CN112029274B - High heat dissipation type LED light source radiator - Google Patents
High heat dissipation type LED light source radiator Download PDFInfo
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- CN112029274B CN112029274B CN202010936780.6A CN202010936780A CN112029274B CN 112029274 B CN112029274 B CN 112029274B CN 202010936780 A CN202010936780 A CN 202010936780A CN 112029274 B CN112029274 B CN 112029274B
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- 230000017525 heat dissipation Effects 0.000 title claims abstract description 19
- 239000007864 aqueous solution Substances 0.000 claims abstract description 190
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 180
- 239000007790 solid phase Substances 0.000 claims abstract description 156
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims abstract description 126
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims abstract description 120
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 107
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 102
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 100
- 238000002791 soaking Methods 0.000 claims abstract description 76
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000000243 solution Substances 0.000 claims abstract description 64
- 239000004471 Glycine Substances 0.000 claims abstract description 60
- 239000000463 material Substances 0.000 claims abstract description 57
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 52
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 52
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 50
- 238000001816 cooling Methods 0.000 claims abstract description 43
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 23
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000011159 matrix material Substances 0.000 claims abstract description 21
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 21
- 229920005989 resin Polymers 0.000 claims abstract description 21
- 239000011347 resin Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 17
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001125 extrusion Methods 0.000 claims abstract description 12
- 238000001746 injection moulding Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 3
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 3
- 239000007822 coupling agent Substances 0.000 claims abstract description 3
- 239000000314 lubricant Substances 0.000 claims abstract description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 96
- 238000001035 drying Methods 0.000 claims description 82
- 239000000203 mixture Substances 0.000 claims description 75
- 239000007788 liquid Substances 0.000 claims description 74
- 238000001914 filtration Methods 0.000 claims description 41
- 238000005406 washing Methods 0.000 claims description 33
- 238000010438 heat treatment Methods 0.000 claims description 32
- 235000006408 oxalic acid Nutrition 0.000 claims description 32
- 239000000843 powder Substances 0.000 claims description 31
- 239000008367 deionised water Substances 0.000 claims description 30
- 229910021641 deionized water Inorganic materials 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 29
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 22
- 238000007873 sieving Methods 0.000 claims description 21
- 238000005303 weighing Methods 0.000 claims description 20
- 229920002292 Nylon 6 Polymers 0.000 claims description 19
- 238000007789 sealing Methods 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims 1
- 239000010452 phosphate Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 2
- ZDYUUBIMAGBMPY-UHFFFAOYSA-N oxalic acid;hydrate Chemical compound O.OC(=O)C(O)=O ZDYUUBIMAGBMPY-UHFFFAOYSA-N 0.000 abstract 1
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 18
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 18
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 11
- 238000004140 cleaning Methods 0.000 description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
- F21V29/00—Protecting lighting devices from thermal damage; Cooling or heating arrangements specially adapted for lighting devices or systems
- F21V29/50—Cooling arrangements
- F21V29/502—Cooling arrangements characterised by the adaptation for cooling of specific components
- F21V29/503—Cooling arrangements characterised by the adaptation for cooling of specific components of light sources
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21Y—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES F21K, F21L, F21S and F21V, RELATING TO THE FORM OR THE KIND OF THE LIGHT SOURCES OR OF THE COLOUR OF THE LIGHT EMITTED
- F21Y2115/00—Light-generating elements of semiconductor light sources
- F21Y2115/10—Light-emitting diodes [LED]
Abstract
The invention discloses a high heat dissipation type LED light source radiator, which is prepared by the following steps: (1) Soaking carbon nanotubes in H 2 O 2 Treating in a mixed aqueous solution of phosphoric acid; (2) Treating zinc oxide powder with oxalic acid water solution, soaking in mixed water solution of copper nitrate and cerium nitrate, and calcining to obtain solid phase A; (3) Soaking the solid phase A in aqueous solution of citric acid and glycine for treatment at 120+/-5 ℃ and adding a nitric acid solution in the process to obtain a solid phase B; (4) Soaking silicon carbide powder in sodium hydroxide to obtain a solid phase C; (5) According to the prior art, mixing and stirring the matrix resin, the carbon nano tube treated in the step (1), the solid phase B, the solid phase C, the antioxidant, the lubricant and the coupling agent, and then carrying out melt extrusion and injection molding on the mixed materials, and cooling to obtain the light source radiator. The radiator prepared by the method has good heat conductivity, can effectively radiate heat generated in the working process of the LED lamp, and prolongs the service life and the use effect of the LED lamp.
Description
Technical Field
The invention relates to the technical field of LED light sources, in particular to a high-heat-dissipation type LED light source radiator.
Background
LED (Light Emitting Diode) A light emitting diode is a solid semiconductor device capable of converting electric energy into light energy, and mainly comprises a chip, electrodes and an optical system. The core of the LED is a semiconductor wafer encapsulated and fixed by epoxy resin, the wafer is fixed on a bracket, two ends of the wafer are LED out through leads, one end of the wafer is used as a negative electrode, and the other end of the wafer is connected with the positive electrode of a power supply. The most important part of the semiconductor wafer is the "P-N junction", the P-N junction material is different, the wavelength of light is different, and the color of light is different accordingly. The study data shows that the luminous flux at the junction temperature of the LED chip is assumed to be 100%; then, with the temperature rise, the light emission amount is only 90% when the chip junction temperature reaches 60 ℃; when the junction temperature is further increased from 100 ℃ to 140 ℃, the light quantity is reduced from 80% to 70%. Therefore, the heat dissipation condition has an important influence on the control of junction temperature and further the light-emitting efficiency of the LED. The heat dissipation materials used at present are basically aluminum alloys, but the heat conductivity of aluminum is not very high, the heat conductivity of gold and silver is relatively high, but the price is too high, the heat conductivity of copper is secondary, but the weight of copper is large, the copper is easy to oxidize, and the price is not low.
Disclosure of Invention
In order to solve the technical problems, the invention provides a high-heat-dissipation type LED light source radiator, which is prepared by the following steps of.
(1) Configuration H 2 O 2 Soaking the carbon nano tube in the mixed aqueous solution of phosphoric acid 2 O 2 And (3) standing for 1-2 h in the mixed aqueous solution of phosphoric acid, filtering after standing, washing the carbon nano tube with deionized water for 2-3 times, and drying for later use.
