CN1260321C - Luminscent-powder in use for LED of white light, preparing method and electric light source produced - Google Patents

Luminscent-powder in use for LED of white light, preparing method and electric light source produced Download PDF

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CN1260321C
CN1260321C CNB031373356A CN03137335A CN1260321C CN 1260321 C CN1260321 C CN 1260321C CN B031373356 A CNB031373356 A CN B031373356A CN 03137335 A CN03137335 A CN 03137335A CN 1260321 C CN1260321 C CN 1260321C
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white light
phosphor
light led
manufacturing
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CN1539919A (en
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庄卫东
黄小卫
方英
何华强
赵春雷
张书生
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Grirem Advanced Materials Co Ltd
Beijing General Research Institute for Non Ferrous Metals
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

The present invention discloses a fluorescent powder for a white light LED, a manufacturing method thereof and a manufactured electric light source. A structural formula of the fluorescent powder is AxM (SiO4) 4X2: Eu<y>, Rz, wherein the A is at least one of Ca, SR and Ba; the M is at least one of Mg, Zn, Ti and Cd; the X is at least one of F, Cl, Br and I; the R is at least one of Dy, Ce, Pr and Tb; the x is more than 7 and is less than 12, the y is more than 0.001 and is less than 0.5, and the z is more than or equal to 0 and is less than 0.5. The manufacturing method comprises the steps: simple substances, oxides or corresponding salts of the elements in the structural formula are added in a fluxing agent, are synthesized by reduction reaction at high temperature after being uniformly mixed and ground, and then the material is obtained by post treatment, and moreover, the manufacturing method relates to selection, material mixture, reduction, post treatment, etc. of raw materials, such as substrates, activating agents, sensitizing agents, etc. The fluorescent powder of the present invention has the characteristics of good chemical stability, high luminous intensity, very wide excitation wavelength, etc. and has the advantages of simple manufacturing method, no pollution and low cost.

