CN107367498A - A kind of test device and method for LD excitated fluorescent powders in integrating sphere - Google Patents
A kind of test device and method for LD excitated fluorescent powders in integrating sphere Download PDFInfo
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- CN107367498A CN107367498A CN201710749743.2A CN201710749743A CN107367498A CN 107367498 A CN107367498 A CN 107367498A CN 201710749743 A CN201710749743 A CN 201710749743A CN 107367498 A CN107367498 A CN 107367498A
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- condensing unit
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
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Abstract
A kind of test device for LD excitated fluorescent powders in integrating sphere, including optical fiber, integrating sphere, bulb stopper, beam condensing unit, light barrier, photo-detector probe and a support;Bulb stopper is provided with through hole and slot, and through hole is located at slot top;Support includes substrate, bracket and fixture, and substrate is provided with the plate with slot Corresponding matching, and bracket is corresponding with beam condensing unit matching, and fixture is corresponding with phosphor sheet matching;Beam condensing unit is provided with through hole corresponding with bulb stopper, and beam condensing unit light extraction end is close to phosphor sheet, and beam condensing unit light extraction end margin radius is less than or equal to phosphor sheet radius;Optical fiber is fixed in beam condensing unit through through hole.The beneficial effects of the invention are as follows can reduce no beam condensing unit test error caused by the reflection and scattering of blue light, so that white light luminous flux improves 50% or so, and colour temperature can reduce 2000K 3000K, tend to actual color temperature value, reduce the interference of blue light, and simple in construction, easy to operate, testing efficiency is high.
Description
Technical field
The present invention relates to a kind of optical detection device, and in particular to a kind of test dress for LD excitated fluorescent powders in integrating sphere
Put and method.
Background technology
With the development of illuminating industry, the demand of high power light source is more and more, and LD excites as the fluorescent material of a new generation
Source, there is the series of advantages such as high brightness, low etendue, long lifespan, stable performance, led especially suitable for special lighting
Domain, thus test using LD excitated fluorescent powders the various parameters of the light beam after exciting.
One of usually used device of the test device of light is integrating sphere, and the basic functional principle of integrating sphere is, light by
Light is uniformly reflected and diffused inside this ball after input hole incidence, therefore the light obtained by delivery outlet is quite uniform
Diffusion light beam, and the incident angle of incident light, spatial distribution and polarization all will not to the beam intensity of output and uniformly
Degree is impacted, and photo-detector probe receives diffusion light beam, and test result is exported.
The test device of LD excitated fluorescent powders in the integrating sphere worked out, similar to candle light, it is wrapped fluorescent material device shape
Optical fiber, integrating sphere, bulb stopper, light barrier and photo-detector probe are included, the center of bulb stopper, light barrier and photo-detector probe is set successively
Put in the same horizontal line, in addition to fluorescent material device, fluorescent material device are fixed on bulb stopper, bulb stopper is provided with through hole, bulb stopper
Surface is provided with reflectorized material, and optical fiber is arranged in fluorescent material device through through hole.The beneficial effect of device is:It can not only complete
LD excites the test of long-distance fluorescent powder, and simple in construction, easy to operate, while good seal performance, and light loss is small.But this
Kind device, single can only be tested a certain fluorescent material, to test a variety of fluorescent material, because fluorescent material device is fixed
, it is necessary to be fixed on bulb stopper by multigroup different fluorescent material device or dismantled and install more on same bulb stopper on bulb stopper
Individual fluorescent material device, so that it is complex for operation step, and then testing efficiency is low.
In a word, the existing test device that can carry out LD excitated fluorescent powders, complex steps, testing efficiency are low.
The content of the invention
The purpose of the present invention, just it is to provide a kind of test for being used for LD excitated fluorescent powders in integrating sphere dress simple in construction
Put, can not only complete the test that LD excites long-distance fluorescent powder, and it is easy to operate, and testing efficiency is high.
