CN110194955A - The manganese ion activated hexafluoro germanium sodium red emission nano fibrous membrane of tetravalence and its application in white light LEDs - Google Patents
The manganese ion activated hexafluoro germanium sodium red emission nano fibrous membrane of tetravalence and its application in white light LEDs Download PDFInfo
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- CN110194955A CN110194955A CN201910557664.0A CN201910557664A CN110194955A CN 110194955 A CN110194955 A CN 110194955A CN 201910557664 A CN201910557664 A CN 201910557664A CN 110194955 A CN110194955 A CN 110194955A
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- 239000012528 membrane Substances 0.000 title claims abstract description 33
- 229910001437 manganese ion Inorganic materials 0.000 title claims abstract description 13
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 title claims abstract description 12
- QGHDLJAZIIFENW-UHFFFAOYSA-N 4-[1,1,1,3,3,3-hexafluoro-2-(4-hydroxy-3-prop-2-enylphenyl)propan-2-yl]-2-prop-2-enylphenol Chemical group C1=C(CC=C)C(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C(CC=C)=C1 QGHDLJAZIIFENW-UHFFFAOYSA-N 0.000 title description 2
- GWNAJLSPZNJDQW-UHFFFAOYSA-N [Na].[Ge] Chemical compound [Na].[Ge] GWNAJLSPZNJDQW-UHFFFAOYSA-N 0.000 title description 2
- 239000000843 powder Substances 0.000 claims abstract description 43
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 25
- -1 hexafluoro germanium sodium Chemical compound 0.000 claims abstract description 25
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- 238000009987 spinning Methods 0.000 claims abstract description 15
- 229920003082 Povidone K 90 Polymers 0.000 claims abstract description 8
- 238000013019 agitation Methods 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 15
- 239000011347 resin Substances 0.000 claims description 14
- 229920005989 resin Polymers 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 229910000590 K2MnF6 Inorganic materials 0.000 claims description 9
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 claims description 9
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium oxide Inorganic materials O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000011734 sodium Substances 0.000 claims description 8
- MFYSUUPKMDJYPF-UHFFFAOYSA-N 2-[(4-methyl-2-nitrophenyl)diazenyl]-3-oxo-n-phenylbutanamide Chemical compound C=1C=CC=CC=1NC(=O)C(C(=O)C)N=NC1=CC=C(C)C=C1[N+]([O-])=O MFYSUUPKMDJYPF-UHFFFAOYSA-N 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000011572 manganese Substances 0.000 claims description 3
- 238000009877 rendering Methods 0.000 claims description 3
- 238000000975 co-precipitation Methods 0.000 claims description 2
- 229920003023 plastic Polymers 0.000 claims description 2
- 239000004033 plastic Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 6
- 230000005284 excitation Effects 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000002070 nanowire Substances 0.000 description 7
- 239000007832 Na2SO4 Substances 0.000 description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 description 5
- 230000004913 activation Effects 0.000 description 4
- 239000002121 nanofiber Substances 0.000 description 4
- 229910052693 Europium Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 3
- QGKBPWOLFJRLKE-UHFFFAOYSA-J distrontium;phosphonato phosphate Chemical compound [Sr+2].[Sr+2].[O-]P([O-])(=O)OP([O-])([O-])=O QGKBPWOLFJRLKE-UHFFFAOYSA-J 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- JHLNERQLKQQLRZ-UHFFFAOYSA-N calcium silicate Chemical compound [Ca+2].[Ca+2].[O-][Si]([O-])([O-])[O-] JHLNERQLKQQLRZ-UHFFFAOYSA-N 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- 235000012241 calcium silicate Nutrition 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000000695 excitation spectrum Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 229910021534 tricalcium silicate Inorganic materials 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
-
- H01L33/502—
-
- H01L33/505—
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a kind of hexafluoro germanium sodium red emission nano fibrous membranes that tetravalence is manganese ion activated, are applied in white light LEDs, so as to improve the luminescent properties of white light LEDs.The nano fibrous membrane prepared is capable of the feux rouges of emitting bright, most strong emission peak is at 628nm under ultraviolet light or blue light excitation.The invention also discloses the preparation methods of such red emission nano fibrous membrane: weighing hexafluoro germanium sodium red fluorescence powder first and PVP-K90 is put into conical flask.Then, DMF is instilled in above-mentioned conical flask and magnetic agitation 48 hours with syringe, obtains spinning solution.Finally, spinning solution is transferred in the device of electrostatic spinning, electrostatic spinning is carried out.Remarkable advantage of the invention is that required equipment and technology requirement is low, and preparation method is simple, and the fluorescent material of synthesis can significantly improve the luminescent properties of white light LEDs.