(2) Preparing a mixed aqueous solution of copper nitrate and cerium nitrate, sieving zinc oxide powder with a 1000-mesh screen, soaking the sieved powder in an oxalic acid aqueous solution for 3-5 min, filtering, soaking the solid phase in the mixed aqueous solution of copper nitrate and cerium nitrate for 1-2 min again, taking out the mixed aqueous solution after soaking, drying the mixed aqueous solution of copper nitrate and cerium nitrate in an environment of 90+/-5 ℃, soaking the mixed aqueous solution of copper nitrate and cerium nitrate again for 1-2 min after drying, taking out the mixed aqueous solution of copper nitrate and cerium nitrate, drying and weighing the mixed aqueous solution, and repeating the processes of soaking, drying and weighing until the solid phase mass is increased by more than 8% compared with that before the mixed aqueous solution of copper nitrate and cerium nitrate is not soaked; and then placing the solid phase in an environment of 420+/-20 ℃ for calcination for more than 1 hour, and air-cooling to normal temperature to obtain a solid phase A.
(3) Preparing aqueous solutions of citric acid and glycine, soaking the solid phase A in the aqueous solutions of citric acid and glycine to form a mixture, placing the mixture into a reaction kettle, sealing the kettle body, heating to 120+/-5 ℃, preserving heat for 10min at the temperature, adding a nitric acid solution into the mixture, continuously preserving heat for 20-30 min, air-cooling the mixture along with the reaction kettle to normal temperature after the heat preservation is finished, taking out the mixture, filtering, washing the solid phase with deionized water for 3-4 times, and drying to obtain a solid phase B.
(4) Sieving silicon carbide powder with a 1000-mesh screen, washing the sieved powder with acetone for 2-3 times, drying, soaking in a sodium hydroxide aqueous solution, heating the solution to 70-80 ℃ for 3-4 hours, air-cooling the solution to normal temperature after heating, filtering, washing the solid phase with deionized water for 3-4 times, and drying to obtain a solid phase C.
(5) Mixing and stirring the matrix resin, the carbon nano tube treated in the step (1), the solid phase B, the solid phase C, the antioxidant, the lubricant and the coupling agent, and carrying out melt extrusion and injection molding on the mixed materials, and cooling to obtain the light source radiator.
Further, the H 2 O 2 In a mixed aqueous solution of phosphoric acid, H 2 O 2 The mass percentage of the phosphoric acid is 10 percent, the mass percentage of the phosphoric acid is 5 to 8 percent, and the balance is water; the carbon nano tube is soaked in H 2 O 2 The mass ratio of the feed liquid in the mixed aqueous solution of phosphoric acid is feed/liquid=1:8-10.
Further, in the mixed aqueous solution of copper nitrate and cerium nitrate, the concentration of copper nitrate is 6-16 g/100mL, the concentration of cerium nitrate is 3-7 g/100mL, and the balance is water; the mass percentage of oxalic acid in the oxalic acid aqueous solution is 6% -8%, and the balance is water; the mass ratio of the material to the liquid of the water solution of the sieved powder soaked in oxalic acid is material/liquid=1:8-10, and the mass ratio of the material to the liquid of the mixed water solution of the solid phase soaked in the copper nitrate and the cerium nitrate is material/liquid=1:6-7.
Further, in the aqueous solution of the citric acid and the glycine, the concentration of the citric acid is 1-4 g/100mL, the concentration of the glycine is 0.8-1.6 g/100mL, and the balance is water; the mass ratio of the solid phase A to the material liquid in the aqueous solution of the citric acid and the glycine is (1:5) - (6), the mass percentage of the solute in the nitric acid solution is (6) - (10%), the balance is water, and the adding amount of the nitric acid solution/the amount of the aqueous solution of the citric acid and the glycine in the reaction kettle is (5) - (9 mL)/100 mL.
Further, the mass percentage of the solute in the sodium hydroxide aqueous solution is 10% -20%, and the mass ratio of the silicon carbide powder to the feed liquid of the sodium hydroxide aqueous solution is (material/liquid=1:5-6).
The invention has the beneficial effects that: the radiator prepared by the method has good heat conductivity, can effectively radiate heat generated in the working process of the LED lamp, and prolongs the service life and the use effect of the LED lamp.
Detailed Description
The invention is further illustrated below with reference to examples.
Example 1.
A high heat dissipation type LED light source radiator is prepared by the following steps.
(1) Configuration H 2 O 2 A mixed aqueous solution of phosphoric acid, said H 2 O 2 In a mixed aqueous solution of phosphoric acid, H 2 O 2 10 mass percent of phosphoric acid, 5 mass percent of water and the balance of water; soaking the carbon nano tube in the H 2 O 2 The carbon nano tube is soaked in H in the mixed water solution of phosphoric acid 2 O 2 The mass ratio of the feed liquid in the mixed water solution of phosphoric acid is feed/liquid=1:8; standing for 1h, filtering after standing, washing the carbon nano tube with deionized water for 3 times, and drying at 80 ℃ for later use.
(2) Preparing a mixed aqueous solution of copper nitrate and cerium nitrate, wherein the concentration of copper nitrate in the mixed aqueous solution of copper nitrate and cerium nitrate is 6g/100mL, the concentration of cerium nitrate is 3g/100mL, and the balance is water; sieving zinc oxide powder with a 1000-mesh sieve, wherein the sieved powder is firstly soaked in an oxalic acid aqueous solution (the mass percentage of oxalic acid is 6%, and the rest is water) for 3min, and the mass ratio of the material liquid of the sieved powder soaked in the oxalic acid aqueous solution is (material/liquid=1:8); then filtering, and soaking the solid phase in the mixed aqueous solution of copper nitrate and cerium nitrate for 1min, wherein the mass ratio of the solid phase to the mixed aqueous solution of copper nitrate and cerium nitrate is (material/liquid=1:6); taking out after the soaking is finished, drying in the environment of 90+/-5 ℃, soaking in the mixed aqueous solution of the copper nitrate and the cerium nitrate again for 1min after the drying, taking out, drying and weighing, and repeating the soaking, drying and weighing processes until the solid phase mass is increased by 8.26% compared with that before the mixed aqueous solution of the copper nitrate and the cerium nitrate is not soaked; and then placing the solid phase in an environment of 420+/-20 ℃ for calcination for 1h, and air-cooling to normal temperature to obtain a solid phase A.
