CN108336208B - LED light source for spectrophotometer and preparation method thereof - Google Patents
LED light source for spectrophotometer and preparation method thereof Download PDFInfo
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
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- H—ELECTRICITY
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
- H01L33/504—Elements with two or more wavelength conversion materials
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Abstract
The invention discloses an LED light source for a spectrophotometer and a preparation method thereof. The LED light source for the spectrophotometer comprises an ultraviolet LED chip and mixed fluorescent powder packaged on the ultraviolet LED chip; the mixed fluorescent powder is composed of blue fluorescent powder, green fluorescent powder, red fluorescent powder and near-infrared fluorescent powder, and the mass ratio is 12-18: 35-45: 0.8-1.2: 500-800 and all can be excited by the ultraviolet light emitted by the ultraviolet LED chip. The device overcomes the defects that the traditional light source lamp (combination of a deuterium lamp and a tungsten lamp) is large in size, short in service life and long in service life, and the light source needs to be switched during wide spectral range testing, and has the advantages that the light source is not easy to damage; meanwhile, the luminous intensities of the ultraviolet and visible light regions at different wavelength positions are similar, so that when a spectrophotometer based on a multi-channel detector is used for rapidly collecting absorption spectra, the method is simple, convenient and rapid, and the signal-to-noise ratio of the obtained absorption spectra is good.
Description
Technical Field
The invention belongs to the field of analytical instruments, and particularly relates to an LED light source for a spectrophotometer and a preparation method thereof.
Background
Spectrophotometers are commonly used spectroscopic instruments for analytical testing. The method is widely applied to production and scientific research in the fields of agriculture, chemical industry, food, environment, materials, medicine and the like. An ideal spectrophotometer light source requires that the light emitted by the light source has a substantially constant intensity at different wavelengths throughout the measured spectral region. However, no light source has yet achieved the desired spectrum.
Currently, a common spectrophotometer generally uses a deuterium tungsten combined light source including two light source lamps, one is a lamp for an ultraviolet region (deuterium lamp, mercury lamp, hydrogen lamp, etc.), and the other is a lamp for a visible region (tungsten lamp, halogen lamp, etc.). The emission spectra of the two lamps are shown in fig. 1 and fig. 2, respectively. This combination of light sources has significant disadvantages in use: 1. the light sources are easy to damage and short in service life; 2. when testing a spectrum covering a wide ultraviolet and visible spectrum range, two light source lamps need to be switched, which not only brings extra trouble to instrument design, but also causes the test effect to be poor; 3. although the deuterium lamp and tungsten lamp combined light source has certain output intensity at different positions of the whole spectrum region, the intensity difference at different wavelength positions is obvious, the intensity of a few wavelengths is too high or too low, when an absorption spectrum test covering an ultraviolet visible wide spectrum range is carried out, the signal to noise ratio of certain spectrum regions is deteriorated, and the deuterium lamp and tungsten lamp combined light source is particularly not suitable for the application of the rapid spectrum detection of a novel spectrophotometer based on a multi-channel detector such as a fiber spectrometer.
White light LEDs have been used as a new light source because of their advantages such as broad wavelength range of emission spectra and long lifetime. However, the application of the spectrophotometer as a light source has not been reported. The following methods are mainly used for realizing the white light LED:
(1) the red, green and blue LED chips are adopted to emit light in a combined manner to obtain white light;
(2) exciting yellow fluorescent powder by using a blue LED chip, and obtaining white light by complementing blue light and yellow light;
(3) the ultraviolet LED chip is used for exciting red, green and blue three-primary-color fluorescent powder to obtain white light.