Description
Technical field
The present invention relates to warm white LED fields, using electrostatic spinning technique that the hexafluoro germanium sodium red of manganese ion doping is glimmering
Light powder is converted to the nano fibrous membrane of red emission.The film is applied in the encapsulation process of white light LEDs, can significantly improve white
The luminescent properties of light LED.
Background technique
In recent years, white light emitting diode (WLED) is quickly grown, due to its with brightness height, energy conservation, long service life,
The features such as environmentally friendly, is widely used in the lighting areas such as indoor and outdoor lighting, display backlight, agricultural.Currently, by blue emission two
Pole pipe chip and yellow fluorescent powder Y3Al5O12:Ce3+(YAG:Ce3+) combine be obtain commercialization WLED device main policies.
Although this device can obtain white light, there are some disadvantages in such WLED, such as colour rendering index low (CRI, Ra
<80), colour temperature is high (CCT>4000K).Under blue excitation, transition metal ions (Mn4+) activation fluorescent powder usually in 620-
Deep red emission is shown at 750nm.It is considered as the optimal candidate substance of red emissive material.
It is with organic resin by Eu in general, during encapsulating LED2+The nitride or Mn of doping4+The fluorination of doping
The red fluorescence powders such as object and YAG:Ce3+Yellow fluorescent powder mixing, and be encapsulated on blue chip to obtain warm white.So
And when red fluorescence powder is blended directly in organic resin, it, can shadow since the refractive index of organic resin and fluorescent powder mismatches
Ring the luminescent properties for arriving red fluorescence powder.Therefore, it is necessary to which finding one kind efficiently separates method, by organic resin and fluorescent powder
It separates.The nano fibrous membrane of red emission can be prepared by simple electrostatic spinning technique, can be avoided organic resin with
The interaction of fluorescent powder, and the performance of WLED can be effectively improved.Nanowire is prepared using electrostatic spinning technique at present
Peacekeeping nano fibrous membrane, and it is seldom to apply it to the report in white light LEDs.The Z.Liu of East China Normal University exists
Ceram.Int., report on 2017,43,5674-5679 and prepared using the method that electrostatic spinning and high temperature sintering combine
CaAl12O19:Mn4+Fiber applies it in white light LEDs the colour rendering index and colour temperature for achieving the purpose that improve white light LEDs.And
In the patent of Patent No. CN103409817B, electrostatic spinning technology of preparing is carefully used, three primary colors fluorescent powder rouge and powder is utilized
For trivalent europium (Eu3+) activation Y2Si2O7；Green powder is divalent europium (Eu2+) activation calcium orthosilicate (Ca3SiO5)；Blue powder is divalent
Europium (Eu2+) activation strontium pyrophosphate (Sr2P2O7) tunica fibrosa is prepared to obtain white light LEDs.According to ours the study found that
Na2GeF6As Mn4+Excellent host material can be obtained by simple coprecipitation.The nano-scale of acquisition
Na2GeF6: Mn4+Red fluorescence powder can be converted to nano fibrous membrane by electrostatic spinning technique, apply it in white light LEDs
The luminescent properties of white light LEDs can significantly be improved.
Summary of the invention
It is an object of the invention to prepare the fluoride nano-fiber film of red emission using simple electrostatic spinning technique,
It can be realized and efficiently separate fluorescent powder and organic resin.
Another object of the present invention is to prepare nanofiber using the manganese ion activated fluoride red fluorescence powder of tetravalence
Film is simultaneously applied in white light LEDs, to obtain the method for improving white light LEDs luminescent properties.The nano fibrous membrane prepared,
Under the excitation of ultraviolet light or blue light, it is capable of the feux rouges of emitting bright, most strong emission peak is near 628nm.
