CN101013050A - Infrared laser detection card and method for making same - Google Patents
Infrared laser detection card and method for making same Download PDFInfo
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- CN101013050A CN101013050A CN 200710056669 CN200710056669A CN101013050A CN 101013050 A CN101013050 A CN 101013050A CN 200710056669 CN200710056669 CN 200710056669 CN 200710056669 A CN200710056669 A CN 200710056669A CN 101013050 A CN101013050 A CN 101013050A
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- rare earth
- infrared laser
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- nano microcrystalline
- detection card
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Abstract
The invention discloses an infrared laser detection card and its preparation method. The infrared laser detection card comprises the bottom substrate and the nanocrystalline powder coated in the bottom substrate and mixed with the rare earth ion, and using PVC plastic molding; the chemical composition of the said nanocrystalline powder is Si2O.Al2O3.PbF2.CdF2:Re3+, in which Re3+ is one or more combinations of the rare earth ion Yb, Er, Pr, Ho, Eu or Tm. The nanocrystal is that the rare-earth ions exists in the fluoride nanocrystal of glass ceramic, the nanocrystal size for the 10-90nm. The invention uses the rare earth nanocrystalline powder for the infrared laser detection card of luminous preparation, and when infrared laser irradiating, the rare earth ion-doped nanocrystalline powder takes luminous effect to convert the unseen infrared laser into visible light, and it can detect the infrared laser location and intensity with the 0.8-2.2 micron wavelength.
Description
[technical field]
The present invention relates to the infrared laser detection range, particularly a kind of rare earth nano crystallite powder is made photoluminescence infrared laser detection card of luminescent layer preparation and preparation method thereof.
[background technology]
The infrared laser wavelength is positioned at the not visible scope of human eye, brings the difficulty that detects and regulate in the use.Existing infrared laser detection technique has two kinds, and one is to use the InGaAs infrared eye that links to each other with electronic equipment, can accurately measure infrared laser position and intensity, and its weakness is complex structure and cost height; Another kind is infrared sensing card or detecting card, the infrared sensing card that organic material is made is highly sensitive but easily saturated phenomenon is serious, can not display light spot size and pattern, and there are the problems such as infrared laser wavelength coverage finite sum up-conversion luminescence efficient is low that detect in existing inorganic infrared laser detecting card.
Rare earth ion has abundant energy level, and rare earth compound is potential up-conversion luminescent material, and the phonon energy of host material is the principal element of decision rare earth ion up-conversion luminescence, and the up-conversion luminescence efficient of the more little rare earth ion of phonon energy is high more.The phonon energy of sulfide that uses and aluminate material is bigger at present, and therefore rare earth luminous efficient is lower; And the poor chemical stability of the halogenide of low phonon energy and oxyhalide should not be promoted.The rare earth ion doped oxyfluoride glass ceramic material of the early 1990s birth has overcome the shortcoming of above-mentioned many compounds, be that the high host material of present good stability and up-conversion luminescence efficient is (referring to Y.Wang and J.Ohwaki, Appl.Phys.Lett.63,3268 (1993)), it is reported; the glass ceramic material that erbium Yb mixes altogether can make the infrared laser of 808nm, 980nm and 1500nm be converted to visible light, is the potential inorganic material that is applied to optical waveguide, short wavelength's solid state laser and optical communication field.
[summary of the invention]
The objective of the invention is to detect the little and inefficient technical matters of up-conversion luminescence of wavelength coverage in order to solve existing test card, and provide a kind of infrared laser detection card and preparation method thereof, this infrared laser detection card is made up-conversion with rare earth nano crystallite powder, can detect position and the intensity of wavelength at the infrared laser of 0.8-2.2 micron.