There are a lot of papers and patents on the manufacturing method of the above white LED and the development of the related phosphor, but most of the application fields of the schemes are focused on the illumination field, and the main disadvantages of these reports are transferred to the spectrophotometer light source as follows:
as for the method (1), chinese utility model CN 201520204294.X discloses an ultraviolet LED lamp, which comprises a carrier substrate, the carrier substrate on be equipped with three separately-controlled ultraviolet LED chips respectively, the ultraviolet LED chip on coat respectively with red phosphor, blue phosphor and green phosphor, when the phosphor is excited by the ultraviolet chip to emit the color light of red light, green light, blue light, remove the control spectrum stack and form white light. Although the white light LED obtained by the scheme is high and adjustable in color rendering index, the spectrophotometer has higher requirement on the stability of a light source, and the three-chip scheme has a complex structure and can lead to poor stability of the light source due to the independent control of each chip, so that the effect of the white light LED is not as good as that of a single-chip mixed fluorescent powder when being used for the light source of the spectrophotometer.
The method (2) is improved in chinese patent application No. CN102127436A by using ultraviolet light or purple light in the spectrum of a blue LED to excite green phosphor and red phosphor to generate green light and red light, respectively, and the generated green light and red light are further mixed with the blue light to form white light, thereby improving the light utilization rate of the blue LED, and realizing control of the color rendering property of the white light in a large range, and being used as a green illumination light source. However, the LED light source obtained by the above solution cannot be used as a spectrophotometer light source well, mainly because the main application field is illumination, and the evaluation of the light emission spectrum of the LED light source for this application is better in the case of simulating the solar spectrum, and the relative light emission intensity of the light source at different wavelengths is required to be similar to the solar spectrum, which is contrary to the use requirement that the spectrophotometer requires the light source to have close light emission intensity at different wavelengths; meanwhile, the spectrophotometer also requires a light source to emit light with a wide wavelength range, and the LED obtained by the scheme is only limited to the visible light range, so the effect is not ideal when the LED is used as the light source of the spectrophotometer.
As for the method (3), chinese patent application CN201710696238.6 discloses an ultraviolet-excited white light LED containing a trichromatic phosphor, which includes a UVLED chip, a trichromatic phosphor colloid formed by mixing red phosphor, green phosphor, blue phosphor and phosphor colloid, and the trichromatic phosphor colloid is coated on the UVLED chip. Similarly, the white light LED obtained by the scheme is mainly used for illumination, and the luminous intensity is not uniform at different wavelengths in the ultraviolet-visible light range, so that the white light LED is difficult to be used as a light source of a spectrophotometer.
In summary, there is still a lack of a white LED which can emit light with uniform intensity over a wide wavelength range and has good stability and can be used as a light source of a spectrophotometer.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention mainly aims to provide the LED light source for the spectrophotometer.
The invention also aims to provide a preparation method of the LED light source for the spectrophotometer.
The purpose of the invention is realized by the following technical scheme:
an LED light source for a spectrophotometer comprises an ultraviolet LED chip and mixed fluorescent powder packaged on the ultraviolet LED chip; the mixed fluorescent powder consists of the following components: blue fluorescent powder with emission peak wavelength of 420-450 nm, green fluorescent powder with emission peak wavelength of 520-540 nm, red fluorescent powder with emission peak wavelength of 590-680 nm and near infrared fluorescent powder with emission peak wavelength of 750-850 nm; the mass ratio of the blue fluorescent powder to the green fluorescent powder to the red fluorescent powder to the near-infrared fluorescent powder is 12-18: 35-45: 0.8-1.2: 500-800 and all can be excited by the ultraviolet light emitted by the ultraviolet LED chip.
Preferably, the coverage range of the emission wavelength of the blue fluorescent powder is 380-480 nm, the coverage range of the emission wavelength of the green fluorescent powder is 490-560 nm, the coverage range of the emission wavelength of the red fluorescent powder is 570-700 nm, and the coverage range of the emission wavelength of the near-infrared fluorescent powder is 710-900 nm.