(3) Preparing aqueous solutions of citric acid and glycine, wherein the concentration of the citric acid in the aqueous solutions of the citric acid and the glycine is 1g/100mL, the concentration of the glycine is 0.8g/100mL, and the balance is water; soaking the solid phase A in the aqueous solution of the citric acid and the glycine to form a mixture, wherein the mass ratio of the solid phase A to the aqueous solution of the citric acid and the glycine in the mixture is (material/liquid=1:5); placing the mixture into a reaction kettle, sealing the kettle body, heating to 120+/-5 ℃, preserving heat at the temperature for 10min, and then adding a nitric acid solution (the mass percent of solute is 6% and the balance is water) into the mixture, wherein the adding amount of the nitric acid solution/the amount of the citric acid and glycine aqueous solution in the reaction kettle is 5mL/100mL; continuing to keep the temperature for 20min, air cooling the mixture to normal temperature along with the reaction kettle after the temperature is kept, taking out the mixture, filtering, washing the solid phase with deionized water for 3 times, and drying at 80 ℃ to obtain a solid phase B.
(4) Sieving silicon carbide powder with a 1000-mesh sieve, cleaning the sieved powder with acetone for 3 times, drying, and soaking in a sodium hydroxide aqueous solution, wherein the mass percentage of solute in the sodium hydroxide aqueous solution is 10%, and the mass ratio of the silicon carbide powder to the sodium hydroxide aqueous solution is (material/liquid=1:5); heating the solution to 75+/-5 ℃ and preserving heat for 3 hours, cooling the solution to normal temperature by air after heating, filtering, washing the solid phase with deionized water for 3 times, and drying at 80 ℃ to obtain a solid phase C.
(5) Mixing and stirring polyamide-6 matrix resin, the carbon nano tube treated in the step (1), the solid phase B, the solid phase C, an antioxidant 1010, barium stearate and gamma-aminopropyl triethoxysilane, wherein the components in the mixture are as follows in parts by weight: 60 parts of polyamide-6 matrix resin, 5 parts of carbon nano tubes treated in the step (1), 3 parts of solid phase B, 3 parts of solid phase C, 1.5 parts of antioxidant 1010, 0.6 part of barium stearate and 0.6 part of gamma-aminopropyl triethoxysilane, and carrying out melt extrusion, injection molding and cooling on the mixture to obtain the light source radiator.
Example 2.
A high heat dissipation type LED light source radiator is prepared by the following steps.
(1) Configuration H 2 O 2 A mixed aqueous solution of phosphoric acid, said H 2 O 2 In a mixed aqueous solution of phosphoric acid, H 2 O 2 10 mass percent of phosphoric acid, 6 mass percent of water and the balance of water; soaking the carbon nano tube in the H 2 O 2 The carbon nano tube is soaked in H in the mixed water solution of phosphoric acid 2 O 2 The mass ratio of the feed liquid in the mixed water solution of phosphoric acid is feed/liquid=1:8; standing for 1h, filtering after standing, washing the carbon nano tube with deionized water for 3 times, and drying at 80 ℃ for later use.
(2) Preparing a mixed aqueous solution of copper nitrate and cerium nitrate, wherein the concentration of the copper nitrate is 9g/100mL, the concentration of the cerium nitrate is 5g/100mL, and the balance is water; sieving zinc oxide powder with a 1000-mesh sieve, wherein the sieved powder is firstly soaked in an oxalic acid aqueous solution (the mass percentage of oxalic acid is 7%, and the rest is water) for 3min, and the mass ratio of the material liquid of the sieved powder soaked in the oxalic acid aqueous solution is (material/liquid=1:8); then filtering, and soaking the solid phase in the mixed aqueous solution of copper nitrate and cerium nitrate for 1min, wherein the mass ratio of the solid phase to the mixed aqueous solution of copper nitrate and cerium nitrate is (material/liquid=1:6); taking out after the soaking is finished, drying in the environment of 90+/-5 ℃, soaking in the mixed aqueous solution of the copper nitrate and the cerium nitrate again for 1min after the drying, taking out, drying and weighing, and repeating the soaking, drying and weighing processes until the solid phase mass is increased by 8.09% compared with that before the mixed aqueous solution of the copper nitrate and the cerium nitrate is not soaked; and then placing the solid phase in an environment of 420+/-20 ℃ for calcination for 1h, and air-cooling to normal temperature to obtain a solid phase A.
(3) Preparing aqueous solutions of citric acid and glycine, wherein the concentration of the citric acid in the aqueous solutions of the citric acid and the glycine is 2g/100mL, the concentration of the glycine is 1.1g/100mL, and the balance is water; soaking the solid phase A in the aqueous solution of the citric acid and the glycine to form a mixture, wherein the mass ratio of the solid phase A to the aqueous solution of the citric acid and the glycine in the mixture is (material/liquid=1:5); placing the mixture into a reaction kettle, sealing the kettle body, heating to 120+/-5 ℃, preserving heat at the temperature for 10min, and then adding a nitric acid solution (the mass percent of solute is 8% and the balance is water) into the mixture, wherein the adding amount of the nitric acid solution/the amount of the citric acid and glycine aqueous solution in the reaction kettle is 7mL/100mL; continuing to keep the temperature for 20min, air cooling the mixture to normal temperature along with the reaction kettle after the temperature is kept, taking out the mixture, filtering, washing the solid phase with deionized water for 3 times, and drying at 80 ℃ to obtain a solid phase B.
(4) Sieving silicon carbide powder with a 1000-mesh sieve, cleaning the sieved powder with acetone for 3 times, drying, and soaking in a sodium hydroxide aqueous solution, wherein the mass percentage of solute in the sodium hydroxide aqueous solution is 10%, and the mass ratio of the silicon carbide powder to the sodium hydroxide aqueous solution is (material/liquid=1:5); heating the solution to 75+/-5 ℃ and preserving heat for 3 hours, cooling the solution to normal temperature by air after heating, filtering, washing the solid phase with deionized water for 3 times, and drying at 80 ℃ to obtain a solid phase C.
(5) Mixing and stirring polyamide-6 matrix resin, the carbon nano tube treated in the step (1), the solid phase B, the solid phase C, an antioxidant 1010, barium stearate and gamma-aminopropyl triethoxysilane, wherein the components in the mixture are as follows in parts by weight: 60 parts of polyamide-6 matrix resin, 5 parts of carbon nano tubes treated in the step (1), 3 parts of solid phase B, 3 parts of solid phase C, 1.5 parts of antioxidant 1010, 0.6 part of barium stearate and 0.6 part of gamma-aminopropyl triethoxysilane, and carrying out melt extrusion, injection molding and cooling on the mixture to obtain the light source radiator.
Example 3.