Description

A kind of phosphor for white light LED and manufacture method thereof and made electric light source
Technical field
The present invention relates to a kind of phosphor for white light LED and manufacture method thereof and made electric light source.
Background technology
At present, LED substitutes existing lighting system to Creating High Efficiency, low-cost solid state light emitter and has meaning of crucial importance, be characterized in having little electric current, at room temperature can obtain enough intensity, luminescence response is fast, stable performance, life-span is long, and volume is little, and is durable in use, therefore advantages such as shock resistance are widely used in fields such as general lighting, pilot lamp, signal lamps
At present, LED realizes that the method for white light mainly is that coating efficiently can be by blue-light excited yellow fluorescent powder on blue-light LED chip, and blue light and yellow light mix form white light; Or coating is by blue-light excited and fluorescent material transmitting green light and ruddiness on blue-light LED chip, and ruddiness, blue light, green glow mix and form white light; Or on purple light or ultraviolet LED chip, apply efficiently three primary colors fluorescent powder and make white light LEDs.
United States Patent (USP) 6255670 has been reported Ba 2(Mg, Zn) Si 2O 7: Eu fluorescent material and preparation method thereof, and Mg, the Zn ratio is to the influence of quantum yield and synthesis temperature.This fluorescent material is the green emitting phosphor with ultraviolet excitation, and chemical property is stable, but luminous intensity awaits further to improve.
A kind of Chlorosilicate phosphor powder with ultraviolet excitation of United States Patent (USP) 6294800 reports, its structural formula is Ca 8Mg (SiO 4) 4Cl 2: Eu, Mn is a kind of green LED fluorescent material.This fluorescent material chemical stability is good, and the emission main peak is about 540nm, but its luminous intensity still can not satisfy requirement of actual application.
Therefore, chemical stability is good, and the LED fluorescent material of good luminous performance is demanded urgently studying.
The present invention improves luminous intensity by add activator and sensitizing agent in halogen silicate, obtained a kind of excellent performance, can widespread use phosphor for white light LED.Ca with United States Patent (USP) 6294800 reports 8Mg (SiO 4) 4Cl 2: Eu, Mn fluorescent material is compared, and it locates not have emission peak about 540nm, its height of strength ratio.
Summary of the invention
The purpose of this invention is to provide that a kind of chemical property is stable, the phosphor for white light LED of good luminous performance.
Another object of the present invention provides a kind of method of making this fluorescent material, this fluorescent material manufacture method is simple, easy handling, pollution-free, cost is low.
A further object of the present invention provides a kind of by the made electric light source of this phosphor for white light LED.
For achieving the above object, the present invention takes following technical scheme:
The structural formula of a kind of phosphor for white light LED of the present invention is: A xM (SiO 4) 4X 2: Eu yR zWherein, A is Ca, and Sr is at least a among the Ba; M is Mg, Zn, and Ti, at least a among the Cd; X is F, Cl, and Br, at least a among the I; R is Dy, Pr, at least a 7＜x＜12 among the Tb; 0.001＜y＜0.5; 0＜z＜0.5.
The method of making described a kind of phosphor for white light LED comprises the steps:
(1), with Ca, Sr, Ba, Mg, Zn, Ti, Cd, Si, F, Cl, Br, I, Eu, Dy, Pr, the simple substance of Tb, oxide compound or corresponding salt are raw material, and form and stoichiometry takes by weighing described raw material by the structural formula of above-mentioned materials;
(2), in above-mentioned raw materials, add a certain amount of reaction flux, and with raw material and the abundant mixing of reaction flux;
(3), the said mixture material is carried out reducing roasting;
(4), again through last handling process, promptly make a kind of phosphor for white light LED.
In described step (2), with MX 2(M is Ca, Sr, and Ba, at least a among the Mg, X is F, Cl, Br, at least a among the I) be reaction flux.
In described step (2), the consumption of solubility promoter is 10%～300% of a synthetic materials mole number.