The purpose of the present invention realizes that it includes optical fiber, integrating sphere, bulb stopper, optically focused dress by such technical scheme
Put, light barrier and photo-detector probe, the center of bulb stopper, light barrier and photo-detector probe is successively set on same horizontal line
On, in addition to a support;Bulb stopper is provided with through hole and slot, and through hole is located at slot top;Support includes substrate, bracket and folder
Tool, substrate one end are provided with the plate with slot Corresponding matching, and bracket is corresponding with beam condensing unit matching, and fixture matches with phosphor sheet
It is corresponding;Beam condensing unit is provided with through hole corresponding with bulb stopper, and beam condensing unit light extraction end is close to phosphor sheet, and beam condensing unit light extraction
End margin radius is not more than phosphor sheet radius;Optical fiber is fixed in beam condensing unit through through hole.
In the present invention, support is provided with structure;Bulb stopper is provided with through hole and slot, and through hole is located at slot top;On support
Provided with substrate, bracket and fixture, substrate one end is provided with the plate with slot Corresponding matching, passes through the correspondence of plate and slot
Match somebody with somebody so that support is fixed on bulb stopper;Bracket is corresponding with beam condensing unit matching, and fixture is corresponding with phosphor sheet matching, and bracket can
To ensure the stability of beam condensing unit, fixture is the fixed structure to phosphor sheet, and phosphor sheet can be according to the needs of test
Carry out quick-replaceable;Beam condensing unit light extraction end is close to phosphor sheet, and beam condensing unit light extraction end margin radius is not more than fluorescence
Powder piece radius, optical fiber are fixed in beam condensing unit through through hole, so that more light beams is got on phosphor sheet as far as possible, to obtain
Obtain most accurate test data.
By adopting the above-described technical solution, the present invention has the advantage that:It can be reduced by this device and do not gathered
Electro-optical device test error caused by the reflection and scattering of blue light so that white light luminous flux improves 50% or so, and colour temperature can reduce
2000K-3000K, tend to actual color temperature value, reduce the interference of blue light, and it is simple in construction, and easy to operate, testing efficiency is high.
Brief description of the drawings
Fig. 1 is a kind of schematic diagram that the present invention is used for the test device of LD excitated fluorescent powders in integrating sphere.
Fig. 2 is the diagrammatic cross-section at A-A in Fig. 1.
Fig. 3 is a kind of schematic diagram that the present invention is used for part-structure in the test device of LD excitated fluorescent powders in integrating sphere.
Fig. 4 is a kind of Fig. 3 exploded perspective view.
Fig. 5 is a kind of schematic diagram of bulb stopper.
Fig. 6 is the schematic diagram in a Fig. 5 face.
Fig. 7 is diagrammatic cross-section at B-B in Fig. 6.
Fig. 8 is a kind of schematic diagram of beam condensing unit.
Fig. 9 is diagrammatic cross-section at C-C in Fig. 8.
Figure 10 is a kind of schematic diagram of fixture.
Figure 11 is light beam reacting flow chart.
Figure 12 is a kind of schematic diagram of test result.
1. optical fiber;2. integrating sphere;3. bulb stopper;4. beam condensing unit;5. it is light barrier;6. photo-detector is popped one's head in;7. support;8.
Through hole;9. slot;10. substrate;11. bracket;12. fixture;13. plate;14. phosphor sheet;15. neck.
Embodiment
The present invention is further illustrated with reference to the accompanying drawings and examples.
As shown in Figures 1 to 10, a kind of test device for LD excitated fluorescent powders in integrating sphere of the present invention, including optical fiber
1st, integrating sphere 2, bulb stopper 3, beam condensing unit 4, light barrier 5 and photo-detector probe 6, bulb stopper 3, light barrier 5 and photo-detector probe 6
Center set gradually in the same horizontal line, an in addition to support 7;Bulb stopper 3 is provided with through hole 8 and slot 9, and through hole 8 is located at
The top of slot 9;Support 7 includes substrate 10, bracket 11 and fixture 12, and the one end of substrate 10 is provided with the plate with the Corresponding matching of slot 9
13, bracket 11 is corresponding with the matching of beam condensing unit 4, and fixture 12 is corresponding with the matching of phosphor sheet 14;Beam condensing unit 4 is provided with and bulb stopper 3
Corresponding through hole 8, the light extraction end of beam condensing unit 4 are close to phosphor sheet 14, and the light extraction end margin radius of beam condensing unit 4 is no more than glimmering
The radius of light powder piece 14;Optical fiber 1 is fixed in beam condensing unit 4 through through hole 8.
