CN111323849B - Composite material with high reflectivity of short-wave ultraviolet light, preparation process and application - Google Patents
Composite material with high reflectivity of short-wave ultraviolet light, preparation process and application Download PDFInfo
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- CN111323849B CN111323849B CN202010137601.2A CN202010137601A CN111323849B CN 111323849 B CN111323849 B CN 111323849B CN 202010137601 A CN202010137601 A CN 202010137601A CN 111323849 B CN111323849 B CN 111323849B
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- G—PHYSICS
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- C03—GLASS; MINERAL OR SLAG WOOL
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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Abstract
The invention discloses a composite material with high reflectivity of short-wave ultraviolet light, a preparation process and application thereof. The intermediate glass powder formula comprises silicon oxide, aluminum oxide, borax, sodium carbonate, potassium carbonate and bismuth oxide; the silver powder is nano silver powder. The invention provides an inorganic ternary composite material with high reflectivity for the application of a short-wave ultraviolet LED, and through experimental tests, the effective reflectivity of 272nm ultraviolet light is 91%, so that the requirement of commercial application is met, and the commercial application of the short-wave ultraviolet LED is facilitated. The invention belongs to a composite inorganic material system, can stand the irradiation of ultraviolet light for a long time without aging failure, and has low material composition cost and easy wide popularization. The invention adopts environment-friendly materials and the preparation process does not generate harmful substances.
Description
Technical Field
The invention relates to a nano composite material, in particular to a composite material with high reflectivity of short-wave ultraviolet light, a preparation process and application thereof.
Background
Ultraviolet light, generally having a wavelength of 100nm to 400nm, is classified into extreme ultraviolet, deep ultraviolet, and near ultraviolet. The extreme ultraviolet light refers to ultraviolet light with the wavelength below 200 nanometers, and the obtaining condition of the extreme ultraviolet light is too harsh and relatively less applied; deep ultraviolet generally refers to ultraviolet light with a wavelength of 200-280 nanometers, also called short-wave ultraviolet light, and the wavelength is easily absorbed by metal and glass materials, so that the reflectivity is generally very low, and even the ultraviolet light is not reflected at all. The ultraviolet light with the wavelength of 100-254 nanometers has high ionization energy, can directly irradiate and ionize hydrogen bonds, organic compounds and covalent bonds with low bond energy, and generally has a good sterilization function. Near ultraviolet refers generally to wavelengths of 290nm to 400nm, and is commonly used in phototherapy and gel curing. The photoionization energy of the material with the wavelength of 365-420 nanometers is moderate, the active nanometer material with the bridge oxygen or the oxygen vacancy structure is irradiated by the wavelength of 365-420 nanometers, for example, the rutile-structure material doped with the rare earth oxide, the bridge oxygen or the vacancy oxygen obtains energy after the material is irradiated by the light of 365-420 nanometers, and the material formed by the strong oxidizing particle with negative charges and the material with lower bond energy in the environment, such as hydrogen bonds, organic compounds and covalent bonds, is subjected to oxidation reaction.
The intermediate glass material is a glass material with medium expansion coefficient, medium temperature (1000 ℃) sintering, high strength, high toughness, I-grade chemical stability, lower dielectric constant and lower dielectric loss value, and is widely used for ceramic matrix composites, electronic paste, metal and glass, ceramics and metal, and direct connection or transitional connection between ceramics and glass. The intermediate glass material is an indispensable material in some special application fields, and the formulation and the preparation process technology of the intermediate glass material are relatively unique compared with the traditional glass material.
The traditional short wavelength ultraviolet LED packaging generally does not consider the reflection problem of materials, although similar organic composite materials are used as high-reflection materials of the short wavelength ultraviolet LED, the organic materials are aged and failed by ultraviolet light irradiating for a long time, so that few materials in the existing system can simultaneously meet the following three conditions:
(1) a reflectance of 90% or more;
(2) can bear long-term ultraviolet radiation without aging and denaturation;
(3) the preparation process and the forming are simple, the cost is low, and the environment is protected.