In described step (3), the reducing roasting number of times can be once also can be repeatedly.
In described step (3), the reducing roasting temperature is 900～1500 ℃.
In described step (3), 0.5～15 hour single reducing roasting time.
In described step (4), last handling process is a conventional process, is about to the secondary reduction product of roasting and washes 3～5 times, filters the process of oven dry.
In described step (4), bake out temperature is 90～160 ℃.
The fluorescent material of gained of the present invention can be used for making white light LEDs.This phosphor for white light LED can both well be used on following two kinds of methods.That is, coating is by blue-light excited and fluorescent material transmitting green light and ruddiness on blue-light LED chip, and ruddiness, blue light, green glow mix and form white light; Or on purple light or ultraviolet LED chip, apply efficiently three primary colors fluorescent powder and make white light LEDs.Therefore, adopt a kind of phosphor for white light LED of the present invention can make the electric light source of following white light LEDs.
A kind of electric light source contains UV-light or purple light or blue-light LED chip and phosphor for white light LED A of the present invention xM (SiO 4) 4X 2: Eu yR z
Wherein: A is Ca, and Sr is at least a among the Ba;
M is Mg, Zn, and Ti, at least a among the Cd;
X is F, Cl, and Br, at least a among the I;
R is Dy, and Pr is at least a among the Tb;
7＜x＜12；0.001＜y＜0.5；0＜z＜0.5。
Characteristics of the present invention are:
1, Fa Ming matrix of materials is highly stable, and it is through bubble, and the intensity of processing fluorescent material such as heat does not change substantially.2, the non-constant width of the excitation spectrum of material of the present invention, all very good from the stimulation effect of 300nm-460nm scope.(see figure 1) 3, simple, the easy handling of this fluorescent material manufacture method.
The structural formula of reporting with United States Patent (USP) 6294800 is Ca 8Mg (SiO 4) 4Cl 2: Eu, Mn fluorescent material is compared, and the present invention has following characteristics:
1, fluorescent material A of the present invention xM (SiO 4) 4X 2: Eu y, R zIn, A is Ca, and Sr is at least a among the Ba, and M is Mg, Zn, Ti, at least a among the Cd, X is F, Cl, Br, at least a among the I, except that containing Eu, also contain Dy in the coactivator, Ce, Pr, at least a among the Tb, but do not contain Mn;
2, the fluorescent material of gained of the present invention has only an emission peak at 450nm to 530nm place, and at the no emission peak in 540nm place;
3, the light-emitting phosphor intensity of gained of the present invention is higher.
Description of drawings
Fig. 1 is Ca 8Mg 0.6Zn 0.4(SiO 4) 4Cl 2: Eu 0.1, Dy 0.05The exciting light spectrogram
Fig. 2 is Ca 8Mg 0.6Zn 0.4(SiO 4) 4Cl 2: Eu 0.1, Dy 0.05Emmission spectrum figure
Embodiment
Embodiment 1. takes by weighing CaCO 38.426g, MgO 0.291g, ZnO 0.391g, SiO 22.893g, CaCl 22.672g, Eu 2O 3.2118g, Dy 2O 30.1122g, CaCl wherein 2Excessive 100% as fusing assistant, and above raw material is analytical pure, with above raw material mix grinding evenly after, roasting is 2 hours under 1100 ℃ of reductive conditions, with product of roasting washing 3 times, filters, and dries under 120 ℃ of conditions, promptly gets molecule and consists of Ca 8Mg 0.6Zn 0.4(SiO 4) 4Cl 2: Eu 0.1Dy 0.05Sample, its excitation spectrum is seen Fig. 1, the monitoring wavelength: 505nm.Find out from Fig. 1, this excitation spectrum excitation peak broad, all very good from the stimulation effect of 300nm-460nm scope, suitable with the YAG light-emitting phosphor intensity that excites of same wavelength when 460nm excites, it can be used for UV-light, purple light or blue-light LED chip and excites, and has purposes widely.Its emmission spectrum is seen Fig. 2, excitation wavelength: 400nm, and as can be seen, its emissive porwer is higher from Fig. 2, and the emission main peak is at 505nm, at the no emission peak in 540nm place.And its intensity is apparently higher than comparative example.Its luminous intensity sees Table 1.
Embodiment 2:CaCO 38.565g, MgO 0.493g, SiO 22.942g, CaCl 22.716g, Eu 2O 30.2153g, Dy 2O 30.0684g its manufacture method is identical with embodiment 1.Obtaining molecular formula is: Ca 8Mg (SiO 4) 4Cl 2: Eu 0.1Dy 0.03. its luminous intensity sees Table 1, and its intensity is also apparently higher than comparative example.
