CN1161447C - Prepn of color up converting material - Google Patents
Prepn of color up converting material Download PDFInfo
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- CN1161447C CN1161447C CNB011389206A CN01138920A CN1161447C CN 1161447 C CN1161447 C CN 1161447C CN B011389206 A CNB011389206 A CN B011389206A CN 01138920 A CN01138920 A CN 01138920A CN 1161447 C CN1161447 C CN 1161447C
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Abstract
The present invention relates to a preparation method of color up-conversion materials, which belongs to a synthetic method of luminescent materials in luminescence physics. The material comprises the following components: 55 to 90 mol% of at least one of compounds containing yttrium, gadolinium or lanthanum, 18 to 40 mol% of a compound containing yttrium, 2 to 4 mol% of at least one of compounds containing erbium, thulium, holmium, dysprosium, cerium or praseodymium, and 1 to 2 mol% of at least one of compounds containing sodium, potassium, lithium, beryllium, barium, aluminum, calcium, zirconium, boron, magnesium or zinc. The components are weighed according to the mol percentage and are uniformly ground, and the temperature of the components is kept at 500 to 1100 DEG C for 2 to 8 hours in order to prepare a sintered body which can be in a glass state, a ceramic state and a microcrystal particle state. Subsequently, the sintered body is ground into powder whose granularity is 100 to 400 meshes. The present invention has the characteristics of simple technology, low cost of chemical synthesis and higher luminous efficiency of the materials, and is suitable for industrial production on a large scale.
Description
Technical field
The invention belongs to the synthetic method of luminescent material in the shiner Neo-Confucianism.
Background technology
Color up converting material can convert various invisible infrared band light beams to visible light, as is used for: the infrared light detection of classes of semiconductors laser apparatus, infrarede emitting diode emission light is followed the tracks of, the check and correction of large-scale laser light beams such as YAG.Be used for infrared anti-false and can print and be applied in paper, plastics, fibre product surface, be mainly used in the false proof of commodity, trade mark security etc., as long as its identification is by infrared remote controller or semiconductor laser.Have characteristics such as simple in structure, response sensitivity, long service life, safety performance are good, applied range.This series products can effectively be realized surveying, follows the tracks of, discerns, proofread infrared beam, is applicable to fields such as scientific research, medical treatment, opticfiber communication, industrial processes, military and national defense.
The existing at present method for preparing up-conversion is to adopt dry method or wet method to make mostly, and scale operation has only green colour conversion material to realize at present, and such complicated process of preparation is difficult for stablizing, and costs an arm and a leg.Among patent documentation CN1183552, CN1185475, US5525380, the US5541012 aforesaid method is reported to some extent.
Summary of the invention
The invention provides a kind of preparation of color up converting material, use this method can realize redness, blueness, green emitting.The technical scheme that the present invention takes is:
(a) it is as follows that this material feedstock is formed weight part:
Y
2O
3Or La
2O
35～14 parts
Yb
2O
31.6～15 parts
Er
2O
3Or Tm
2O
30.04～2 parts
NaF or magnesium MgF
20～10 part
(b) said components is weighed, ground and mixed is even, 500～1100 ℃ of constant temperature 2～4 hours, makes sintered compact, is ground into granularity again and is 400 purpose powder.
In preparation method of the present invention, in oxide compound, add hydrofluoric acid, make fluorochemical, capable again sintering; When synthetic in a vacuum or contain sintering under the protection of oxygen atmosphere, fluorine gas atmosphere, chlorine atmosphere, sulphur atmosphere.
The preparation method of a kind of color up converting material of the present invention:
(a) it is as follows that this material feedstock is formed weight part:
14 parts of YF
23 parts of GdF
YbF
33 parts
DyF
30.5 part
2.8 parts of NaF
(b) said components is ground evenly, sintering under the sulphur atmosphere protection, 1100 ℃ of constant temperature 4 hours is made sintered compact, and being ground into granularity again is that 400 order powder get final product.
It is simple that the present invention has technology, and chemosynthesis is with low cost, and material luminous efficiency is higher, is fit to the commercial scale production characteristics.Such material can be by the 0.8-1.6 micron invisible infrared ray excited, send red, blue, green visible light, its granularity is 10-50um or block, above-mentioned infrared lumious material uses power 10mW can rise bright, its luminous intensity becomes certain direct ratio to increase relation with infrared device power, device products base material with its production can be: cardboard, plastics, glass, pottery, iron plate, and can customized as requested different shape, the product of area, color, pattern, property.
Embodiment
Embodiment one:
Weighing Y
2O
39g,
Yb
2O
3?3.8g，
Er
2O
3?2g，
Add hydrofluoric acid 20ml, the fluorochemical precipitation that makes is added NaF 5g, grind mixing together, during sintering, 630 ℃ of constant temperature 4 hours is made sintered compact, being ground into granularity again is that 400 order powder get final product, and this material excites at infrared wavelength 970nm and promptly sends green visible light down.