In the present invention, support 7 is provided with structure;Bulb stopper 3 is provided with through hole 8 and slot 9, and through hole 8 is located at the top of slot 9;
Support 7 is provided with substrate 10, bracket 11 and fixture 12, and the one end of substrate 10 is provided with the plate 13 with the Corresponding matching of slot 9, by inserting
The Corresponding matching of plate 13 and slot 9 so that support 7 is fixed on bulb stopper 3;Bracket 11 is corresponding with the matching of beam condensing unit 4, fixture 12
Corresponding with the matching of phosphor sheet 14, bracket 11 can ensure the stability of beam condensing unit 4, and fixture 12 is consolidating to phosphor sheet 14
Determine structure, phosphor sheet 14 can need progress quick-replaceable according to test;The light extraction end of beam condensing unit 4 and phosphor sheet 14 are tight
Patch, and the light extraction end margin radius of beam condensing unit 4 is not more than the radius of phosphor sheet 14, optical fiber 1 is fixed on beam condensing unit through through hole 8
In 4, so that more light beams is got on phosphor sheet 14 as far as possible, to obtain most accurate test data.
As shown in figure 8, beam condensing unit 4 is reflector or reflector.
As shown in Figures 2 to 4, bracket 11 is semicircle bracket, is fixed on the substrate 10.
As shown in Fig. 2, Fig. 3, Fig. 4 and Figure 10, fixture 12 is semicircular clamp, is fixed on the substrate 10, fixture side is provided with
Neck 15 corresponding with phosphor sheet 14.Fixture 12 mainly plays a part of holding phosphor sheet 14.
A kind of method for exciting the test device of long-distance fluorescent powder piece to test fluorescent material for LD in integrating sphere of the present invention:
Step 1, PC controls pressure-stabilizing constant flow source control LD to send light beam;
Step 2, light beam coupling is entered optical fiber by coupling device;
Step 3, optical fiber 1 through the through hole 8 on bulb stopper 3 by the beam condensing unit 4 in beam Propagation to bracket 11;
Step 4, beam condensing unit 4 gets to as far as possible more light beams on phosphor sheet 14;
Step 5, phosphor sheet 14 can be constantly reflected to increase the efficiency of conversion light between beam condensing unit 4, and emergent light shines product
Bulb separation 2, the detector probe 6 of the inside of integrating sphere 2 detect light;
Step 6, detector detection is exported the parameters such as the spectrogram of fluorescent material, luminous flux, colour temperature, colour rendering index by PC ends.
Further, the light beam that LD is sent is wavelength 450nm blue light.
Further, light beam can select different illumination or intensity according to test needs.
Further, phosphor sheet is tested device, and its thickness is needed to set with color according to test.
Further, can be with the numerical value of test voltage, electric current, power consumption, power and color accounting.
As shown in figure 11, the light for having 50%-60% when blue light gets to phosphor sheet 14 reflects back, then phosphor sheet 14
Can constantly it be reflected between beam condensing unit 4 to increase the efficiency of conversion light, emergent light shines integrating sphere 2, the spy of the inside of integrating sphere 2
Survey device probe 6 and detect light, related data is then returned into PC.
As shown in figure 12, the test device of long-distance fluorescent powder piece is excited to test fluorescence to be used for LD in integrating sphere in the present invention
A kind of test result of powder, specially LD send the data knot that 450nm blue lasers excite 565nm yellow fluorescent powder pieces to draw
Fruit.Wherein, the left side is spectrogram, and the right is output parameter:Spectrum abscissa is wavelength, unit nm;Φ is luminous flux, unit
lm;CCT is colour temperature, unit K;Ra is colour rendering index;η is light efficiency;λ d are dominant wavelength;λ p are wavelength peak-peak;Δ λ p are ripple
Long crest half-wave is wide;X, y, U ', V ' is chromaticity coordinate;Pur is excitation;U is operating voltage;I is operating current;P is power consumption;
PF is power factor;T is the time of integration;Ip is main channel peak;Red Ratio are red accounting.As seen from the figure, filled by this
No beam condensing unit 4 test error caused by the reflection and scattering of blue light can be reduced by putting so that white light luminous flux improves 50%
Left and right, and colour temperature can reduce 2000K-3000K, tend to actual color temperature value, reduce the interference of blue light.