Embodiment 3: take by weighing SrCO 39.402g, MgO 0.367g, SiO 22.187g, SrCl 22.884g, Eu 2O 30.1601g its manufacture method is identical with embodiment 1.Obtaining molecular formula is: Sr 8Mg (SiO 4) 4Cl 2: Eu 0.1, its luminous intensity sees Table 1, and its intensity is also apparently higher than comparative example.
Embodiment 4-embodiment 58
Except that forming by the molecular formula of each embodiment in the table 1 and stoichiometry takes by weighing the raw material, remaining manufacturing step is all identical with embodiment 1, obtains molecular composition and luminous intensity sees Table 1, and its intensity is all apparently higher than comparative example.
Comparative example: take by weighing CaCO 38.564g, MgO 0.493g, SiO 22.941g CaCl 22.716g, Eu 2O 30.215g, MnCO 30.0703g its manufacture method is identical with embodiment 1, obtaining molecular composition is Ca 8Mg (SiO 4) 4Cl 2: Eu 0.iMn 0.05Sample.Its luminous intensity sees Table 1, and its intensity is starkly lower than each embodiment.
The molecular formula of table 1 embodiment 1-58 and comparative example and luminous intensity thereof
Embodiment Molecular formula Relative intensity (%)
460nm excites 400nm excites
1 Ca 8Mg 0.6Zn 0.4(SiO 4) 4Cl 2:Eu 0.1Dy 0.05 125 141
2 Ca 8Mg(SiO 4) 4Cl 2:Eu 0.1Dy 0.03 123 140
3 Sr 8Mg(SiO 4) 4Cl 2:Eu 0.1 102 115
4 Sr 8Mg(SiO 4) 4Cl 2:Eu 0.07 103 117
5 Ca 8Mg 0.8Zn 0.2(SiO 4) 4Cl 2:Eu 0.1 107 120
6 Ca 8Mg 0.6Zn 0.4(SiO 4) 4Cl 2:Eu 0.1 106 119
7 Ca 8Mg 0.4Zn 0.6(SiO 4) 4Cl 2:Eu 0.1 109 122
8 Ca 8Mg(SiO 4) 4Cl 2:Eu 0.05Ce 0.03 125 140
9 Ca 8Mg(SiO 4) 4Cl 2:Eu 0.07Ce 0.03 110 125
10 Ca 8Mg(SiO 4) 4Cl 2:Eu 0.1Ce 0.03 108 122
11 Ca 8Mg(SiO 4) 4Cl 2:Eu 0.1Dy 0.1 128 144
12 Ca 8Mg(SiO 4) 4Cl 2:Eu 0.05Dy 0.03 125 141
13 Ca 8Zn(SiO 4) 4Cl 2:Eu 0.1Dy 0.03 127 143
14 Ca 8Mg(SiO 4) 4Cl 2:Eu 0.1，Ce 0.03，Tb 0.001 102 114
15 Ca 8Mg(SiO 4) 4Cl 2:Eu 0.1，Pr 0.02 105 117
16 Ca 8Zn(SiO 4) 4Cl 2:Eu 0.08，Pr 0.005 103 116
17 Ca 8Zn(SiO 4) 4Cl 2:Eu 0.05，Ce 0.08，Tb 0.05 107 120
18 Sr 8Zn(SiO 4) 4Cl 2:Eu 0.1 115 130
19 Sr 8Zn(SiO 4) 4Cl 2:Eu 0.1，Dy 0.03 125 141
20 Sr 8Zn(SiO 4) 4Cl 2:Eu 0.1，Ce 0.05 120 134
21 Sr 8Mg(SiO 4) 4Cl 2:Eu 0.1 110 122
22 Sr 8Mg(SiO 4) 4Cl 2:Eu 0.1，Dy 0.03 120 135
23 Sr 8Mg(SiO 4) 4Cl 2:Eu 0.1，Ce 0.05 112 126
24 Sr 8Mg 0.6Zn 0.4(SiO 4) 4Cl 2:Eu 0.1，Dy 0.03 123 137
25 Ca 8Mg(SiO 4) 4Cl 2:Eu 0.1，Pr 0.005 109 124
26 Ca 8Mg(SiO 4) 4Cl 2:Eu 0.05，Ce 0.05，Tb 0.03 102 117
27 Sr 8Mg 0.5Zn 0.5(SiO 4) 4Cl 2:Eu 0.5，Dy 0.03 108 122
28 Sr 8Mg 0.3Zn 0.7(SiO 4) 4Cl 2:Eu 0.1，Dy 0.03 123 140
29 Ca 8Cd(SiO 4) 4Cl 2:Eu 0.1 103 117
30 Ca 8Cd(SiO 4) 4Cl 2:Eu 0.1Dy 0.03 112 126
31 Sr 8Cd(SiO 4) 4Cl 2:Eu 0.1 101 115
32 Ca 8Cd(SiO 4) 4Cl 2:Eu 0.04，Ce 0.2，Tb 0.1 113 129
33 Ca 8Cd(SiO 4) 4Cl 2:Eu 0.3，Pr 0.05 112 127
34 Sr 8Cd(SiO 4) 4Cl 2:Eu 0.1 126 141
35 Sr 8Cd(SiO 4) 4Cl 2:Eu 0.1，Dy 0.05 114 128
36 Sr 8Cd(SiO 4) 4Cl 2:Eu 0.1，Ce 0.2 117 133
37 Ca 8Ti(SiO 4) 4Cl 2:Eu 0.1 118 133
38 Ca 8Ti(SiO 4) 4Cl 2:Eu 0.1Dy 0.03 119 135
39 Sr 8Ti(SiO 4) 4Cl 2:Eu 0.1 110 126
40 Ca 8Ti(SiO 4) 4Cl 2:Eu 0.05，Ce 0.3，Tb 0.15 116 132
41 Ca 8Ti(SiO 4) 4Cl 2:Eu 0.2，Pr 0.02 106 120
42 Ca 8Ti(SiO 4) 4Cl 2:Eu 0.03，Ce 0.3， 114 128
43 Sr 8Ti(SiO 4) 4Cl 2:Eu 0.1 119 135
44 Sr 8Ti(SiO 4) 4Cl 2:Eu 0.1，Dy 0.05 124 138
45 Sr 8Ti(SiO 4) 4Cl 2:Eu 0.1，Ce 0.08 106 119
46 Ba 8Mg(SiO 4) 4Cl 2:Eu 0.1 124 137
47 Ba 8Mg(SiO 4) 4Cl 2:Eu 0.1，Dy 0.06 109 124
48 Ba 8Mg 0.8Zn 0.2(SiO 4) 4Cl 2:Eu 0.1 115 129
49 Ba 8Mg 0.8Zn 0.2(SiO 4) 4Cl 2:Eu 0.1，Dy 0.06 104 118
50 Ba 8Mg(SiO 4) 4Cl 2:Eu 0.1，Ce 0.02 116 129
51 Ca 8Mg(SiO 4) 4F 2:Eu 0.05Dy 0.03 112 124
52 Ca 8Zn(SiO 4) 4Br 2:Eu 0.05Dy 0.03 108 121
53 Ca 5Sr 3Mg(SiO 4) 4I 2:Eu 0.05Dy 0.03 106 116
54 Ca 2Sr 6Zn(SiO 4) 4Cl 2:Eu 0.1Dy 0.03 125 140
55 Ca 2Sr 6Zn 0.5Mg 0.5(SiO 4) 4Cl 2:Eu 0.1，Ce 0.2 126 140
56 Sr 8Zn 0.5Mg 0.5(SiO 4) 4Cl 2:Eu 0.1，Ce 0.05 115 129
57 Ca 4Sr 4Mg(SiO 4) 4Cl 2:Eu 0.05，Ce 0.05，Tb 0.03 105 119
58 Ca 4Sr 4Mg(SiO 4) 4Cl 2:Eu 0.07，Pr 0.002 106 121
Comparative example Ca 8Mg(SiO 4) 4Cl 2:Eu 0.1Mn 0.05 100 110
As seen from Table 1, from embodiment 1-embodiment 58, the intensity of these fluorescent material is all very high, all is higher than comparative example.
In sum, fluorescent material of the present invention has characteristics such as chemical stability is good, luminous intensity is high, the non-constant width of excitation wavelength, and manufacture method is simple, pollution-free, cost is low.