A high heat dissipation type LED light source radiator is prepared by the following steps.
(1) Configuration H 2 O 2 A mixed aqueous solution of phosphoric acid, said H 2 O 2 In a mixed aqueous solution of phosphoric acid, H 2 O 2 10 mass percent of phosphoric acid, 7 mass percent of water and the balance of water; soaking the carbon nano tube in the H 2 O 2 The carbon nano tube is soaked in H in the mixed water solution of phosphoric acid 2 O 2 The mass ratio of the feed liquid in the mixed water solution of phosphoric acid is feed/liquid=1:8; standing for 1h, filtering after standing, washing the carbon nano tube with deionized water for 3 times at 80 DEG CAnd (5) drying for standby.
(2) Preparing a mixed aqueous solution of copper nitrate and cerium nitrate, wherein the concentration of the copper nitrate is 12g/100mL, the concentration of the cerium nitrate is 6g/100mL, and the balance is water; sieving zinc oxide powder with a 1000-mesh sieve, wherein the sieved powder is firstly soaked in an oxalic acid aqueous solution (the mass percentage of oxalic acid is 7%, and the rest is water) for 3min, and the mass ratio of the material liquid of the sieved powder soaked in the oxalic acid aqueous solution is (material/liquid=1:8); then filtering, and soaking the solid phase in the mixed aqueous solution of copper nitrate and cerium nitrate for 1min, wherein the mass ratio of the solid phase to the mixed aqueous solution of copper nitrate and cerium nitrate is (material/liquid=1:6); taking out after the soaking is finished, drying in the environment of 90+/-5 ℃, soaking in the mixed aqueous solution of the copper nitrate and the cerium nitrate again for 1min after the drying, taking out, drying and weighing, and repeating the soaking, drying and weighing processes until the solid phase mass is increased by 8.04% compared with that before the mixed aqueous solution of the copper nitrate and the cerium nitrate is not soaked; and then placing the solid phase in an environment of 420+/-20 ℃ for calcination for 1h, and air-cooling to normal temperature to obtain a solid phase A.
(3) Preparing aqueous solutions of citric acid and glycine, wherein the concentration of the citric acid in the aqueous solutions of the citric acid and the glycine is 3g/100mL, the concentration of the glycine is 1.4g/100mL, and the balance is water; soaking the solid phase A in the aqueous solution of the citric acid and the glycine to form a mixture, wherein the mass ratio of the solid phase A to the aqueous solution of the citric acid and the glycine in the mixture is (material/liquid=1:5); placing the mixture into a reaction kettle, sealing the kettle body, heating to 120+/-5 ℃, preserving heat at the temperature for 10min, and then adding a nitric acid solution (the mass percent of solute is 8% and the balance is water) into the mixture, wherein the adding amount of the nitric acid solution/the amount of the citric acid and glycine aqueous solution in the reaction kettle is 8mL/100mL; continuing to keep the temperature for 20min, air cooling the mixture to normal temperature along with the reaction kettle after the temperature is kept, taking out the mixture, filtering, washing the solid phase with deionized water for 3 times, and drying at 80 ℃ to obtain a solid phase B.
(4) Sieving silicon carbide powder with a 1000-mesh sieve, cleaning the sieved powder with acetone for 3 times, drying, and soaking in a sodium hydroxide aqueous solution, wherein the mass percentage of solute in the sodium hydroxide aqueous solution is 10%, and the mass ratio of the silicon carbide powder to the sodium hydroxide aqueous solution is (material/liquid=1:5); heating the solution to 75+/-5 ℃ and preserving heat for 3 hours, cooling the solution to normal temperature by air after heating, filtering, washing the solid phase with deionized water for 3 times, and drying at 80 ℃ to obtain a solid phase C.
(5) Mixing and stirring polyamide-6 matrix resin, the carbon nano tube treated in the step (1), the solid phase B, the solid phase C, an antioxidant 1010, barium stearate and gamma-aminopropyl triethoxysilane, wherein the components in the mixture are as follows in parts by weight: 60 parts of polyamide-6 matrix resin, 5 parts of carbon nano tubes treated in the step (1), 3 parts of solid phase B, 3 parts of solid phase C, 1.5 parts of antioxidant 1010, 0.6 part of barium stearate and 0.6 part of gamma-aminopropyl triethoxysilane, and carrying out melt extrusion, injection molding and cooling on the mixture to obtain the light source radiator.
Example 4.
A high heat dissipation type LED light source radiator is prepared by the following steps.
(1) Configuration H 2 O 2 A mixed aqueous solution of phosphoric acid, said H 2 O 2 In a mixed aqueous solution of phosphoric acid, H 2 O 2 10 mass percent of phosphoric acid, 8 mass percent of water and the balance of water; soaking the carbon nano tube in the H 2 O 2 The carbon nano tube is soaked in H in the mixed water solution of phosphoric acid 2 O 2 The mass ratio of the feed liquid in the mixed water solution of phosphoric acid is feed/liquid=1:8; standing for 1h, filtering after standing, washing the carbon nano tube with deionized water for 3 times, and drying at 80 ℃ for later use.
(2) Preparing a mixed aqueous solution of copper nitrate and cerium nitrate, wherein the concentration of the copper nitrate in the mixed aqueous solution of copper nitrate and cerium nitrate is 16g/100mL, the concentration of the cerium nitrate is 7g/100mL, and the balance is water; sieving zinc oxide powder with a 1000-mesh sieve, wherein the sieved powder is firstly soaked in an oxalic acid aqueous solution (the mass percentage of oxalic acid is 8%, and the rest is water) for 3min, and the mass ratio of the material liquid of the sieved powder soaked in the oxalic acid aqueous solution is (material/liquid=1:8); then filtering, and soaking the solid phase in the mixed aqueous solution of copper nitrate and cerium nitrate for 1min, wherein the mass ratio of the solid phase to the mixed aqueous solution of copper nitrate and cerium nitrate is (material/liquid=1:6); taking out after the soaking is finished, drying in the environment of 90+/-5 ℃, soaking in the mixed aqueous solution of the copper nitrate and the cerium nitrate again for 1min after the drying, taking out, drying and weighing, and repeating the soaking, drying and weighing processes until the solid phase mass is increased by 8.21% compared with that before the mixed aqueous solution of the copper nitrate and the cerium nitrate is not soaked; and then placing the solid phase in an environment of 420+/-20 ℃ for calcination for 1h, and air-cooling to normal temperature to obtain a solid phase A.