Preferably, the mass ratio of the blue fluorescent powder to the green fluorescent powder to the red fluorescent powder to the near-infrared fluorescent powder is 15: 40: 1: 600.
preferably, the chemical formula of the near-infrared fluorescent powder is Ca1.96Mg0.999WO6:0.02Bi3+,0.001Cr3+The preparation method comprises the following steps:
(1) according to the formula Ca1.96Mg0.999WO6:0.02Bi3+,0.001Cr3+Weighing CaCO at a stoichiometric ratio3、WO3、MgO、Bi2O3And Cr (NO)3)3And mixing them uniformly;
(2) heating the raw material mixture obtained in the step (1) at 600 ℃ for 2 h;
(3) and (3) cooling and grinding the sample obtained after heating in the step (2), then sintering at 1300 ℃ for 5h, and cooling and grinding to obtain the near-infrared fluorescent powder.
Preferably, the thickness of the mixed fluorescent powder is 0.10-0.25 cm.
The preparation method of the LED light source for the spectrophotometer comprises the following steps:
(1) uniformly mixing the blue fluorescent powder, the green fluorescent powder, the red fluorescent powder and the near-infrared fluorescent powder;
(2) mixing the LED packaging adhesive with the mixed fluorescent powder obtained in the step (1), uniformly stirring, and performing vacuum defoaming to obtain a mixed fluorescent colloid;
(3) coating the mixed fluorescent colloid obtained in the step (2) on the surface of an ultraviolet LED chip;
(4) and (4) baking the ultraviolet LED chip coated with the mixed fluorescent colloid in the step (3) to obtain the LED light source for the spectrophotometer.
Preferably, the mass ratio of the mixed fluorescent powder in the step (2) to the LED packaging adhesive is 1: 1.5 to 2.5.
Preferably, the glue material of the packaging glue in the step (2) is silica gel, and the silica gel is firstly stirred for 5-10 min and then mixed with the mixed fluorescent powder obtained in the step (1).
Preferably, the stirring time in the step (2) is 5-10 min, and the vacuum defoaming time is 3-5 h.
Preferably, the baking in the step (4) is baking for 1-2 hours at 90-100 ℃, and then heating to 130-160 ℃ for further baking for 2.5-3.5 hours.
The principle of the spectrophotometer light source with wide spectral range based on the ultraviolet LED is similar to that of the white light LED (3) in the background technology, and the spectrophotometer light source consists of an LED chip capable of emitting ultraviolet light after being electrified and fluorescent powder with spectral conversion function. Compared with a three-chip scheme, a single-chip LED is prone to cross-reabsorption of different phosphors, which results in a problem of greatly reduced luminous efficiency, and thus, the single-chip LED scheme is practically eliminated in white LED applications for illumination. The reduction of the luminous efficiency is a fatal problem for the use of a high-power white light LED, but because the spectrophotometer light source does not require high luminous intensity, the power of the light source is low, and the reduction of the LED luminous efficiency is easily compensated by properly improving the LED power, the defect of the single-chip LED light source is completely acceptable when the single-chip LED light source is used as the spectrophotometer light source. Meanwhile, the single-chip mixed fluorescent powder scheme has better luminous stability, and is particularly more favorable for adjusting the light path of a spectrophotometer in actual work, so that the single-chip mixed fluorescent powder has ideal effect in the aspect of application of the spectrophotometer.
Considering that the LED light source for the spectrophotometer needs to emit a spectrum with approximate equal intensity in a wide wavelength range, the invention also adds near infrared fluorescent powder in a proper wavelength range in addition to the conventional red, green and blue fluorescent powder. The spectrophotometer has lower requirement on the luminous intensity, the cross reabsorption influence caused by the increase of the types of the fluorescent powder is not large, and the addition of a proper amount of near-infrared fluorescent powder can expand the luminous range of the white light LED to a near-infrared region (800 plus 1000nm), so that the requirements of the spectrophotometer can be better met.
At present, two light source lamps are commonly used for a common spectrophotometer, one is a lamp (deuterium lamp or hydrogen lamp) used in an ultraviolet region, and the other is a lamp (tungsten lamp) used in a visible light region.
Compared with the prior art, the LED light source for the spectrophotometer provided by the invention has the following advantages and effects:
(1) the output intensity of the basic equal intensity in the wide wavelength range can be seen in fig. 4-6, and the operation is simple without additional equipment acquisition cost and energy consumption;
(2) small in size, the nature is stable, and long service life is expected to be used for various spectrophotometers, especially novel optic fibre spectroscopy system, can simplify the instrument design greatly, improves the stability of instrument, realizes the miniaturization and the miniaturization of instrument.