Ultraviolet light is usually generated by a low-pressure mercury lamp, the wavelength of the ultraviolet light is 100-420 nm due to gaseous emission, the trade of mercury-containing products is forbidden in the Water Authority from 6 months 2020, and the EQE quantum efficiency of short-wave ultraviolet light, particularly ultraviolet LED light sources emitting in a solid state, is very low (usually within 5%), so that how to solve the light emitting efficiency of packaged ultraviolet LEDs is particularly important.
Disclosure of Invention
The invention aims to provide a composite material with high reflectivity of short-wave ultraviolet light, a preparation process and application thereof, so as to solve the problems in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
the formula of the composite material with high reflectivity of short-wave ultraviolet light comprises nano alumina powder, intermediate glass powder and silver powder. The nano alumina has small particle size and can be used for artificial gem, analytical reagent, nano catalyst andthe carrier is used for luminescent materials, can greatly improve the luminescent intensity, toughens ceramics and rubber by several times higher than common alumina, particularly improves the compactness, the smoothness, the cold and hot fatigue and the like of the ceramics, and has particularly good ultraviolet reflection performance in common materials; the ratio of the surface atomic number to the total atomic number of the nano silver powder is sharply increased along with the reduction of the particle size, and the specific surface area of the nano silver powder can reach 1-10m2The melting point is lower, the surface of the nano silver particle has stronger local field and quantum size effect, and the nano silver particle has better reflection effect on ultraviolet light waves of 20nm-433 nm; the ceramic material mainly comprises ionic bonds and covalent bonds, the metal material mainly comprises metal bonds, and the metal bonds and the metal materials are hardly infiltrated, so the problem of wettability of the ceramic and the metal materials needs to be considered, in addition, the linear expansion coefficients of the ceramic and the metal materials are generally greatly different, when heat sealing or mechanical connection is adopted, the joint of the ceramic and the metal has large stress residue, the mechanical property of the joint is weakened, and even the joint is damaged and cracked, so the problem of thermal stress relief at the joint needs to be considered. The development of the intermediate glass powder can better solve the problems and provides a material choice with high cost performance for the direct connection or transition connection among ceramic matrix composites, electronic paste, metal and glass, ceramic and metal, and ceramic and glass.
As optimization, the formula of the intermediate glass powder comprises silicon oxide, nano-alumina, borax, sodium carbonate, potassium carbonate and bismuth oxide; the silver powder is nano silver powder. Sodium carbonate is one of the ingredients of commonly used fining agents; the potassium carbonate is added into the glass to play a role in fluxing and improve the transparency and the refractive index of the glass; bismuth oxide has high refractive index, infrared transmission and nonlinear optics; the borax can reduce the expansion coefficient of the material, improve the thermal stability, chemical stability and mechanical strength of the material, and increase the refractive index. The reflectivity of the short-wave ultraviolet light reflection composite material prepared by the formula is up to more than 91%, and the short-wave ultraviolet light reflection composite material has longer service life compared with similar organic materials.
As optimization, the intermediate glass powder formula comprises: by weight, 70-76 parts of silicon oxide, 3-5 parts of nano aluminum oxide, 20-30 parts of borax, 2-5 parts of sodium carbonate, 2-5 parts of potassium carbonate and 3-10 parts of bismuth oxide; the formula of the composite material comprises: the nano-silver powder comprises, by weight, 40-50 parts of nano-alumina powder, 1-5 parts of intermediate glass powder and 1-5 parts of nano-silver powder.
Further, the formula of the intermediate glass powder is as follows: 73 parts of silicon oxide, 4 parts of nano-alumina, 25 parts of borax, 4 parts of sodium carbonate, 4 parts of potassium carbonate and 6 parts of bismuth oxide, and through experimental tests, the performance of the intermediate glass powder selected according to the formula is optimal.
Preferably, the average particle size of the nano alumina is 100 nanometers, the average particle size of the intermediate glass powder is 500 nanometers, the average particle size of the nano silver powder is 100 nanometers, and the smaller particles can improve the reflectivity of the composite material and reduce the sintering temperature so as to obtain the required composition phase.
A preparation process of a composite material with high reflectivity of short-wave ultraviolet light comprises the following steps:
(1) preparing intermediate glass powder;
(2) weighing the following raw materials: nano alumina powder, intermediate glass powder and nano silver powder;
(3) drying the raw materials weighed in the step (2), and mixing by a planetary mill;
(4) detecting the mixing uniformity of the mixture obtained in the step (3);
(5) preparing the mixture obtained in the step (3) into slurry, and carrying out hot air centrifugal spray granulation;
(6) and (5) separating the coarse particles granulated in the step (5) to obtain the composite material with high reflectivity of the short-wave ultraviolet light.