Technical solution of the present invention:
The preparation process of the hexafluoro germanium sodium red fluorescence powder of tetravalence manganese ion doping, includes the following steps:
Step 1: raw material is weighed, by the elemental mole ratios Na:Ge:Mn=2:1:X (and of X=0.01,0.03,0.05,0.07
0.09).Precise Na respectively2SO4、GeO2And K2MnF6And measure hydrofluoric acid solution and deionized water.
Step 2: hydrofluoric acid solution and deionized water that step (1) weighs are respectively placed in plastic beaker, it will be in step 1
Weighed GeO2After hydrofluoric acid solution is added, GeF is formed with magnetic stirrer at room temperature6 3-Solution.
Step 3: by weighed K2MnF6It is added in above-mentioned solution, continues stirring 10 minutes.
Step 4: and then the Na that will be accurately weighed2SO4It is add to deionized water, is added drop-wise to above-mentioned solution after completely dissolution
In, it stirs 30 minutes, beaker standing is obtained into light-yellow precipitate after ten minutes, is centrifugated, washing for several times, after dry, obtains
Hexafluoro germanium sodium red fluorescence powder.
The preparation method of red emission nano fibrous membrane, includes the following steps:
Step 1: weighing hexafluoro germanium sodium red fluorescence powder and PVP-K90 (as skeleton) is put into conical flask.
Step 2: using syringe to instill DMF (as dispersing agent) in above-mentioned conical flask and magnetic agitation 48 hours, obtain
To spinning solution.
Step 3: spinning solution being transferred in the device of electrostatic spinning, electrostatic spinning is carried out, finally obtains red emission
Nano fibrous membrane.
The preparation method of warm white LED, includes the following steps:
Step 1: by yellow fluorescent powder (YAG:Ce3+) mixed with organic resin, it is coated in the surface blue chip (InGaN).
Step 2: and then lie in the red emission nano fibrous membrane of preparation on chip.
The nano fibrous membrane of red emission of the invention, can be realized and efficiently separate fluorescent powder and organic resin, high
Fluorescence intensity is expected to become a kind of red fluorescence material haveing excellent performance and be applied to warm white LED.Feux rouges prepared by the present invention
The nano fibrous membrane of transmitting can be excited by ultraviolet light or blue light, suitable for current LED blue chip.Swash in blue light source
Under the conditions of hair, the luminosity of red fluorescence is shown in the section 550-700nm, the centre of luminescence, can be near~628nm
It applies in display fields such as solid state LEDs.For the present invention using the nano fibrous membrane of red emission as red fluorescence material, use is coprecipitated
Prepared by shallow lake method and electrostatic spinning technique, this method is simple and easy, low to equipment and technique requirement, does not need at high-temperature and high-pressure conditions
Reason, synthesis cycle are short.At room temperature, using the nano fibrous membrane of red emission as the available property of red fluorescence material
The excellent warm white LED of energy.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram of prepared nano fibrous membrane；
Fig. 2 is the stereoscan photograph of prepared nano fibrous membrane；
Fig. 3 is the excitation spectrum and launching light spectrogram of prepared nano fibrous membrane；
Fig. 4 is the chromatic diagram of prepared nano fibrous membrane；
Fig. 5 is the electroluminescent light of blue chip, commercial warm white LED and the white light LEDs using nanofiber film preparation
Spectrogram；
Fig. 6 is the chromatic diagram of commercial warm white LED and the white light LEDs using nanofiber film preparation, and illustration is Nanowire
The pictorial diagram of film is tieed up, which doubles as being Figure of abstract；
Specific embodiment
Embodiment 1:0.4866g GeO2After being added to 20mL hydrofluoric acid solution, formed at room temperature with magnetic stirrer
GeF6 3-Solution.Weighed 0.0123g K2MnF6It is added in above-mentioned solution, continues stirring 10 minutes.Then it accurately weighs
1.4204g Na2SO4It is add to deionized water, is added drop-wise in above-mentioned solution after completely dissolution, stirred 30 minutes, beaker is quiet
It sets and obtains light-yellow precipitate after ten minutes, be centrifugated, washing for several times, after dry, obtains hexafluoro germanium sodium red fluorescence powder.It weighs
1.0000g hexafluoro germanium sodium red fluorescence powder and 1.0000g PVP-K90 (as skeleton) are put into conical flask.It will with syringe
5.0000g DMF (as dispersing agent) is instilled in above-mentioned conical flask and magnetic agitation 48 hours, obtains spinning solution.By spinning
Solution is transferred in the device of electrostatic spinning, is carried out electrostatic spinning, is finally obtained red emission nano fibrous membrane.By yellow fluorescence
Powder (YAG:Ce3+) mixed with organic resin, it is coated in the surface blue chip (InGaN).Then by the red emission Nanowire of preparation
Dimension film is lain on chip.