The present invention discloses a kind of infrared laser detection card for addressing the above problem, and it is characterized in that by the bottom substrate and be sprayed on the rare-earth-ion-doped nano microcrystalline powder constituent of bottom substrate one or both sides, and with the moulding of PVC plastic packaging; The chemical composition of said nano microcrystalline powder is Si
2OAl
2O
3PbF
2CdF
2: Re
3+, Re wherein
3+Be one or more the combination among rare earth ion Yb, Er, Pr, Ho, Eu or the Tm; Nano microcrystalline is meant that rare earth ion is present in the fluoride nano crystallite of glass ceramics, and nano microcrystalline is of a size of 10-90nm; Each component and mole percent level thereof are as follows:
Si
2O 20-40mol％；
Al
2O
3 10-40mol％；
PbF
2 1-49mol％；
CdF
2 1-49mol％；
Re
3+ 0.01-3mol％。
The invention also discloses the preparation method of this infrared laser detection card, it is characterized in that comprising following processing step:
(1) preparation precursor glass: get following component by mole number percent:
Si
2O 20-40mol％；
Al
2O
3 10-40mol％；
PbF
2 1-49mol％；
CdF
2 1-49mol％；
Re
3+ 0.01-3mol％；
Put into the agate mortar mixed grinding, the platinum crucible of packing into then; At 900-1200 ℃ of following calcination 1-3 hour, at high temperature the glass metal of fusion is poured over rapidly again and carries out chilling on the mould, obtain transparent oxyfluoride presoma glass material;
(2) preparation glass ceramics: with presoma glass material under nucleation temperature thermal treatment 1-36 hour, be cooled to room temperature with furnace temperature then, obtain the rare earth ion doped nano microcrystalline oxyfluoride glass ceramic that contains;
(3) preparation rare earth nano microcrystalline powder:, obtain rare earth nano crystallite powder with the rare earth ion doped nano microcrystalline oxyfluoride glass ceramic pulverize that contains;
(4) the rare earth nano microcrystalline powder is adopted spraying method, be sprayed on the substrate that has the coordinate sign, finish with PVC plastic packaging machine plastic packaging then.
The present invention adopts the rare earth nano microcrystalline powder to make the infrared laser detection card of luminescent layer preparation, when infrared laser shines, the up-conversion luminescence effect of rare earth ion doped nano microcrystalline powder can make sightless infrared laser convert visible light to, and the back of the body end is the infrared laser detection card of coordinate paper, when detecting, can measure the size and the position of infrared laser hot spot, and by detecting the power that spot intensity comes detection laser.Its advantage is:
The first, by using rare earth nano crystallite powder that the up-conversion luminescence efficient of rare earth ion is improved, strengthened the detectability of infrared laser detecting card; The use of multiple rare earth ion enlarges the wavelength coverage to infrared light detection, improves service efficiency;
The second, the use at the coordinate back of the body end can make test card directly measure infrared laser pattern and spot size in the test card;
[embodiment]
Infrared laser detection card of the present invention comprises following structure: bottom substrate that (1) single or double has a coordinate is as cardboard, and length and width are any, and thickness is between 0.5-2.0mm; (2) on the surface of the cardboard that has coordinate, scribble transparent epoxy resin glue, the rare earth nano microcrystalline powder of the about 1.0-5.0 micron of coating thickness on it; (3) select the transparent PVC material will scribble the cardboard plastic packaging moulding of nano microcrystalline powder with plastic packaging machine.
Aforesaid infrared laser detection card, rare earth nano crystallite powder is wherein implemented by following technological process:
(1) preparation precursor glass: choose host material Si
2O, Al
2O
3, PbF
2And CdF
2, selecting purity is the rare earth material Yb of 4N
2O
3Or Er
2O
3, Pr
6O
11, Ho
2O
3, Tm
2O
3, Tb
4O
7, Nb
2O
3In one or more combination, the volumetric molar concentration of every kind of rare earth ion is between 0.1-5mol%, the ratio of oxide and fluoride is 1: 1.The abundant mixed grinding in agate mortar with host material and rare earth compound, the platinum crucible of packing into then.At 900-1200 ℃ of following calcination 1-3 hour, under the high temperature glass metal of fusion is poured over rapidly and carries out chilling on the iron pan, obtain transparent oxyfluoride presoma glass material.
(2) preparation glass ceramics: with presoma glass material under nucleation temperature thermal treatment 1-36 hour, nucleation temperature was determined by raw-material differential thermal analysis curve between 300-550 °.Be cooled to room temperature with furnace temperature then, obtain rare earth ion doped oxyfluoride glass ceramic.It is characterized in that being embedded with rare-earth-ion-doped fluoride microcrystal in the oxide glass body, crystallite dimension is at 10-90nm.
(3) preparation rare earth nano microcrystalline powder: rare earth ion doped oxyfluoride glass ceramic crushing and pulverize are obtained the rare earth nano microcrystalline powder, and the granularity size of microcrystalline powder is at the 1-5 micron.Also the nano microcrystalline powder of doping different rare earth ions evenly can be mixed in proportion, the up-conversion luminescence wavelength is at the rare earth nano crystallite powder of visible-range when obtaining infrared laser and exciting.