Drawings
Fig. 1 is an emission spectrum of a deuterium lamp;
FIG. 2 is an emission spectrum of a tungsten lamp;
FIG. 3 is a view showing an LED light source for a spectrophotometer obtained in example 1;
FIG. 4 is an emission spectrum of an LED light source for a spectrophotometer obtained in example 1;
FIG. 5 is an emission spectrum of an LED light source for a spectrophotometer obtained in example 1;
FIG. 6 is an emission spectrum of an LED light source for a spectrophotometer obtained in example 1;
FIG. 7 shows emission spectra of red, green, blue, and near-infrared phosphors used in the examples.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
The specific types and performance parameters of the phosphor and the ultraviolet LED chips used in the following examples are as follows:
the blue fluorescent powder is rare earth doped tungstate compound fluorescent powder, the emission peak value is 450nm under the excitation of the ultraviolet LED chip, and the emission spectrum is shown in figure 7.
The green fluorescent powder is rare earth doped fluosilicate compound fluorescent powder, the emission peak value is 520nm under the excitation of the ultraviolet LED chip, and the emission spectrum is shown in figure 7.
The red fluorescent powder is ion-doped titanate fluorescent powder, the emission peak value is 675nm under the excitation of the ultraviolet LED chip, and the emission spectrum is shown in figure 7.
The chemical formula of the near-infrared fluorescent powder is Ca1.96Mg0.999WO6:0.02Bi3+,0.001Cr3+. The preparation method of the fluorescent powder comprises the following steps:
(1) according to Ca1.96Mg0.999WO6:0.02Bi3+,0.001Cr3+The stoichiometric ratio of the raw material CaCO is accurately weighed3、WO3、MgO、Bi2O3And Cr (NO)3)3Fully grinding and uniformly mixing the raw materials in an agate mortar to obtain a raw material mixture;
(2) and (2) placing the raw material mixture obtained in the step (1) in a corundum crucible and transferring the corundum crucible into a muffle furnace. The muffle furnace is heated to 600 ℃ and kept at the constant temperature for 2 hours;
(3) and (3) cooling the sample obtained in the step (2), taking out the sample, grinding again, sintering at the high temperature of 1300 ℃ for 5 hours, furnace-cooling to room temperature, and grinding the obtained sintered body into powder.
The emission spectrum is shown in FIG. 7.
The emission wavelength of the ultraviolet external LED chip is 260-390 nm.
Example 1
The preparation method of the LED light source for the spectrophotometer comprises the following steps:
(1) mixing 15mg of blue fluorescent powder, 40mg of green fluorescent powder, 1mg of red fluorescent powder and 600mg of near-infrared fluorescent powder, and grinding and uniformly mixing in an agate mortar to obtain mixed fluorescent powder;
(2) taking a container, adding 1g of silica gel (My graph, IVS4542) and stirring with a glass rod for 5min, then adding the mixed fluorescent powder obtained in the step (1), stirring with the glass rod for 5min, and then defoaming in vacuum for 4h to obtain a mixed fluorescent colloid;
(3) coating 0.2g of the mixed fluorescent colloid obtained in the step (2) on the surface of an ultraviolet LED chip, wherein the thickness of the mixed fluorescent colloid is 0.1 cm;
(4) and (3) curing: and (3) baking the colloid-coated ultraviolet chip at 100 ℃ for 1h, and then heating to 150 ℃ for baking for 3h to obtain the LED light source for the spectrophotometer. The resulting spectrophotometer with the LED light source is shown in FIG. 3, and the emission spectrum is shown in FIG. 4.