Embodiment 2:0.4866g GeO2After being added to 20mL hydrofluoric acid solution, formed at room temperature with magnetic stirrer
GeF6 3-Solution.Weighed 0.0370g K2MnF6It is added in above-mentioned solution, continues stirring 10 minutes.Then it accurately weighs
1.4204g Na2SO4It is add to deionized water, is added drop-wise in above-mentioned solution after completely dissolution, stirred 30 minutes, beaker is quiet
It sets and obtains light-yellow precipitate after ten minutes, be centrifugated, washing for several times, after dry, obtains hexafluoro germanium sodium red fluorescence powder.It weighs
1.0000g hexafluoro germanium sodium red fluorescence powder and 1.0000g PVP-K90 (as skeleton) are put into conical flask.It will with syringe
5.0000gDMF (as dispersing agent) is instilled in above-mentioned conical flask and magnetic agitation 48 hours, obtains spinning solution.By spinning
Solution is transferred in the device of electrostatic spinning, is carried out electrostatic spinning, is finally obtained red emission nano fibrous membrane.By yellow fluorescence
Powder (YAG:Ce3+) mixed with organic resin, it is coated in the surface blue chip (InGaN).Then by the red emission Nanowire of preparation
Dimension film is lain on chip.
Embodiment 3:0.4866g GeO2After being added to 20mL hydrofluoric acid solution, formed at room temperature with magnetic stirrer
GeF6 3-Solution.Weighed 0.0617g K2MnF6It is added in above-mentioned solution, continues stirring 10 minutes.Then it accurately weighs
1.4204g Na2SO4It is add to deionized water, is added drop-wise in above-mentioned solution after completely dissolution, stirred 30 minutes, beaker is quiet
It sets and obtains light-yellow precipitate after ten minutes, be centrifugated, washing for several times, after dry, obtains hexafluoro germanium sodium red fluorescence powder.It weighs
1.0000g hexafluoro germanium sodium red fluorescence powder and 1.0000g PVP-K90 (as skeleton) are put into conical flask.It will with syringe
5.0000gDMF (as dispersing agent) is instilled in above-mentioned conical flask and magnetic agitation 48 hours, obtains spinning solution.By spinning
Solution is transferred in the device of electrostatic spinning, is carried out electrostatic spinning, is finally obtained red emission nano fibrous membrane.By yellow fluorescence
Powder (YAG:Ce3+) mixed with organic resin, it is coated in the surface blue chip (InGaN).Then by the red emission Nanowire of preparation
Dimension film is lain on chip.
Embodiment 4:0.4866g GeO2After being added to 20mL hydrofluoric acid solution, formed at room temperature with magnetic stirrer
GeF6 3-Solution.Weighed 0.0864g K2MnF6It is added in above-mentioned solution, continues stirring 10 minutes.Then it accurately weighs
1.4204g Na2SO4It is add to deionized water, is added drop-wise in above-mentioned solution after completely dissolution, stirred 30 minutes, beaker is quiet
It sets and obtains light-yellow precipitate after ten minutes, be centrifugated, washing for several times, after dry, obtains hexafluoro germanium sodium red fluorescence powder.It weighs
1.0000g hexafluoro germanium sodium red fluorescence powder and 1.0000g PVP-K90 (as skeleton) are put into conical flask.It will with syringe
5.0000gDMF (as dispersing agent) is instilled in above-mentioned conical flask and magnetic agitation 48 hours, obtains spinning solution.By spinning
Solution is transferred in the device of electrostatic spinning, is carried out electrostatic spinning, is finally obtained red emission nano fibrous membrane.By yellow fluorescence
Powder (YAG:Ce3+) mixed with organic resin, it is coated in the surface blue chip (InGaN).Then by the red emission Nanowire of preparation
Dimension film is lain on chip.