Claims (9)
1. a kind of test device that long-distance fluorescent powder piece is excited for LD in integrating sphere, including optical fiber(1), integrating sphere(2), bulb stopper
(3), beam condensing unit(4), light barrier(5)Popped one's head in photo-detector(6), bulb stopper(3), light barrier(5)Popped one's head in photo-detector(6)
Center set gradually in the same horizontal line, it is characterised in that:Also include a support(7);Bulb stopper(3)It is provided with through hole(8)
And slot(9), through hole(8)Positioned at slot(9)Top;Support(7)It is upper to include substrate(10), bracket(11)And fixture(12), base
Bottom(10)One end is provided with and slot(9)The plate of Corresponding matching(13), bracket(11)With beam condensing unit(4)Matching is corresponding, fixture
(12)With phosphor sheet(14)Matching is corresponding;Beam condensing unit(4)It is provided with and bulb stopper(3)Corresponding through hole(8), beam condensing unit(4)
Light extraction end and phosphor sheet(14)It is close to, and beam condensing unit(4)Light extraction end margin radius is less than or equal to phosphor sheet(14)Half
Footpath;Optical fiber(1)Through through hole(8)It is fixed on beam condensing unit(4)It is interior.
2. the test device according to claim 1 that long-distance fluorescent powder piece is excited for LD in integrating sphere, it is characterised in that:
Beam condensing unit(4)For reflector or reflector.
3. the test device according to claim 1 that long-distance fluorescent powder piece is excited for LD in integrating sphere, it is characterised in that:
Bracket(11)For semicircle bracket, substrate is fixed on(10)On.
4. the test device according to claim 1 that long-distance fluorescent powder piece is excited for LD in integrating sphere, it is characterised in that:
Fixture(12)For semicircular clamp, substrate is fixed on(10)On, fixture side is provided with and phosphor sheet(14)Corresponding neck(15).
5. a kind of method for exciting the test device of long-distance fluorescent powder piece to test fluorescent material for LD in integrating sphere, its feature exist
In methods described includes:
Step 1, PC controls pressure-stabilizing constant flow source control LD to send light beam;
Step 2, light beam coupling is entered optical fiber by coupling device;
Step 3, optical fiber(1)Through bulb stopper(3)On through hole(8)By beam Propagation to bracket(11)On beam condensing unit(4)It is interior;
Step 4, beam condensing unit(4)As far as possible more light beams is got into phosphor sheet(14)On;
Step 5, phosphor sheet(14)Can be with beam condensing unit(4)Between constantly reflection to increase the efficiency of conversion light, emergent light shines
To integrating sphere(2), integrating sphere(2)The detector probe of the inside(6)Detect light;
Step 6, detector detection by the spectrogram of fluorescent material and luminous flux, colour temperature, colour rendering index, wavelength, ripple be wide, peak value,
The numerical value of channel peak, excitation and chromaticity is exported by PC ends.
A kind of 6. test device test fluorescence that long-distance fluorescent powder piece is excited for LD in integrating sphere according to claim 5
The method of powder, it is characterised in that the light beam that LD is sent is wavelength 450nm blue light.
A kind of 7. test device test fluorescence that long-distance fluorescent powder piece is excited for LD in integrating sphere according to claim 5
The method of powder, it is characterised in that light beam can select different illumination or intensity according to test needs.
A kind of 8. test device test fluorescence that long-distance fluorescent powder piece is excited for LD in integrating sphere according to claim 5
The method of powder, it is characterised in that phosphor sheet is tested device, and its thickness is needed to set with color according to test.