As optimization, the preparation process of the composite material with high reflectivity of short-wave ultraviolet light comprises the following steps:
(1) preparing intermediate glass powder;
a) weighing the following raw materials: 73 parts of silicon oxide, 4 parts of nano-alumina, 25 parts of borax, 4 parts of sodium carbonate, 4 parts of potassium carbonate and 6 parts of bismuth oxide;
b) drying the raw materials weighed in the step a) of the step (1), weighing and mixing the materials, and uniformly mixing the materials by a planetary mill;
c) melting the mixture obtained in step (1) b) to obtain intermediate glass powder:
i. feeding materials, heating for 60min from 20 to 300 ℃, continuously heating for 120min from 300 to 800 ℃, continuously heating for 120min from 800 to 1300 ℃, and continuously heating for 180min from 1300 to 1600 ℃;
iii, preserving the heat for 120min, and homogenizing;
cooling for 30min at 1600-1400 ℃;
v.1400 ℃ molten material is quenched and discharged by water cooling, and is ground and sieved by a 200-mesh sieve after being cooled;
(2) weighing 40-50 parts of nano alumina powder, 1-5 parts of intermediate glass powder and 1-5 parts of nano silver powder;
(3) drying the raw materials weighed in the step (2), and mixing by a planetary mill;
(4) and (4) detecting the mixing uniformity of the mixture obtained in the step (3):
a) sampling the mixture obtained in the step (3), adding a nitric acid solution, putting the mixture into a beaker, heating, and keeping the temperature;
b) stirring the mixture after the heat preservation in the step a) of the step (4), filtering the solution, and weighing the solid matters and the filter paper which are remained after calcination.
(5) Preparing the mixture obtained in the step (3) into slurry, uniformly mixing the slurry, adding 3% of PVA (polyvinyl alcohol) to prepare the slurry, and carrying out hot air centrifugal spray granulation;
(6) and (5) separating the coarse particles granulated in the step (5) by using a vibrating screen of 400 meshes to obtain the composite material with high reflectivity of the short-wave ultraviolet light.
Further optimizing, in the step b) and the step (3) of the step (1), the drying temperature is 150 ℃, the drying mode is infrared drying, the rotating speed of the planetary mill is 70Hz, and the mixing time is 1 h; the PVA is polyvinyl alcohol polymer; in the step a) of the step (4), the nitric acid solution is a 10% nitric acid solution, the heating temperature is 80 ℃, and the heat preservation time is 10 min.
The composite material with high reflectivity of short-wave ultraviolet light can be used for preparing solid-state light-emitting ultraviolet LED light sources.
The composite material with high reflectivity of short-wave ultraviolet light can be used for preparing a reflective cup.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a new inorganic ternary composite material obtained by actual tests, which is a CerMeG material prepared by uniformly mixing and granulating nano alumina powder, an intermediate glass material and nano silver powder, and can simultaneously meet the following conditions:
1. the invention provides an inorganic ternary composite material with high reflectivity for the application of a short-wave ultraviolet LED, and through experimental tests, the effective reflectivity of 272nm ultraviolet light is 91 percent, thereby meeting the requirements of commercial application and being beneficial to the commercial application of the short-wave ultraviolet LED;
2. the invention belongs to a composite inorganic material system, can stand the irradiation of ultraviolet light for a long time without aging and losing efficacy, and has low material composition cost and easy wide popularization;
3. the invention adopts environment-friendly materials and the preparation process does not generate harmful substances.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparing intermediate glass powder: 70 parts of silicon oxide, 3 parts of nano-alumina, 20 parts of borax, 2 parts of sodium carbonate, 2 parts of potassium carbonate and 3 parts of bismuth oxide.
(1) Weighing the following raw materials: 70 parts of silicon oxide, 3 parts of nano-alumina, 20 parts of borax, 2 parts of sodium carbonate, 2 parts of potassium carbonate and 3 parts of bismuth oxide;
(2) drying the raw materials weighed in the step (1), weighing and mixing the materials, and uniformly mixing the materials by a planetary mill;
(3) and (3) melting the mixture obtained in the step (2) to obtain intermediate glass powder.