Embodiment 5:0.4866g GeO2After being added to 20mL hydrofluoric acid solution, formed at room temperature with magnetic stirrer
GeF6 3-Solution.Weighed 0.1111g K2MnF6It is added in above-mentioned solution, continues stirring 10 minutes.Then it accurately weighs
1.4204g Na2SO4It is add to deionized water, is added drop-wise in above-mentioned solution after completely dissolution, stirred 30 minutes, beaker is quiet
It sets and obtains light-yellow precipitate after ten minutes, be centrifugated, washing for several times, after dry, obtains hexafluoro germanium sodium red fluorescence powder.It weighs
1.0000g hexafluoro germanium sodium red fluorescence powder and 1.0000g PVP-K90 (as skeleton) are put into conical flask.It will with syringe
5.0000g DMF (as dispersing agent) is instilled in above-mentioned conical flask and magnetic agitation 48 hours, obtains spinning solution.By spinning
Solution is transferred in the device of electrostatic spinning, is carried out electrostatic spinning, is finally obtained red emission nano fibrous membrane.By yellow fluorescence
Powder (YAG:Ce3+) mixed with organic resin, it is coated in the surface blue chip (InGaN).Then by the red emission Nanowire of preparation
Dimension film is lain on chip.
Claims (5)
1. the nano fibrous membrane of the hexafluoro germanium sodium red fluorescence powder preparation red emission using tetravalence manganese ion doping.Its feature exists
In, first using coprecipitation preparation tetravalence manganese ion doping hexafluoro germanium sodium red fluorescence powder, then utilize electrostatic spinning technique
Prepare the nano fibrous membrane of the hexafluoro germanium sodium red emission of manganese ion doping.
2. the nano fibrous membrane of the hexafluoro germanium sodium red emission of the manganese ion doping prepared according to claim 1 is applied to white
In light LED, which is characterized in that the nano fibrous membrane launch wavelength is located at 575-675nm, and most strong emission peak is located near 628nm,
It is applied to the nano fibrous membrane of red emission that can significantly improve the colour rendering index of white light LEDs in white light LEDs and reduces color
Temperature value.
3. the preparation process of the hexafluoro germanium sodium red fluorescence powder of tetravalence manganese ion doping, which comprises the steps of:
Step 1: raw material is weighed, by elemental mole ratios Na:Ge:Mn=2:1:X (X=0.01,0.03,0.05,0.07 and 0.09),
Na is weighed respectively2SO4、GeO2And K2MnF6And measure hydrofluoric acid solution and deionized water；
Step 2: hydrofluoric acid solution and deionized water that step (1) weighs being respectively placed in plastic beaker, will be weighed in step 1
GeO2After hydrofluoric acid solution is added, GeF is formed with magnetic stirrer at room temperature6 3-Solution；
Step 3: by weighed K2MnF6It is added in above-mentioned solution, continues stirring 10 minutes；
Step 4: the Na that will be accurately weighed2SO4It is add to deionized water, is added drop-wise in above-mentioned solution after completely dissolution, stirring 30
Minute, beaker standing is obtained into light-yellow precipitate after ten minutes, is centrifugated, washing for several times, after dry, obtains manganese ion doping
Hexafluoro germanium sodium red fluorescence powder.
4. the preparation method of the hexafluoro germanium sodium red emission nano fibrous membrane of manganese ion doping, which is characterized in that including walking as follows
It is rapid:
Step 1: weighing hexafluoro germanium sodium red fluorescence powder and PVP-K90 (as skeleton) is put into conical flask；
Step 2: using syringe to instill DMF (as dispersing agent) in above-mentioned conical flask and magnetic agitation 48 hours, spun
Silk solution；
Step 3: spinning solution being transferred in the device of electrostatic spinning, electrostatic spinning is carried out, finally obtains red emission nanometer
Tunica fibrosa.
5. the preparation method of warm white LED, which comprises the steps of:
Step 1: by yellow fluorescent powder (YAG:Ce3+) mixed with organic resin, it is coated in the surface blue chip (InGaN)；
Step 2: and then lie in the red emission nano fibrous membrane of preparation on chip.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116200193A (en) * | 2023-01-18 | 2023-06-02 | 大连工业大学 | Mn (Mn) 4+ Activation K 0.6 Ba 0.7 Si 0.5 Ge 0.5 F 6 Preparation of red fluorescent powder and application of red fluorescent powder in warm white light LED |
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