A kind of 9. test device test fluorescence that long-distance fluorescent powder piece is excited for LD in integrating sphere according to claim 5
The method of powder, it is characterised in that can be with the numerical value of test voltage, electric current, power consumption, power and color accounting.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110161010A (en) * | 2019-07-01 | 2019-08-23 | 河海大学常州校区 | A kind of reflective controllable temperature laser excitation remote fluorescence material testing apparatus |
Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20100277059A1 (en) * | 2009-05-01 | 2010-11-04 | Renaissance Lighting, Inc. | Light fixture using doped semiconductor nanophosphor in a gas |
CN102563539A (en) * | 2012-01-11 | 2012-07-11 | 山东浪潮华光照明有限公司 | Optical fiber type remote light distribution method realized by aid of fluorescent powder |
US20120264236A1 (en) * | 2011-04-15 | 2012-10-18 | Chang Gung University | Fluorescent powder applying device and method capable of detecting instantly color temperature of white light in a manufacturing process |
WO2012154446A1 (en) * | 2011-05-12 | 2012-11-15 | 3M Innovative Properties Company | Optical structure for remote phosphor led |
CN103308499A (en) * | 2013-05-24 | 2013-09-18 | 厦门大学 | Device and method for testing performance of blue light-emitting diode (LED) excitation fluorescent powder |
CN103557457A (en) * | 2013-10-30 | 2014-02-05 | 山东明华光电科技有限公司 | Remote excitation fluorescent powder LED (light emitting diode) lamp |
CN203868787U (en) * | 2014-06-16 | 2014-10-08 | 厦门大学 | Remote fluorescent powder LED (Light-Emitting Diode) lamp |
CN104198453A (en) * | 2014-09-15 | 2014-12-10 | 厦门大学 | Remote fluorescent powder performance test device and test method |
CN207198042U (en) * | 2017-08-28 | 2018-04-06 | 重庆光遥光电科技有限公司 | LD excites the test device of long-distance fluorescent powder in a kind of integrating sphere |
-
2017
- 2017-08-28 CN CN201710749743.2A patent/CN107367498A/en active Pending
Patent Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20100277059A1 (en) * | 2009-05-01 | 2010-11-04 | Renaissance Lighting, Inc. | Light fixture using doped semiconductor nanophosphor in a gas |
US20120264236A1 (en) * | 2011-04-15 | 2012-10-18 | Chang Gung University | Fluorescent powder applying device and method capable of detecting instantly color temperature of white light in a manufacturing process |
WO2012154446A1 (en) * | 2011-05-12 | 2012-11-15 | 3M Innovative Properties Company | Optical structure for remote phosphor led |
CN102563539A (en) * | 2012-01-11 | 2012-07-11 | 山东浪潮华光照明有限公司 | Optical fiber type remote light distribution method realized by aid of fluorescent powder |
CN103308499A (en) * | 2013-05-24 | 2013-09-18 | 厦门大学 | Device and method for testing performance of blue light-emitting diode (LED) excitation fluorescent powder |
CN103557457A (en) * | 2013-10-30 | 2014-02-05 | 山东明华光电科技有限公司 | Remote excitation fluorescent powder LED (light emitting diode) lamp |
CN203868787U (en) * | 2014-06-16 | 2014-10-08 | 厦门大学 | Remote fluorescent powder LED (Light-Emitting Diode) lamp |
CN104198453A (en) * | 2014-09-15 | 2014-12-10 | 厦门大学 | Remote fluorescent powder performance test device and test method |
CN207198042U (en) * | 2017-08-28 | 2018-04-06 | 重庆光遥光电科技有限公司 | LD excites the test device of long-distance fluorescent powder in a kind of integrating sphere |
Non-Patent Citations (1)
Title |
---|
肖华;郭自泉;党思佳;王阳夏;肖俊;史园;: "远程荧光粉形状对LED发光性能的影响" * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110161010A (en) * | 2019-07-01 | 2019-08-23 | 河海大学常州校区 | A kind of reflective controllable temperature laser excitation remote fluorescence material testing apparatus |
CN110161010B (en) * | 2019-07-01 | 2021-10-08 | 河海大学常州校区 | Reflective temperature-controllable laser excitation remote fluorescent material testing device |
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