Embodiment two
Weighing YF14g, GdF 23
YbF
3?3g
DyF
3?0.5g，
NaF 2.8g
Grind mixing together, sintering under the sulphur atmosphere protection, 1100 ℃ of constant temperature 4 hours is made sintered compact, and being ground into granularity again is that 400 order powder get final product, and this material excites at infrared wavelength 970nm and promptly sends green visible light down.
Embodiment three:
Weighing La
2O
35g,
Yb
2O
3?1.6g
Er
2O
3?0.2g
MgF
2 10g
Grind mixing together, during sintering, under the sulphur atmosphere protection, 1020 ℃ of constant temperature 2 hours is made sintered compact, and being ground into granularity again is that 400 order powder get final product, and this material excites at infrared wavelength 970nm and promptly sends red visible light down.
Embodiment four:
Y
2O
3 14g
Yb
2O
3?15g
Tm
2O
3?0.04g
Add hydrofluoric acid 20m1, with the fluorochemical precipitation that makes, grind mixing, during sintering, 650 ℃ of constant temperature 4 hours is made sintered compact, and being ground into granularity again is that 400 order powder get final product, and this material excites the visible light that promptly sends blueness down at infrared wavelength 970nm.
Claims (4)
1, a kind of preparation of color up converting material is characterized in that:
(a) it is as follows that this material feedstock is formed weight part:
Y
2O
3Or La
2O
35～14 parts
Yb
2O
31.6～15 parts
Er
2O
3Or Tm
2O
30.04～2 parts
NaF or magnesium MgF
20～10 part
(b) said components is weighed, ground and mixed is even, 500～1100 ℃ of constant temperature 2～4 hours, makes sintered compact, is ground into granularity again and is 400 purpose powder.
2, preparation of color up converting material according to claim 1 is characterized in that: add hydrofluoric acid in oxide compound, make fluorochemical, capable again sintering.
3, preparation of color up converting material according to claim 1 is characterized in that: when synthetic in a vacuum or contain sintering under the protection of oxygen atmosphere, fluorine gas atmosphere, chlorine atmosphere, sulphur atmosphere.
4, a kind of preparation of color up converting material is characterized in that:
(a) it is as follows that this material feedstock is formed weight part:
14 parts of YF
23 parts of GdF
YbF
33 parts
DyF
30.5 part
2.8 parts of NaF
(b) said components is ground evenly, sintering under the sulphur atmosphere protection, 1100 ℃ of constant temperature 4 hours is made sintered compact, and being ground into granularity again is that 400 order powder get final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011389206A CN1161447C (en) | 2001-12-23 | 2001-12-23 | Prepn of color up converting material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011389206A CN1161447C (en) | 2001-12-23 | 2001-12-23 | Prepn of color up converting material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1357599A CN1357599A (en) | 2002-07-10 |
| CN1161447C true CN1161447C (en) | 2004-08-11 |
Family
ID=4674872
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011389206A Expired - Fee Related CN1161447C (en) | 2001-12-23 | 2001-12-23 | Prepn of color up converting material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1161447C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1157462C (en) * | 2002-04-15 | 2004-07-14 | 清华大学 | Nano-class conversion fluorescence material on fluoride matrix and its preparing process |
| CN103059853B (en) * | 2011-10-19 | 2014-11-05 | 海洋王照明科技股份有限公司 | Titanate phosphors for up-conversion luminescence, and preparation method and application thereof |
| CN103235347B (en) * | 2013-04-23 | 2016-07-13 | 上海洞舟实业有限公司 | A kind of preparation of multiband detection of infrared laser device |
-
2001
- 2001-12-23 CN CNB011389206A patent/CN1161447C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1357599A (en) | 2002-07-10 |
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|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| ASS | Succession or assignment of patent right |
Owner name: SHANGHAI KE RUN PHOTOELECTRIC MATERIALS CO., LTD. Free format text: FORMER OWNER: ZHENG YAN Effective date: 20021121 Owner name: ZHENG YAN Free format text: FORMER OWNER: CHANGCHUN KERUI PHOTOELECTRONIC MATERIAL TECHNOLOGY CO.,LTD. |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20021121 Address after: 130021 No. 1, Yanan Road, Changchun, Jilin Address after: Shanghai city Minhang District Donglan road 201102 No. 208 Applicant after: Zheng Yan Co-applicant after: Shanghai Kerune Phosphor Technology Co., Ltd. Address before: 130021 No. 1, Yanan Road, Changchun, Jilin Applicant before: Changchun Kerun Photoelectronic Material Science &. Technology Co., Ltd. Co-applicant before: Zheng Yan |
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| ASS | Succession or assignment of patent right |
Owner name: NONE Free format text: FORMER OWNER: SHANGHAI KE RUN PHOTOELECTRIC MATERIALS CO., LTD. Effective date: 20040115 |
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| C41 | Transfer of patent application or patent right or utility model | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20040115 Address after: No. 1, Yanan Road, Changchun, Jilin Applicant after: Zheng Yan Address before: No. 1, Yanan Road, Changchun, Jilin Applicant before: Zheng Yan Co-applicant before: Shanghai Kerune Phosphor Technology Co., Ltd. |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20040811 Termination date: 20101223 |