Claims (8)

1, a kind of phosphor for white light LED is characterized in that: the structural formula of this material is: A xM (SiO 4) 4X 2: Eu yR z
Wherein: A is Ca, and Sr is at least a among the Ba;
M is Mg, Zn, and Ti, at least a among the Cd;
X is F, Cl, and Br, at least a among the I;
R is Dy, and Pr is at least a among the Tb;
7＜x＜12；0.001＜y＜0.5；0＜z＜0.5。
2, a kind of method of making the described a kind of phosphor for white light LED of claim 1, it is characterized in that: this method comprises the steps
(1), with Ca, Sr, Ba, Mg, Zn, Ti, Cd, Si, F, Cl, Br, I, Eu, Dy, Pr, the simple substance of Tb, oxide compound or corresponding salt are raw material, and form and stoichiometry takes by weighing described raw material by the structural formula of above-mentioned materials;
(2), in above-mentioned raw materials, add a certain amount of reaction flux, and with raw material and the abundant mixing of reaction flux;
(3), the said mixture material is carried out reducing roasting;
(4), again through last handling process, promptly make a kind of phosphor for white light LED.
3, the method for a kind of phosphor for white light LED of manufacturing according to claim 2 is characterized in that: in described step (2), with MX 2Be reaction flux, wherein, M is Ca, Sr, and Ba, at least a among the Mg, X is F, Cl, Br, at least a among the I.
4, according to the method for claim 2 or 3 described a kind of phosphor for white light LED of manufacturing, it is characterized in that: in described step (2), the consumption of fusing assistant is 10%～300% of a synthetic materials mole number.
5, according to the method for claim 2 or a kind of phosphor for white light LED of 3 described manufacturings, it is characterized in that: in described step (3), the reducing roasting number of times can be once, or repeatedly.
6, according to the method for claim 2 or a kind of phosphor for white light LED of 3 described manufacturings, it is characterized in that: in described step (3), the reducing roasting temperature is 900～1500 ℃.
7, according to the method for claim 2 or a kind of phosphor for white light LED of 3 described manufacturings, it is characterized in that: in described step (3), the single reducing roasting time is 0.5～15 hour.
8, a kind of electric light source is characterized in that: contain the described phosphor for white light LED A of UV-light or purple light or blue-light LED chip and claim 1 xM (SiO 4) 4X 2: Eu yR z
Wherein: A is Ca, and Sr is at least a among the Ba;
M is Mg, Zn, and Ti, at least a among the Cd;
X is F, Cl, and Br, at least a among the I;
R is Dy, and Pr is at least a among the Tb;
7＜x＜12；0.001＜y＜0.5；0＜z＜0.5。
CNB031373356A 2003-06-18 2003-06-18 Luminscent-powder in use for LED of white light, preparing method and electric light source produced Expired - Fee Related CN1260321C (en)

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CN101565620B (en) * 2009-06-05 2012-04-11 中国科学院长春光学精密机械与物理研究所 Single-phase white-emitting phosphor based on near ultraviolet excitation and preparation method thereof
CN102492418A (en) * 2011-12-12 2012-06-13 苏州大学 Green emitting phosphor applicable to near ultraviolet light excitation and preparation method thereof
CN103289685A (en) * 2013-06-27 2013-09-11 苏州大学 Eu<2+> activated fluosilicate blue fluorescent powder, and preparation method and application thereof

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