(3) Preparing aqueous solutions of citric acid and glycine, wherein the concentration of the citric acid in the aqueous solutions of the citric acid and the glycine is 4g/100mL, the concentration of the glycine is 1.6g/100mL, and the balance is water; soaking the solid phase A in the aqueous solution of the citric acid and the glycine to form a mixture, wherein the mass ratio of the solid phase A to the aqueous solution of the citric acid and the glycine in the mixture is (material/liquid=1:5); placing the mixture into a reaction kettle, sealing the kettle body, heating to 120+/-5 ℃, preserving heat at the temperature for 10min, and then adding a nitric acid solution (the mass percent of solute is 10% and the balance is water) into the mixture, wherein the adding amount of the nitric acid solution/the amount of the citric acid and glycine aqueous solution in the reaction kettle is 9mL/100mL; continuing to keep the temperature for 20min, air cooling the mixture to normal temperature along with the reaction kettle after the temperature is kept, taking out the mixture, filtering, washing the solid phase with deionized water for 3 times, and drying at 80 ℃ to obtain a solid phase B.
(4) Sieving silicon carbide powder with a 1000-mesh sieve, cleaning the sieved powder with acetone for 3 times, drying, and soaking in a sodium hydroxide aqueous solution, wherein the mass percentage of solute in the sodium hydroxide aqueous solution is 10%, and the mass ratio of the silicon carbide powder to the sodium hydroxide aqueous solution is (material/liquid=1:5); heating the solution to 75+/-5 ℃ and preserving heat for 3 hours, cooling the solution to normal temperature by air after heating, filtering, washing the solid phase with deionized water for 3 times, and drying at 80 ℃ to obtain a solid phase C.
(5) Mixing and stirring polyamide-6 matrix resin, the carbon nano tube treated in the step (1), the solid phase B, the solid phase C, an antioxidant 1010, barium stearate and gamma-aminopropyl triethoxysilane, wherein the components in the mixture are as follows in parts by weight: 60 parts of polyamide-6 matrix resin, 5 parts of carbon nano tubes treated in the step (1), 3 parts of solid phase B, 3 parts of solid phase C, 1.5 parts of antioxidant 1010, 0.6 part of barium stearate and 0.6 part of gamma-aminopropyl triethoxysilane, and carrying out melt extrusion, injection molding and cooling on the mixture to obtain the light source radiator.
Comparative example 1.
A high heat dissipation type LED light source radiator is prepared by the following steps.
(1) Preparing a mixed aqueous solution of copper nitrate and cerium nitrate, wherein the concentration of the copper nitrate is 9g/100mL, the concentration of the cerium nitrate is 5g/100mL, and the balance is water; sieving zinc oxide powder with a 1000-mesh sieve, wherein the sieved powder is firstly soaked in an oxalic acid aqueous solution (the mass percentage of oxalic acid is 7%, and the rest is water) for 3min, and the mass ratio of the material liquid of the sieved powder soaked in the oxalic acid aqueous solution is (material/liquid=1:8); then filtering, and soaking the solid phase in the mixed aqueous solution of copper nitrate and cerium nitrate for 1min, wherein the mass ratio of the solid phase to the mixed aqueous solution of copper nitrate and cerium nitrate is (material/liquid=1:6); taking out after the soaking is finished, drying in the environment of 90+/-5 ℃, soaking in the mixed aqueous solution of the copper nitrate and the cerium nitrate again for 1min after the drying, taking out, drying and weighing, and repeating the soaking, drying and weighing processes until the solid phase mass is increased by 8.13% compared with that before the mixed aqueous solution of the copper nitrate and the cerium nitrate is not soaked; and then placing the solid phase in an environment of 420+/-20 ℃ for calcination for 1h, and air-cooling to normal temperature to obtain a solid phase A.
(2) Preparing aqueous solutions of citric acid and glycine, wherein the concentration of the citric acid in the aqueous solutions of the citric acid and the glycine is 2g/100mL, the concentration of the glycine is 1.1g/100mL, and the balance is water; soaking the solid phase A in the aqueous solution of the citric acid and the glycine to form a mixture, wherein the mass ratio of the solid phase A to the aqueous solution of the citric acid and the glycine in the mixture is (material/liquid=1:5); placing the mixture into a reaction kettle, sealing the kettle body, heating to 120+/-5 ℃, preserving heat at the temperature for 10min, and then adding a nitric acid solution (the mass percent of solute is 8% and the balance is water) into the mixture, wherein the adding amount of the nitric acid solution/the amount of the citric acid and glycine aqueous solution in the reaction kettle is 7mL/100mL; continuing to keep the temperature for 20min, air cooling the mixture to normal temperature along with the reaction kettle after the temperature is kept, taking out the mixture, filtering, washing the solid phase with deionized water for 3 times, and drying at 80 ℃ to obtain a solid phase B.
(3) Sieving silicon carbide powder with a 1000-mesh sieve, cleaning the sieved powder with acetone for 3 times, drying, and soaking in a sodium hydroxide aqueous solution, wherein the mass percentage of solute in the sodium hydroxide aqueous solution is 10%, and the mass ratio of the silicon carbide powder to the sodium hydroxide aqueous solution is (material/liquid=1:5); heating the solution to 75+/-5 ℃ and preserving heat for 3 hours, cooling the solution to normal temperature by air after heating, filtering, washing the solid phase with deionized water for 3 times, and drying at 80 ℃ to obtain a solid phase C.
(4) Mixing and stirring polyamide-6 matrix resin, carbon nano tubes, the solid phase B, the solid phase C, an antioxidant 1010, barium stearate and gamma-aminopropyl triethoxysilane, wherein the components in the mixture are as follows in parts by weight: 60 parts of polyamide-6 matrix resin, 5 parts of carbon nano tubes, 3 parts of solid phase B, 3 parts of solid phase C, 1.5 parts of antioxidant 1010, 0.6 part of barium stearate and 0.6 part of gamma-aminopropyl triethoxysilane, and carrying out melt extrusion, injection molding and cooling on the mixture to obtain the light source radiator of the comparative example.
Comparative example 2.
A high heat dissipation type LED light source radiator is prepared by the following steps.
(1) Configuration H 2 O 2 A mixed aqueous solution of phosphoric acid, said H 2 O 2 In a mixed aqueous solution of phosphoric acid, H 2 O 2 10 mass percent of phosphoric acid, 6 mass percent of water and the balance of water; soaking the carbon nano tube in the H 2 O 2 The carbon nano tube is soaked in H in the mixed water solution of phosphoric acid 2 O 2 The mass ratio of the feed liquid in the mixed water solution of phosphoric acid is feed/liquid=1:8; standing for 1h, filtering after standing, washing the carbon nano tube with deionized water for 3 times, and drying at 80 ℃ for later use.