Example 2
Preparing intermediate glass powder: 73 parts of silicon oxide, 4 parts of nano-alumina, 25 parts of borax, 4 parts of sodium carbonate, 4 parts of potassium carbonate and 6 parts of bismuth oxide.
(1) Weighing the following raw materials: 73 parts of silicon oxide, 4 parts of nano-alumina, 25 parts of borax, 4 parts of sodium carbonate, 4 parts of potassium carbonate and 6 parts of bismuth oxide;
(2) drying the raw materials weighed in the step (1), weighing and mixing the materials, and uniformly mixing the materials by a planetary mill;
(3) and (3) melting the mixture obtained in the step (2) to obtain intermediate glass powder.
Example 3
Preparing intermediate glass powder: 75 parts of silicon oxide, 5 parts of nano-alumina, 30 parts of borax, 5 parts of sodium carbonate, 5 parts of potassium carbonate and 10 parts of bismuth oxide.
(1) Weighing the following raw materials: 75 parts of silicon oxide, 5 parts of nano-alumina, 30 parts of borax, 5 parts of sodium carbonate, 5 parts of potassium carbonate and 10 parts of bismuth oxide;
(2) drying the raw materials weighed in the step (1), weighing and mixing the materials, and uniformly mixing the materials by a planetary mill;
(3) and (3) melting the mixture obtained in the step (2) to obtain intermediate glass powder.
The results of examples 1-3 are shown in Table 1:
TABLE 1 physical Properties of different compositions of intermediate glass materials
Other conditions are basically the same, and the optimal formula of the intermediate glass powder is selected according to the dielectric constant as follows: 73 parts of silicon oxide, 4 parts of nano-alumina, 25 parts of borax, 4 parts of sodium carbonate, 4 parts of potassium carbonate and 6 parts of bismuth oxide, and the physical properties of the material can be ensured to be uniform by selecting the formula and the process.
Example 4:
a composite material with high reflectivity of short-wave ultraviolet light comprises the following processing steps:
(1) preparing intermediate glass powder;
a) weighing the following raw materials: 73 parts of silicon oxide, 4 parts of nano-alumina, 25 parts of borax, 4 parts of sodium carbonate, 4 parts of potassium carbonate and 6 parts of bismuth oxide;
b) drying the raw materials weighed in the step a) of the step (1), weighing and mixing the materials, and uniformly mixing the materials by a planetary mill;
c) melting the mixture obtained in step (1) b) to obtain intermediate glass powder:
i. feeding materials, heating for 60min from 20 to 300 ℃, continuously heating for 120min from 300 to 800 ℃, continuously heating for 120min from 800 to 1300 ℃, and continuously heating for 180min from 1300 to 1600 ℃;
keeping the temperature for 120min, and homogenizing;
cooling for 30min from 1600 to 1400 ℃;
viii cooling the melted material at 1400 ℃, quenching and discharging, cooling, grinding and sieving by a 200-mesh sieve;
(2) weighing 40 parts of nano alumina powder, 1 part of intermediate glass powder and 1 part of nano silver powder;
(3) drying the raw materials weighed in the step (2), and mixing by a planetary mill;
(4) and (4) detecting the mixing uniformity of the mixture obtained in the step (3):
a) sampling the mixture obtained in the step (3), adding a nitric acid solution, putting the mixture into a beaker, heating, and keeping the temperature;
b) stirring the mixture after the heat preservation in the step a) of the step (4), filtering the solution, and weighing the solid matters and the filter paper which are remained after calcination.
(5) Preparing the mixture obtained in the step (3) into slurry, uniformly mixing the slurry, adding 3% of PVA (polyvinyl alcohol) to prepare the slurry, and carrying out hot air centrifugal spray granulation;
(6) and (5) separating the coarse particles granulated in the step (5) by using a vibrating screen of 400 meshes to obtain the composite material with high reflectivity of the short-wave ultraviolet light.