Example 2
The preparation method of the LED light source for the spectrophotometer comprises the following steps:
(1) mixing 12mg of blue fluorescent powder, 35mg of green fluorescent powder, 0.8mg of red fluorescent powder and 500mg of near-infrared fluorescent powder, and grinding and uniformly mixing in an agate mortar to obtain mixed fluorescent powder;
(2) taking a container, adding 1g of silica gel (My graph, IVS4542), uniformly stirring with a glass rod for 5min, then adding the mixed fluorescent powder obtained in the step (1), uniformly stirring with the glass rod for 5min, and then defoaming in vacuum for 4h to obtain a mixed fluorescent colloid;
(3) coating 0.3g of the mixed fluorescent colloid obtained in the step (2) on the surface of an ultraviolet LED chip, wherein the thickness of the mixed fluorescent colloid is 0.2 cm;
(4) and (3) curing: and (3) baking the colloid-coated ultraviolet chip at 100 ℃ for 1h, and then heating to 150 ℃ for baking for 3h to obtain the LED light source for the spectrophotometer. The emission spectrum is shown in fig. 5.
Example 3
The preparation method of the LED light source for the spectrophotometer comprises the following steps:
(1) mixing 18mg of blue fluorescent powder, 45mg of green fluorescent powder, 1.2mg of red fluorescent powder and 800mg of near-infrared fluorescent powder, and grinding and uniformly mixing in an agate mortar to obtain mixed fluorescent powder;
(2) taking a container, adding 1.4g of silica gel (My graph, IVS4542), uniformly stirring with a glass rod for 5min, then adding the mixed fluorescent powder obtained in the step (1), uniformly stirring with the glass rod for 5min, and then defoaming in vacuum for 4h to obtain a mixed fluorescent colloid;
(3) coating 0.3g of the mixed fluorescent colloid obtained in the step (2) on the surface of an ultraviolet LED chip, wherein the thickness of the mixed fluorescent colloid is 0.2 cm;
(4) and (3) curing: and (3) baking the colloid-coated ultraviolet chip at 100 ℃ for 1h, and then heating to 150 ℃ for baking for 3h to obtain the LED light source for the spectrophotometer. The emission spectrum is shown in FIG. 6.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (8)
1. An LED light source for a spectrophotometer is characterized by comprising an ultraviolet LED chip and mixed fluorescent powder packaged on the ultraviolet LED chip; the mixed fluorescent powder consists of the following components: blue fluorescent powder with emission peak wavelength of 420 nm-450 nm, green fluorescent powder with emission peak wavelength of 520-540 nm, red fluorescent powder with emission peak wavelength of 590-680 nm and near infrared fluorescent powder with emission peak wavelength of 750-850 nm; the mass ratio of the blue fluorescent powder to the green fluorescent powder to the red fluorescent powder to the near-infrared fluorescent powder is 12-18: 35-45: 0.8-1.2: 500-800 and all can be excited by the ultraviolet light emitted by the ultraviolet LED chip.
2. The LED light source for spectrophotometer of claim 1, wherein the blue phosphor emission wavelength coverage is 380-480 nm, the green phosphor emission wavelength coverage is 490-560 nm, the red phosphor emission wavelength coverage is 570-700 nm, and the near infrared phosphor emission wavelength coverage is 710-900 nm.
3. The LED light source for the spectrophotometer of claim 1, wherein the mass ratio of the blue phosphor to the green phosphor to the red phosphor to the near-infrared phosphor is 15: 40: 1: 600.
4. the LED light source for spectrophotometer of claim 1, wherein the chemical expression of the near infrared phosphor is Ca1.96Mg0.999WO6:0.02Bi3+,0.001Cr3+。
5. The LED light source for the spectrophotometer of claim 1, wherein the thickness of the mixed phosphor is 0.10 to 0.25 cm.
6. The method for preparing an LED light source for a spectrophotometer according to any one of claims 1 to 5, comprising the steps of:
(1) uniformly mixing the blue fluorescent powder, the green fluorescent powder, the red fluorescent powder and the near-infrared fluorescent powder;
(2) mixing the LED packaging adhesive with the mixed fluorescent powder obtained in the step (1), uniformly stirring, and performing vacuum defoaming to obtain a mixed fluorescent colloid;
(3) coating the mixed fluorescent colloid obtained in the step (2) on the surface of an ultraviolet LED chip;
(4) and (4) baking the ultraviolet LED chip coated with the mixed fluorescent colloid in the step (3) to obtain the LED light source for the spectrophotometer.