At last rare earth nano microcrystalline powder material is sprayed at the substrate that has the coordinate sign, coating thickness is the 1.0-5.0 micron.Substrate scribbles transparent epoxy resin glue on its surface before spraying rare earth nano microcrystalline powder.Use the moulding of PVC plastic packaging machine plastic packaging then.
Embodiment 1
By mole component 30Si
2O15Al
2O
340PbF
210CdF
2: 1Yb
2O
34Er
2O
3Take by weighing raw material, the platinum crucible of in agate mortar, packing into behind the mixed grinding, 950 ℃ of following calcinations 2 hours, hot conditions is poured over the glass metal of fusion rapidly and carries out chilling on the mould then, obtains transparent oxyfluoride presoma glass material; With presoma glass 450 ℃ of following thermal treatments 1 hour, be cooled to room temperature with furnace temperature then, obtain the rare earth ion doped nano microcrystalline oxyfluoride glass ceramic that contains, obtain the rare earth nano microcrystalline powder after the grinding: the rare earth nano microcrystalline powder is sprayed on the substrate that has coordinate sign and transparent epoxy resin glue, microcrystalline powder thickness is 3.0 microns, finish with PVC plastic packaging machine plastic packaging then, test card is of a size of 85 * 55mm
2
Embodiment 2
By mole component 30Si
2O15Al
2O
340PbF
210CdF
2: 1Yb
2O
34Ho
2O
3Take by weighing raw material, the platinum crucible of in agate mortar, packing into behind the mixed grinding, 950 ℃ of following calcinations 2 hours, hot conditions is poured over the glass metal of fusion rapidly and carries out chilling on the mould then, obtains transparent oxyfluoride presoma glass material; With presoma glass 450 ℃ of following thermal treatments 2 hours, be cooled to room temperature with furnace temperature then, obtain the rare earth ion doped nano microcrystalline oxyfluoride glass ceramic that contains, obtain the rare earth nano microcrystalline powder after the grinding: the rare earth nano microcrystalline powder is sprayed on the substrate that has coordinate sign and transparent epoxy resin glue, microcrystalline powder thickness is 3.0 microns, finish with PVC plastic packaging machine plastic packaging then, test card is of a size of 85 * 55mm
2
Embodiment 3
By mole component 30Si
2O15Al
2O
340PbF
210CdF
2: 1Yb
2O
30.5Tm
2O
33.5Er
2O
3Take by weighing raw material, the platinum crucible of in agate mortar, packing into behind the mixed grinding, 950 ℃ of following calcinations 2 hours, hot conditions is poured over the glass metal of fusion rapidly and carries out chilling on the mould then, obtains transparent oxyfluoride presoma glass material; With presoma glass 480 ℃ of following thermal treatments 2 hours, be cooled to room temperature with furnace temperature then, obtain the rare earth ion doped nano microcrystalline oxyfluoride glass ceramic that contains, obtain the rare earth nano microcrystalline powder after the grinding: the rare earth nano microcrystalline powder is sprayed on the substrate that has coordinate sign and transparent epoxy resin glue, microcrystalline powder thickness is 3.0 microns, finish with PVC plastic packaging machine plastic packaging then, test card is of a size of 85 * 55mm
2
Embodiment 4
Prepare embodiment 1 respectively, three kinds of rare earth nano microcrystalline powders in 2 and 3, take by weighing in 1: 2: 2 ratio then, be sprayed at after fully mixing on the substrate that has coordinate sign and transparent epoxy resin glue, microcrystalline powder thickness is 3.0 microns, finish with PVC plastic packaging machine plastic packaging then, test card is of a size of 85 * 55mm
2
Claims (6)
1. infrared laser detection card is characterized in that by the bottom substrate and is sprayed on the rare-earth-ion-doped nano microcrystalline powder constituent of bottom substrate one or both sides, and with the moulding of PVC plastic packaging; The chemical composition of said nano microcrystalline powder is Si
2OAl
2O
3PbF
2CdF
2: Re
3+, Re wherein
3+Be one or more the combination among rare earth ion Yb, Er, Pr, Ho, Eu or the Tm, nano microcrystalline is of a size of 10-90nm; Each component and mole percent level thereof are as follows:
Si
2O 20-40mol％；
Al
2O
3 10-40mol％；
PbF
2 1-49mol％；
CdF
2 1-49mol％；
Re
3+ 0.01-3mol％。
2. infrared laser detection card according to claim 1 is characterized in that said bottom substrate has the coordinate sign at one or both sides, and thickness is between 0.5-2.0mm.