Example 5:
a composite material with high reflectivity of short-wave ultraviolet light comprises the following processing steps:
(1) preparing intermediate glass powder;
a) weighing the following raw materials: 73 parts of silicon oxide, 4 parts of nano-alumina, 25 parts of borax, 4 parts of sodium carbonate, 4 parts of potassium carbonate and 6 parts of bismuth oxide;
b) drying the raw materials weighed in the step a) of the step (1), weighing and mixing the materials, and uniformly mixing the materials by a planetary mill;
c) melting the mixture obtained in step (1) b) to obtain intermediate glass powder:
i. feeding materials, heating for 60min from 20 to 300 ℃, continuously heating for 120min from 300 to 800 ℃, continuously heating for 120min from 800 to 1300 ℃, and continuously heating for 180min from 1300 to 1600 ℃;
keeping the temperature for 120min, and homogenizing;
x, cooling for 30min at the temperature of 1600-1400 ℃;
water-cooling, quenching and discharging the melt material at xi.1400 ℃, and grinding and sieving the melt material by a 200-mesh sieve after cooling;
(2) weighing 45 parts of nano alumina powder, 3 parts of intermediate glass powder and 3 parts of nano silver powder;
(3) drying the raw materials weighed in the step (2), and mixing by a planetary mill;
(4) and (4) detecting the mixing uniformity of the mixture obtained in the step (3):
a) sampling the mixture obtained in the step (3), adding a nitric acid solution, putting the mixture into a beaker, heating, and keeping the temperature;
b) stirring the mixture after the heat preservation in the step a) of the step (4), filtering the solution, and weighing the solid matters and the filter paper which are remained after calcination.
(5) Preparing the mixture obtained in the step (3) into slurry, uniformly mixing the slurry, adding 3% of PVA (polyvinyl alcohol) to prepare the slurry, and carrying out hot air centrifugal spray granulation;
(6) and (5) separating the coarse particles granulated in the step (5) by using a vibrating screen of 400 meshes to obtain the composite material with high reflectivity of the short-wave ultraviolet light.
Example 6:
a composite material with high reflectivity of short-wave ultraviolet light comprises the following processing steps:
(1) preparing intermediate glass powder;
a) weighing the following raw materials: 73 parts of silicon oxide, 4 parts of nano-alumina, 25 parts of borax, 4 parts of sodium carbonate, 4 parts of potassium carbonate and 6 parts of bismuth oxide;
b) drying the raw materials weighed in the step a) of the step (1), weighing and mixing the materials, and uniformly mixing the materials by a planetary mill;
c) melting the mixture obtained in step (1) b) to obtain intermediate glass powder:
i. feeding materials, heating for 60min from 20 to 300 ℃, continuously heating for 120min from 300 to 800 ℃, continuously heating for 120min from 800 to 1300 ℃, and continuously heating for 180min from 1300 to 1600 ℃;
keeping the temperature for 120min, and homogenizing;
cooling for 30min at 1600-1400 deg.C;
water-cooling, quenching and discharging the melt material at the temperature of xiv.1400 ℃, and grinding and sieving the melt material with a 200-mesh sieve after cooling;
(2) weighing 50 parts of nano alumina powder, 5 parts of intermediate glass powder and 5 parts of nano silver powder;
(3) drying the raw materials weighed in the step (2), and mixing by a planetary mill;
(4) and (4) detecting the mixing uniformity of the mixture obtained in the step (3):
a) sampling the mixture obtained in the step (3), adding a nitric acid solution, putting the mixture into a beaker, heating, and keeping the temperature;
b) stirring the mixture after the heat preservation in the step a) of the step (4), filtering the solution, and weighing the solid matters and the filter paper which are remained after calcination.
(5) Preparing the mixture obtained in the step (3) into slurry, uniformly mixing the slurry, adding 3% of PVA (polyvinyl alcohol) to prepare the slurry, and carrying out hot air centrifugal spray granulation;
(6) and (5) separating the coarse particles granulated in the step (5) by using a vibrating screen of 400 meshes to obtain the composite material with high reflectivity of the short-wave ultraviolet light.
Comparative example 1:
45 parts of nano alumina powder, 10 parts of calcium carbonate, 2 parts of barium sulfate, 1 part of sodium oxide, 7 parts of silicon oxide and 2 parts of silver powder.