(2) Preparing aqueous solutions of citric acid and glycine, wherein the concentration of the citric acid in the aqueous solutions of the citric acid and the glycine is 2g/100mL, the concentration of the glycine is 1.1g/100mL, and the balance is water; immersing zinc oxide powder passing through a 1000-mesh screen in the aqueous solution of citric acid and glycine to form a mixture, wherein the mass ratio of the zinc oxide powder to the aqueous solution of citric acid and glycine in the mixture is (material/liquid=1:5); placing the mixture into a reaction kettle, sealing the kettle body, heating to 120+/-5 ℃, preserving heat at the temperature for 10min, and then adding a nitric acid solution (the mass percent of solute is 8% and the balance is water) into the mixture, wherein the adding amount of the nitric acid solution/the amount of the citric acid and glycine aqueous solution in the reaction kettle is 7mL/100mL; continuing to keep the temperature for 20min, air cooling the mixture to normal temperature along with the reaction kettle after the temperature is kept, taking out the mixture, filtering, washing the solid phase with deionized water for 3 times, and drying at 80 ℃ to obtain a solid phase B.
(3) Sieving silicon carbide powder with a 1000-mesh sieve, cleaning the sieved powder with acetone for 3 times, drying, and soaking in a sodium hydroxide aqueous solution, wherein the mass percentage of solute in the sodium hydroxide aqueous solution is 10%, and the mass ratio of the silicon carbide powder to the sodium hydroxide aqueous solution is (material/liquid=1:5); heating the solution to 75+/-5 ℃ and preserving heat for 3 hours, cooling the solution to normal temperature by air after heating, filtering, washing the solid phase with deionized water for 3 times, and drying at 80 ℃ to obtain a solid phase C.
(4) Mixing and stirring polyamide-6 matrix resin, the carbon nano tube treated in the step (1), the solid phase B, the solid phase C, an antioxidant 1010, barium stearate and gamma-aminopropyl triethoxysilane, wherein the components in the mixture are as follows in parts by weight: 60 parts of polyamide-6 matrix resin, 5 parts of carbon nano tubes treated in the step (1), 3 parts of solid phase B, 3 parts of solid phase C, 1.5 parts of antioxidant 1010, 0.6 part of barium stearate and 0.6 part of gamma-aminopropyl triethoxysilane, and carrying out melt extrusion, injection molding and cooling on the mixture to obtain the light source radiator of the comparative example.
Comparative example 3.
A high heat dissipation type LED light source radiator is prepared by the following steps.
(1) Configuration H 2 O 2 A mixed aqueous solution of phosphoric acid, said H 2 O 2 In a mixed aqueous solution of phosphoric acid, H 2 O 2 10 mass percent of phosphoric acid, 6 mass percent of water and the balance of water; soaking the carbon nano tube in the H 2 O 2 Phosphorus (P)The carbon nano tube is soaked in H in the mixed aqueous solution of acid 2 O 2 The mass ratio of the feed liquid in the mixed water solution of phosphoric acid is feed/liquid=1:8; standing for 1h, filtering after standing, washing the carbon nano tube with deionized water for 3 times, and drying at 80 ℃ for later use.
(2) Preparing a mixed aqueous solution of copper nitrate and cerium nitrate, wherein the concentration of the copper nitrate is 9g/100mL, the concentration of the cerium nitrate is 5g/100mL, and the balance is water; sieving zinc oxide powder with a 1000-mesh sieve, wherein the sieved powder is firstly soaked in an oxalic acid aqueous solution (the mass percentage of oxalic acid is 7%, and the rest is water) for 3min, and the mass ratio of the material liquid of the sieved powder soaked in the oxalic acid aqueous solution is (material/liquid=1:8); then filtering, and soaking the solid phase in the mixed aqueous solution of copper nitrate and cerium nitrate for 1min, wherein the mass ratio of the solid phase to the mixed aqueous solution of copper nitrate and cerium nitrate is (material/liquid=1:6); taking out after the soaking is finished, drying in the environment of 90+/-5 ℃, soaking in the mixed aqueous solution of the copper nitrate and the cerium nitrate again for 1min after the drying, taking out, drying and weighing, and repeating the soaking, drying and weighing processes until the solid phase mass is increased by 8.16% compared with that before the mixed aqueous solution of the copper nitrate and the cerium nitrate is not soaked; and then placing the solid phase in an environment of 420+/-20 ℃ for calcination for 1h, and air-cooling to normal temperature to obtain a solid phase A.
(3) Sieving silicon carbide powder with a 1000-mesh sieve, cleaning the sieved powder with acetone for 3 times, drying, and soaking in a sodium hydroxide aqueous solution, wherein the mass percentage of solute in the sodium hydroxide aqueous solution is 10%, and the mass ratio of the silicon carbide powder to the sodium hydroxide aqueous solution is (material/liquid=1:5); heating the solution to 75+/-5 ℃ and preserving heat for 3 hours, cooling the solution to normal temperature by air after heating, filtering, washing the solid phase with deionized water for 3 times, and drying at 80 ℃ to obtain a solid phase C.
(4) Mixing and stirring polyamide-6 matrix resin, the carbon nano tube treated in the step (1), the solid phase A, the solid phase C, an antioxidant 1010, barium stearate and gamma-aminopropyl triethoxysilane, wherein the components in the mixture are as follows in parts by weight: 60 parts of polyamide-6 matrix resin, 5 parts of carbon nano tubes treated in the step (1), 3 parts of solid phase A, 3 parts of solid phase C, 1.5 parts of antioxidant 1010, 0.6 part of barium stearate and 0.6 part of gamma-aminopropyl triethoxysilane, and carrying out melt extrusion, injection molding and cooling on the mixture to obtain the light source radiator of the comparative example.
Comparative example 4.
A high heat dissipation type LED light source radiator is prepared by the following steps.
(1) Configuration H 2 O 2 A mixed aqueous solution of phosphoric acid, said H 2 O 2 In a mixed aqueous solution of phosphoric acid, H 2 O 2 10 mass percent of phosphoric acid, 6 mass percent of water and the balance of water; soaking the carbon nano tube in the H 2 O 2 The carbon nano tube is soaked in H in the mixed water solution of phosphoric acid 2 O 2 The mass ratio of the feed liquid in the mixed water solution of phosphoric acid is feed/liquid=1:8; standing for 1h, filtering after standing, washing the carbon nano tube with deionized water for 3 times, and drying at 80 ℃ for later use.
