0.9～1.2, Strontium carbonate powder 1.0～2.2, boric acid 0.8～1.2, Secondary ammonium phosphate 0.045～0.055, lime carbonate 0.18-0.5; Dominant activator: europium sesquioxide 0.01～0.012; Selectively activate agent: dysprosium oxide 0.0045～0.011, lanthanum trioxide 0.01～0.012, Neodymium trioxide 0.0045～0.0055.

Its operation steps is as follows:

A, in salpeter solution, add europium sesquioxide, Strontium carbonate powder, stir simultaneously, dissolve;

B, in a solution, add ammoniacal liquor, transfer to weakly alkaline, PH=7.5～8.5, the throw out of separating out filters, oven dry;

C, in the product of b, add boric acid, Secondary ammonium phosphate, aluminium hydroxide, lime carbonate, ground 1～2 hour;

D, c material is moved in the crucible, on cover the capacity carbon dust, 1250～1500 ℃ of following roastings 0.5～3.5 hour;

E, the mixture of d is cooled to room temperature, makes powder on demand and get product.

Through the luminescent material of method for preparing, firing time short (5～20 minutes), time of persistence, long (8-24 hour), color complete (green, blueness, purple, yellow etc.) were "dead", safe, stable, efficient, energy-conservation, be widely used.And production technique is simple, and non-environmental-pollution is with low cost.

Embodiment

Example one

1, gets the salpeter solution of 20% concentration, add 3.36～4.10 gram dysprosium oxides, 3.52～4.22 gram europium sesquioxides and 296～320 gram Strontium carbonate powders therein, after stirring half an hour, in solution, add ammoniacal liquor, transfer pH value to reach between 7.5～8.5, throw out filtering drying with producing in the solution can get mixture A1.

2, add 5.95～7.22 gram Secondary ammonium phosphates, 62～70 gram boric acid and 75～85 gram aluminium hydroxides in the A1 mixture in succession, put into grinding in ball grinder and get mixture B1 after 1～2 hour.

3, mixture B1 is put into crucible, on the raw material surface, cover one deck carbon dust then.

4, crucible is put into be preheating to 500-550 degree centigrade retort furnace, heat up and be heated to 1280～1350 degrees centigrade, constant temperature 1～2 hour is reduced to temperature in the stove below 450～500 degrees centigrade and is taken out crucible, is cooled to room temperature.Promptly get the green emitting powder after pulverizing grinding.

Example two

1, gets the salpeter solution of 20% concentration, add 3.6～4.2 gram europium sesquioxides, 1.52～1.83 gram Neodymium trioxide and 148～170 gram Strontium carbonate powders, fully stir half an hour.In solution, add ammoniacal liquor, transfer pH value to reach 7.5～8.5, after producing the throw out filtering drying in the solution, can get mixture A2.

2, add 6.0～7.0 gram Secondary ammonium phosphates, 50～60 gram boric acid and 71～85 gram aluminium hydroxides, 43～49 gram lime carbonate in the A2 mixture in succession, put into grinding in ball grinder 1～2 hour, get mixture B2.

3, mixture B2 is put into crucible, on the raw material surface, cover one deck carbon dust then.

4, the crucible that will install material is put into and is preheating to 500～550 degrees centigrade retort furnace, heats up and is heated to 1280～1350 degrees centigrade, constant temperature 1～2 hour.Be cooled to below 450～500 degrees centigrade and take out crucible, be cooled to room temperature, pulverizing promptly gets the violet light powder after grinding.

Example three

1, gets the salpeter solution of 20% concentration, add 3.52～4.20 gram europium sesquioxides, 1.73～1.85 gram dysprosium oxides, 3.3～3.8 gram lanthanum trioxides and 149～170 gram Strontium carbonate powders, after stirring half an hour, transfer between pH value to 7.5～8.5 with ammoniacal liquor, throw out filters with producing in the solution, oven dry, can get mixture A3.

2, add 6.0～7.0 gram Secondary ammonium phosphates in the A3 mixture in succession, 51～60 gram boric acid and 83～92 gram aluminium hydroxides, 19～24 gram lime carbonate were put into grinding in ball grinder 1～2 hour, got mixture B3.

3, mixture B3 is put into crucible, on the raw material surface, cover one deck carbon dust.

4, the crucible that will install material is put into and is preheating to 500～550 degrees centigrade retort furnace, heats up and is heated to 1280～1350 degrees centigrade, constant temperature 1～2 hour, temperature in the stove is reduced to below 450-500 degree centigrade, take out crucible, be cooled to room temperature, pulverizing promptly gets the blue-light-emitting powder after grinding.

Claims (2)

1, the long-afterglow energy-accumulating self-luminescent material is to be basic raw material with aluminium hydroxide, boric acid, Strontium carbonate powder, lime carbonate, Secondary ammonium phosphate, add the dominant activator europium sesquioxide, and add optionally activator, comprise: dysprosium oxide, lanthanum trioxide, Neodymium trioxide, the mole that it is characterized in that each raw material consists of base-material: aluminium hydroxide 0.9～1.2, Strontium carbonate powder 1.0～2.2, boric acid 0.8～1.2, Secondary ammonium phosphate 0.045～0.055, lime carbonate 0.18-0.5; Dominant activator: europium sesquioxide 0.01～0.012; Alternative activator: dysprosium oxide 0.0045～0.011, lanthanum trioxide 0.01～0.012, Neodymium trioxide 0.0045～0.0055.

2, the preparation method of long-afterglow energy-accumulating self-luminescent material is characterized in that the described prescription of claim 1 is carried out following preparation process:

A, in salpeter solution, add europium sesquioxide, Strontium carbonate powder, stir simultaneously, dissolve;

B, in a solution, add ammoniacal liquor, transfer to weakly alkaline, PH=7.5～8.5, the throw out of separating out filters, oven dry;

C, in the product of b, add boric acid, Secondary ammonium phosphate, aluminium hydroxide, lime carbonate, ground 1～2 hour;

D, c material is moved in the crucible, on cover the capacity carbon dust, 1250～1500 degrees centigrade of following roastings 0.5～3.5 hour;

E, the mixture of d is cooled to room temperature, makes powder on demand and get product.