3. the preparation method of the described infrared detection card of claim 1 is characterized in that comprising following processing step:
(1) preparation precursor glass: get following component by mole number percent:
Si
2O 20-40mol％；
Al
2O
3 10-40mol％；
PbF
2 1-49mol％；
CdF
2 1-49mol％；
Re
3+ 0.01-3mol％；
Put into the agate mortar mixed grinding, the platinum crucible of packing into then; At 900-1200 ℃ of following calcination 1-3 hour, at high temperature the glass metal of fusion is poured over rapidly again and carries out chilling on the mould, obtain transparent oxyfluoride presoma glass material;
(2) preparation glass ceramics: with presoma glass material under nucleation temperature thermal treatment 1-36 hour, be cooled to room temperature with furnace temperature then, obtain the rare earth ion doped nano microcrystalline oxyfluoride glass ceramic that contains;
(3) preparation rare earth nano microcrystalline powder:, obtain rare earth nano crystallite powder with the rare earth ion doped nano microcrystalline oxyfluoride glass ceramic pulverize that contains;
(4) the rare earth nano microcrystalline powder is adopted spraying method, be sprayed on the substrate that has the coordinate sign, finish with PVC plastic packaging machine plastic packaging then.
4. the preparation method of infrared detection card according to claim 3, the nucleation temperature that it is characterized in that said step (2) is determined by raw-material differential thermal analysis curve between 300 °-550 °.
5. according to the preparation method of claim 3 or 4 described infrared detection cards, it is characterized in that substrate in the said step (4) before spraying rare earth nano microcrystalline powder, scribbles transparent epoxy resin glue on its surface.
6. the preparation method of infrared detection card according to claim 5, the coating thickness that it is characterized in that the nano microcrystalline powder in the said step (4) is the 1.0-5.0 micron.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710056669 CN101013050A (en) | 2007-01-31 | 2007-01-31 | Infrared laser detection card and method for making same |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710056669 CN101013050A (en) | 2007-01-31 | 2007-01-31 | Infrared laser detection card and method for making same |
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| Publication Number | Publication Date |
|---|---|
| CN101013050A true CN101013050A (en) | 2007-08-08 |
Family
ID=38700706
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|---|---|---|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101913766A (en) * | 2010-08-04 | 2010-12-15 | 宁波大学 | Rare earth ion doped oxyhalogen silicate glass and preparation method thereof |
| CN102643031A (en) * | 2011-02-18 | 2012-08-22 | 张一熙 | Glass panel solution scheme for reducing greenhouse effect |
| CN106773018A (en) * | 2015-11-23 | 2017-05-31 | 中国科学院大连化学物理研究所 | A kind of infrared aperture-variable diaphragm |
| CN107312540A (en) * | 2017-06-22 | 2017-11-03 | 哈尔滨学院 | Preparation method based on the brilliant 980 nm near infrared lights detection card of rare-earth doping fluoride nano |
| CN108165255A (en) * | 2017-12-27 | 2018-06-15 | 哈尔滨工业大学 | A kind of all solid state photochromic crystal material laser card and its preparation and application |
-
2007
- 2007-01-31 CN CN 200710056669 patent/CN101013050A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101913766A (en) * | 2010-08-04 | 2010-12-15 | 宁波大学 | Rare earth ion doped oxyhalogen silicate glass and preparation method thereof |
| CN101913766B (en) * | 2010-08-04 | 2012-05-30 | 宁波大学 | Rare earth ion doped oxyhalogen silicate glass and preparation method thereof |
| CN102643031A (en) * | 2011-02-18 | 2012-08-22 | 张一熙 | Glass panel solution scheme for reducing greenhouse effect |
| CN106773018A (en) * | 2015-11-23 | 2017-05-31 | 中国科学院大连化学物理研究所 | A kind of infrared aperture-variable diaphragm |
| CN107312540A (en) * | 2017-06-22 | 2017-11-03 | 哈尔滨学院 | Preparation method based on the brilliant 980 nm near infrared lights detection card of rare-earth doping fluoride nano |
| CN107312540B (en) * | 2017-06-22 | 2020-06-02 | 哈尔滨学院 | Preparation method of 980nm near-infrared light detection card based on rare earth doped fluoride nanocrystalline |
| CN108165255A (en) * | 2017-12-27 | 2018-06-15 | 哈尔滨工业大学 | A kind of all solid state photochromic crystal material laser card and its preparation and application |
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