(2) Preparing an aqueous solution of copper nitrate, wherein the concentration of the copper nitrate in the aqueous solution of copper nitrate is 9g/100mL, and the balance is water; sieving zinc oxide powder with a 1000-mesh sieve, wherein the sieved powder is firstly soaked in an oxalic acid aqueous solution (the mass percentage of oxalic acid is 7%, and the rest is water) for 3min, and the mass ratio of the material liquid of the sieved powder soaked in the oxalic acid aqueous solution is (material/liquid=1:8); then filtering, and soaking the solid phase in the aqueous solution of copper nitrate for 1min again, wherein the mass ratio of the solid phase to the aqueous solution of copper nitrate is (material/liquid=1:6); taking out after the soaking is finished, drying in the environment of 90+/-5 ℃, soaking in the aqueous solution of copper nitrate again for 1min after the drying, taking out, drying and weighing, and repeating the soaking, drying and weighing processes until the solid phase mass is increased by 8.02% compared with that before the copper nitrate is not soaked in the aqueous solution; and then placing the solid phase in an environment of 420+/-20 ℃ for calcination for 1h, and air-cooling to normal temperature to obtain a solid phase A.
(3) Preparing aqueous solutions of citric acid and glycine, wherein the concentration of the citric acid in the aqueous solutions of the citric acid and the glycine is 2g/100mL, the concentration of the glycine is 1.1g/100mL, and the balance is water; soaking the solid phase A in the aqueous solution of the citric acid and the glycine to form a mixture, wherein the mass ratio of the solid phase A to the aqueous solution of the citric acid and the glycine in the mixture is (material/liquid=1:5); placing the mixture into a reaction kettle, sealing the kettle body, heating to 120+/-5 ℃, preserving heat at the temperature for 10min, and then adding a nitric acid solution (the mass percent of solute is 8% and the balance is water) into the mixture, wherein the adding amount of the nitric acid solution/the amount of the citric acid and glycine aqueous solution in the reaction kettle is 7mL/100mL; continuing to keep the temperature for 20min, air cooling the mixture to normal temperature along with the reaction kettle after the temperature is kept, taking out the mixture, filtering, washing the solid phase with deionized water for 3 times, and drying at 80 ℃ to obtain a solid phase B.
(4) Sieving silicon carbide powder with a 1000-mesh sieve, cleaning the sieved powder with acetone for 3 times, drying, and soaking in a sodium hydroxide aqueous solution, wherein the mass percentage of solute in the sodium hydroxide aqueous solution is 10%, and the mass ratio of the silicon carbide powder to the sodium hydroxide aqueous solution is (material/liquid=1:5); heating the solution to 75+/-5 ℃ and preserving heat for 3 hours, cooling the solution to normal temperature by air after heating, filtering, washing the solid phase with deionized water for 3 times, and drying at 80 ℃ to obtain a solid phase C.
(5) Mixing and stirring polyamide-6 matrix resin, the carbon nano tube treated in the step (1), the solid phase B, the solid phase C, an antioxidant 1010, barium stearate and gamma-aminopropyl triethoxysilane, wherein the components in the mixture are as follows in parts by weight: 60 parts of polyamide-6 matrix resin, 5 parts of carbon nano tubes treated in the step (1), 3 parts of solid phase B, 3 parts of solid phase C, 1.5 parts of antioxidant 1010, 0.6 part of barium stearate and 0.6 part of gamma-aminopropyl triethoxysilane, and carrying out melt extrusion, injection molding and cooling on the mixture to obtain the light source radiator of the comparative example.
Comparative example 5.
A high heat dissipation type LED light source radiator is prepared by the following steps.
(1) Configuration H 2 O 2 A mixed aqueous solution of phosphoric acid, said H 2 O 2 In a mixed aqueous solution of phosphoric acid, H 2 O 2 10 mass percent of phosphoric acid, 6 mass percent of water and the balance of water; soaking the carbon nano tube in the H 2 O 2 The carbon nano tube is soaked in H in the mixed water solution of phosphoric acid 2 O 2 The mass ratio of the feed liquid in the mixed water solution of phosphoric acid is feed/liquid=1:8; standing for 1h, filtering after standing, washing the carbon nano tube with deionized water for 3 times, and drying at 80 ℃ for later use.
(2) Preparing a mixed aqueous solution of copper nitrate and cerium nitrate, wherein the concentration of the copper nitrate is 9g/100mL, the concentration of the cerium nitrate is 5g/100mL, and the balance is water; sieving zinc oxide powder with a 1000-mesh sieve, wherein the sieved powder is firstly soaked in an oxalic acid aqueous solution (the mass percentage of oxalic acid is 7%, and the rest is water) for 3min, and the mass ratio of the material liquid of the sieved powder soaked in the oxalic acid aqueous solution is (material/liquid=1:8); then filtering, and soaking the solid phase in the mixed aqueous solution of copper nitrate and cerium nitrate for 1min, wherein the mass ratio of the solid phase to the mixed aqueous solution of copper nitrate and cerium nitrate is (material/liquid=1:6); taking out after the soaking is finished, drying in the environment of 90+/-5 ℃, soaking in the mixed aqueous solution of the copper nitrate and the cerium nitrate again for 1min after the drying, taking out, drying and weighing, and repeating the soaking, drying and weighing processes until the solid phase mass is increased by 8.09% compared with that before the mixed aqueous solution of the copper nitrate and the cerium nitrate is not soaked; and then placing the solid phase in an environment of 420+/-20 ℃ for calcination for 1h, and air-cooling to normal temperature to obtain a solid phase A.
(3) Preparing aqueous solutions of citric acid and glycine, wherein the concentration of the citric acid in the aqueous solutions of the citric acid and the glycine is 2g/100mL, the concentration of the glycine is 1.1g/100mL, and the balance is water; soaking the solid phase A in the aqueous solution of the citric acid and the glycine to form a mixture, wherein the mass ratio of the solid phase A to the aqueous solution of the citric acid and the glycine in the mixture is (material/liquid=1:5); placing the mixture into a reaction kettle, sealing the kettle body, heating to 120+/-5 ℃, preserving heat at the temperature for 30min, air-cooling the mixture to normal temperature along with the reaction kettle after the heat preservation is finished, taking out the mixture, filtering, washing the solid phase with deionized water for 3 times, and drying at 80 ℃ to obtain a solid phase B.