(1) Weighing the following raw materials: 45 parts of nano alumina powder, 10 parts of calcium carbonate, 2 parts of barium sulfate, 1 part of sodium oxide and 7 parts of silicon oxide, and 2 parts of silver powder;
(2) drying the raw materials weighed in the step (1) (infrared drying at 150 ℃), and fully mixing the raw materials by a planetary mill (rotating speed of 70Hz and time of 1 hour), so that the composite material has uniform performance;
(3) detecting the mixing uniformity of the mixture obtained in the step (2) to ensure the uniform batching;
a) sampling the mixture obtained in the step (2), adding 50mL of 10% nitric acid solution, placing the mixture in a beaker, heating to 80 ℃, and preserving heat for 10 minutes;
b) the solution was stirred well, filtered and the remaining solids and filter paper were calcined and weighed.
If the weight proportion of the nano alumina to the glass is equal to that of the batch, the mixture is uniform. The product performance is uniform, and the reflection effect is good.
(4) Preparing the mixture obtained in the step (2) into slurry, uniformly mixing the slurry and the slurry, adding 3% of PVA (polyvinyl alcohol) to prepare the slurry, and carrying out hot air centrifugal spray granulation;
(5) and (5) separating the coarse particles granulated in the step (4) by using a 400-mesh vibrating screen to obtain the composite material with high reflectivity of the short-wave ultraviolet light.
Detection experiment:
preparation of a test sample: the obtained powders of examples 4 to 6 and comparative example 1 were pressed into test pieces of 10 × 10 mm and 2 mm in thickness, respectively, and formed by the sintering process shown in table 2.
TABLE 2 test piece sintering Process
The test pieces prepared were tested, and the method provided by the present invention is described in detail by the following examples for better clarity, and the reflectivity test method of the short-wave ultraviolet high-reflectivity composite material prepared in the following examples is as follows:
the reflectivity of the sample and the comparison sample to ultraviolet LED light with the wavelength of 272nm and 280nm is tested by using a reflectivity tester of Resonance Limited, Canada.
Table 3 shows the reflectance of short wavelength uv LED light using examples 4-6 of the present invention and comparative example 1 under the same ambient conditions.
TABLE 3 reflectivity of short wave UV LED light
| Example 4 | Example 5 | Example 6 | Comparative example 1 | |
| 272nm reflectivity | 91％ | 93％ | 90％ | 53％ |
| Reflectivity of 280nm | 92％ | 92％ | 91％ | 55％ |
As can be seen from Table 3, the reflectivity of the test piece made of the composite material of the invention to 272nm and 280nm ultraviolet LED light is more than 91%, and the reflectivity of the comparative example is about 53%, which is far smaller than that of the invention.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (7)
1. The composite material with high reflectivity of short-wave ultraviolet light is characterized in that the formula comprises nano alumina powder, intermediate glass powder and silver powder; the intermediate glass powder formula comprises silicon oxide, nano-alumina, borax, sodium carbonate, potassium carbonate and bismuth oxide; the silver powder is nano silver powder;
the intermediate glass powder formula comprises: by weight, 70-76 parts of silicon oxide, 3-5 parts of nano aluminum oxide, 20-30 parts of borax, 2-5 parts of sodium carbonate, 2-5 parts of potassium carbonate and 3-10 parts of bismuth oxide; the composite material formula comprises: the nano-silver powder comprises, by weight, 40-50 parts of nano-alumina powder, 1-5 parts of intermediate glass powder and 1-5 parts of nano-silver powder.
2. The composite material with high reflectivity of short-wave ultraviolet light according to claim 1, wherein the formula of the intermediate glass powder is as follows: 73 parts of silicon oxide, 4 parts of nano-alumina, 25 parts of borax, 4 parts of sodium carbonate, 4 parts of potassium carbonate and 6 parts of bismuth oxide.
3. The composite material with high reflectivity of short-wave ultraviolet light as claimed in claim 2, wherein the average particle size of the nano alumina powder is 100nm, the average particle size of the intermediate glass powder is 500 nm, and the average particle size of the nano silver powder is 100 nm.