7. The method for preparing the LED light source for the spectrophotometer according to claim 6, wherein the LED packaging glue in step (2) is silica gel, the silica gel is firstly stirred for 5-10 min and then mixed with the mixed fluorescent powder obtained in step (1), and the mass ratio of the mixed fluorescent powder to the silica gel is 1: 1.5-2.5;
the preparation method of the near-infrared fluorescent powder comprises the following steps:
(1) according to the formula Ca1.96Mg0.999WO6:0.02Bi3+,0.001Cr3+Weighing CaCO at a stoichiometric ratio3、WO3、MgO、Bi2O3And Cr (NO)3)3And mixing them uniformly;
(2) heating the raw material mixture obtained in the step (1) at 600 ℃ for 2 h;
(3) and (3) cooling and grinding the sample obtained after heating in the step (2), then sintering for 5 hours at 1300 ℃, cooling and grinding to obtain the near-infrared fluorescent powder.
8. The method for preparing the LED light source for the spectrophotometer as claimed in claim 6, wherein the stirring time in step (2) is 5-10 min, the vacuum defoaming time is 3-5 h, and the baking in step (4) is baking at 90-100 ℃ for 1-2 h, and then heating to 130-160 ℃ for 2.5-3.5 h.
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| CN109192844A (en) * | 2018-08-30 | 2019-01-11 | 合肥工业大学智能制造技术研究院 | One kind is repaired and regenerated LED light emitting device and application for retina cell |
| CN109346591A (en) * | 2018-09-29 | 2019-02-15 | 国红（深圳）光电科技有限公司 | Optical devices |
| CN110970541B (en) * | 2018-09-29 | 2023-04-21 | 有研稀土新材料股份有限公司 | Semiconductor light source and optical device prepared by same |
| CN110660892B (en) * | 2019-08-22 | 2021-05-04 | 有研稀土新材料股份有限公司 | Optical device |
| CN111129263A (en) * | 2019-12-30 | 2020-05-08 | 北京宇极芯光光电技术有限公司 | White light LED light source with infrared band added in spectrum |
| CN111207831B (en) * | 2020-01-10 | 2022-05-20 | 安徽皖仪科技股份有限公司 | Light source switching method of multi-light source monochromator |
| CN111189535B (en) * | 2020-01-19 | 2021-02-09 | 广州市轩士佳电子科技有限公司 | LED calibration light source and lamps and lanterns that sensor was used |
| JP2021150360A (en) * | 2020-03-17 | 2021-09-27 | サンケン電気株式会社 | Light-emitting device |
| US20240118220A1 (en) | 2021-02-22 | 2024-04-11 | Panasonic Intellectual Property Management Co., Ltd. | Inspection device and inspection method |
| CN114203887B (en) * | 2021-11-10 | 2024-06-07 | 欧普照明股份有限公司 | Light source module and lighting device comprising same |
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| CN106784264A (en) * | 2017-01-24 | 2017-05-31 | 广东绿爱生物科技股份有限公司 | A kind of LED light source of promotion completely filled fruit |
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| US7259853B2 (en) * | 2004-12-22 | 2007-08-21 | Xerox Corporation | Systems and methods for augmenting spectral range of an LED spectrophotometer |
| JP6080410B2 (en) * | 2012-07-13 | 2017-02-15 | キヤノン株式会社 | Spectral colorimeter |
| US20140273051A1 (en) * | 2013-03-15 | 2014-09-18 | Rakesh Reddy | Chemical sensing apparatus having multiple immobilized reagents |
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| CN106784264A (en) * | 2017-01-24 | 2017-05-31 | 广东绿爱生物科技股份有限公司 | A kind of LED light source of promotion completely filled fruit |
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