(4) Sieving silicon carbide powder with a 1000-mesh sieve, cleaning the sieved powder with acetone for 3 times, drying, and soaking in a sodium hydroxide aqueous solution, wherein the mass percentage of solute in the sodium hydroxide aqueous solution is 10%, and the mass ratio of the silicon carbide powder to the sodium hydroxide aqueous solution is (material/liquid=1:5); heating the solution to 75+/-5 ℃ and preserving heat for 3 hours, cooling the solution to normal temperature by air after heating, filtering, washing the solid phase with deionized water for 3 times, and drying at 80 ℃ to obtain a solid phase C.
(5) Mixing and stirring polyamide-6 matrix resin, the carbon nano tube treated in the step (1), the solid phase B, the solid phase C, an antioxidant 1010, barium stearate and gamma-aminopropyl triethoxysilane, wherein the components in the mixture are as follows in parts by weight: 60 parts of polyamide-6 matrix resin, 5 parts of carbon nano tubes treated in the step (1), 3 parts of solid phase B, 3 parts of solid phase C, 1.5 parts of antioxidant 1010, 0.6 part of barium stearate and 0.6 part of gamma-aminopropyl triethoxysilane, and carrying out melt extrusion, injection molding and cooling on the mixture to obtain the light source radiator of the comparative example.
Example 5.
The heat conductivity coefficients of the light source heat sinks prepared in examples 1 to 4 and comparative examples 1 to 5 were respectively tested, and the results are shown in table 1.
Table 1:
as shown in Table 1, the radiator prepared by the method has good heat conductivity and can effectively radiate heat generated in the working process of the LED lamp.
The foregoing detailed description of the embodiments of the present invention will be provided to those skilled in the art, and the detailed description and the examples should not be construed as limiting the invention.
Claims (5)
1. The high heat dissipation type LED light source radiator is characterized in that the preparation method of the radiator comprises the following steps:
(1) Configuration H 2 O 2 Soaking the carbon nano tube in the mixed aqueous solution of phosphoric acid 2 O 2 Standing for 1-2 h in the mixed aqueous solution of phosphoric acid, filtering after standing, washing with deionized water2-3 times of drying the carbon nano tube for standby;
(2) Preparing a mixed aqueous solution of copper nitrate and cerium nitrate, sieving zinc oxide powder with a 1000-mesh screen, soaking the sieved powder in an oxalic acid aqueous solution for 3-5 min, filtering, soaking the solid phase in the mixed aqueous solution of copper nitrate and cerium nitrate for 1-2 min again, taking out the mixed aqueous solution after soaking, drying the mixed aqueous solution of copper nitrate and cerium nitrate in an environment of 90+/-5 ℃, soaking the mixed aqueous solution of copper nitrate and cerium nitrate again for 1-2 min after drying, taking out the mixed aqueous solution of copper nitrate and cerium nitrate, drying and weighing the mixed aqueous solution, and repeating the processes of soaking, drying and weighing until the solid phase mass is increased by more than 8% compared with that before the mixed aqueous solution of copper nitrate and cerium nitrate is not soaked; then placing the solid phase in an environment of 420+/-20 ℃ for calcination for more than 1 hour, and air-cooling to normal temperature to obtain a solid phase A;
(3) Preparing aqueous solutions of citric acid and glycine, soaking the solid phase A in the aqueous solutions of citric acid and glycine to form a mixture, placing the mixture into a reaction kettle, sealing the kettle body, heating to 120+/-5 ℃, preserving heat for 10min at the temperature, adding a nitric acid solution into the mixture, continuously preserving heat for 20-30 min, air-cooling the mixture along with the reaction kettle to normal temperature after the heat preservation is finished, taking out the mixture, filtering, washing the solid phase with deionized water for 3-4 times, and drying to obtain a solid phase B;
(4) Sieving silicon carbide powder with a 1000-mesh screen, washing the sieved powder with acetone for 2-3 times, drying, soaking in a sodium hydroxide aqueous solution, heating the solution to 70-80 ℃ and preserving heat for 3-4 hours, air-cooling the solution to normal temperature after heating, filtering, washing a solid phase with deionized water for 3-4 times, and drying to obtain a solid phase C;
(5) And (3) mixing and stirring the polyamide-6 matrix resin, the carbon nano tube treated in the step (1), the solid phase B, the solid phase C, the antioxidant, the lubricant and the coupling agent, and carrying out melt extrusion and injection molding on the mixed materials, and cooling to obtain the light source radiator.
2. The high heat dissipation LED light source heatsink of claim 1, wherein the H 2 O 2 In a mixed aqueous solution of phosphoric acid, H 2 O 2 The mass percentage of the phosphate is 10 percentThe weight percentage content is 5-8%, the rest is water; the carbon nano tube is soaked in H 2 O 2 The mass ratio of the feed liquid in the mixed aqueous solution of phosphoric acid is feed/liquid=1:8-10.
3. The high heat dissipation type LED light source radiator according to claim 1, wherein the concentration of copper nitrate in the mixed aqueous solution of copper nitrate and cerium nitrate is 6-16 g/100mL, the concentration of cerium nitrate is 3-7 g/100mL, and the balance is water; the mass percentage of oxalic acid in the oxalic acid aqueous solution is 6% -8%, and the balance is water; the mass ratio of the material to the liquid of the water solution of the sieved powder soaked in oxalic acid is material/liquid=1:8-10, and the mass ratio of the material to the liquid of the mixed water solution of the solid phase soaked in the copper nitrate and the cerium nitrate is material/liquid=1:6-7.
4. The high heat dissipation type LED light source radiator according to claim 1, wherein in the aqueous solution of citric acid and glycine, the concentration of the citric acid is 1-4 g/100mL, the concentration of the glycine is 0.8-1.6 g/100mL, and the balance is water; the mass ratio of the solid phase A to the material liquid in the aqueous solution of the citric acid and the glycine is (1:5) - (6), the mass percentage of the solute in the nitric acid solution is (6) - (10%), the balance is water, and the adding amount of the nitric acid solution/the amount of the aqueous solution of the citric acid and the glycine in the reaction kettle is (5) - (9 mL)/100 mL.
5. The high heat dissipation type LED light source radiator according to claim 1, wherein the mass percentage of solute in the sodium hydroxide aqueous solution is 10% -20%, and the mass ratio of silicon carbide powder to the feed liquid of the sodium hydroxide aqueous solution is 1:5-6.
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