4. A preparation process of a composite material with high reflectivity of short-wave ultraviolet light is characterized by comprising the following steps:
(1) preparing intermediate glass powder:
a) weighing the following raw materials: 73 parts of silicon oxide, 4 parts of nano-alumina, 25 parts of borax, 4 parts of sodium carbonate, 4 parts of potassium carbonate and 6 parts of bismuth oxide;
b) drying the raw materials weighed in the step a) of the step (1), weighing and mixing the materials, and uniformly mixing the materials by a planetary mill;
c) melting the mixture obtained in step (1) b) to obtain intermediate glass powder:
i. feeding materials, heating for 60min from 20 to 300 ℃, continuously heating for 120min from 300 to 800 ℃, continuously heating for 120min from 800 to 1300 ℃, and continuously heating for 180min from 1300 to 1600 ℃;
keeping the temperature for 120min, and homogenizing; cooling for 30min after homogenization, wherein the temperature is from 1600 to 1400 ℃; water-cooling, quenching and discharging the melt at 1400 ℃, cooling, grinding and sieving by a 200-mesh sieve to obtain intermediate glass powder;
(2) weighing 40-50 parts of nano alumina powder, 1-5 parts of intermediate glass powder and 1-5 parts of nano silver powder;
(3) drying the raw materials weighed in the step (2), and mixing by a planetary mill;
(4) and (4) detecting the mixing uniformity of the mixture obtained in the step (3):
a) sampling the mixture obtained in the step (3), adding a nitric acid solution, putting the mixture into a beaker, heating, and keeping the temperature;
b) stirring the mixture subjected to heat preservation in the step a) of the step (4), filtering the solution, and calcining the remaining solid matters and filter paper and then weighing;
(5) preparing the mixture obtained in the step (3) into slurry, uniformly mixing the slurry, adding 3% of PVA (polyvinyl alcohol) to prepare the slurry, and carrying out hot air centrifugal spray granulation;
(6) and (5) separating the coarse particles granulated in the step (5) by using a vibrating screen of 400 meshes to obtain the composite material with high reflectivity of the short-wave ultraviolet light.
5. The preparation process of the short-wave ultraviolet high-reflectivity composite material according to claim 4, wherein in the step b) and the step (3) of the step (1), the drying temperature is 150 ℃, the drying mode is infrared drying, the planetary mill rotation speed is 70Hz, and the mixing time is 1 h; the PVA is polyvinyl alcohol polymer; in the step a) of the step (4), the nitric acid solution is a 10% nitric acid solution, the heating temperature is 80 ℃, and the heat preservation time is 10 min.
6. A solid state light emitting ultraviolet LED light source characterized by: a high reflectivity composite of short wavelength ultraviolet light according to any one of claims 1-3.
7. A reflective cup, comprising: a high reflectivity composite of short wavelength ultraviolet light according to any one of claims 1-3.
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| CN202010137601.2A CN111323849B (en) | 2020-03-02 | 2020-03-02 | Composite material with high reflectivity of short-wave ultraviolet light, preparation process and application |
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| CN111323849B true CN111323849B (en) | 2021-11-09 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104193179A (en) * | 2014-07-04 | 2014-12-10 | 江苏博迁新材料有限公司 | Nanoscale glass powder for silicon solar cell front-side silver paste and preparation method thereof |
| CN105716039A (en) * | 2016-04-12 | 2016-06-29 | 杨阳 | Light conversion device and preparation method and application thereof |
| CN105853239A (en) * | 2011-04-21 | 2016-08-17 | 肖特公开股份有限公司 | Glass powder having improved grain size distribution and process for the production thereof |
| CN107393624A (en) * | 2017-06-29 | 2017-11-24 | 广州市尤特新材料有限公司 | A kind of LOW E glass electrocondution slurries and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105853239A (en) * | 2011-04-21 | 2016-08-17 | 肖特公开股份有限公司 | Glass powder having improved grain size distribution and process for the production thereof |
| CN104193179A (en) * | 2014-07-04 | 2014-12-10 | 江苏博迁新材料有限公司 | Nanoscale glass powder for silicon solar cell front-side silver paste and preparation method thereof |
| CN105716039A (en) * | 2016-04-12 | 2016-06-29 | 杨阳 | Light conversion device and preparation method and application thereof |
| CN107393624A (en) * | 2017-06-29 | 2017-11-24 | 广州市尤特新材料有限公司 | A kind of LOW E glass electrocondution slurries and preparation method thereof |
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