CN116515455B - Ultraviolet LED lamp bead bonded by silazane and preparation method thereof - Google Patents
Ultraviolet LED lamp bead bonded by silazane and preparation method thereof Download PDFInfo
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- CN116515455B CN116515455B CN202310779406.3A CN202310779406A CN116515455B CN 116515455 B CN116515455 B CN 116515455B CN 202310779406 A CN202310779406 A CN 202310779406A CN 116515455 B CN116515455 B CN 116515455B
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- led lamp
- lamp bead
- ultraviolet led
- polysilazane
- adhesive
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- 239000011324 bead Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 230000001070 adhesive effect Effects 0.000 claims abstract description 57
- 239000000853 adhesive Substances 0.000 claims abstract description 56
- 229920001709 polysilazane Polymers 0.000 claims abstract description 50
- -1 aluminum compound Chemical class 0.000 claims abstract description 25
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000012719 thermal polymerization Methods 0.000 claims abstract description 12
- 239000000178 monomer Substances 0.000 claims description 20
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 14
- 229920000642 polymer Polymers 0.000 claims description 9
- WGGNJZRNHUJNEM-UHFFFAOYSA-N 2,2,4,4,6,6-hexamethyl-1,3,5,2,4,6-triazatrisilinane Chemical compound C[Si]1(C)N[Si](C)(C)N[Si](C)(C)N1 WGGNJZRNHUJNEM-UHFFFAOYSA-N 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 238000007865 diluting Methods 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- FIADVASZMLCQIF-UHFFFAOYSA-N 2,2,4,4,6,6,8,8-octamethyl-1,3,5,7,2,4,6,8-tetrazatetrasilocane Chemical compound C[Si]1(C)N[Si](C)(C)N[Si](C)(C)N[Si](C)(C)N1 FIADVASZMLCQIF-UHFFFAOYSA-N 0.000 claims description 6
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 6
- LIQDVINWFSWENU-UHFFFAOYSA-K aluminum;prop-2-enoate Chemical compound [Al+3].[O-]C(=O)C=C.[O-]C(=O)C=C.[O-]C(=O)C=C LIQDVINWFSWENU-UHFFFAOYSA-K 0.000 claims description 6
- GCPCLEKQVMKXJM-UHFFFAOYSA-N ethoxy(diethyl)alumane Chemical compound CCO[Al](CC)CC GCPCLEKQVMKXJM-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- WOZZOSDBXABUFO-UHFFFAOYSA-N tri(butan-2-yloxy)alumane Chemical compound [Al+3].CCC(C)[O-].CCC(C)[O-].CCC(C)[O-] WOZZOSDBXABUFO-UHFFFAOYSA-N 0.000 claims description 6
- JROMGTZTUZNJJY-UHFFFAOYSA-N 1,3,5-tris(ethenyl)-2,4,6-trimethyl-1,3,5,2,4,6-triazatrisilinane Chemical compound C(=C)N1[SiH](N([SiH](N([SiH]1C)C=C)C)C=C)C JROMGTZTUZNJJY-UHFFFAOYSA-N 0.000 claims description 5
- MDDPTCUZZASZIQ-UHFFFAOYSA-N tris[(2-methylpropan-2-yl)oxy]alumane Chemical compound [Al+3].CC(C)(C)[O-].CC(C)(C)[O-].CC(C)(C)[O-] MDDPTCUZZASZIQ-UHFFFAOYSA-N 0.000 claims description 5
- UGXMKSYKRKUMGY-UHFFFAOYSA-N 1,3,5,2,4,6-triazatrisilinane Chemical compound N1[SiH2]N[SiH2]N[SiH2]1 UGXMKSYKRKUMGY-UHFFFAOYSA-N 0.000 claims description 4
- YAYVEQQGOJLBQC-UHFFFAOYSA-N 1,3,5,7-tetrakis(ethenyl)-2,4,6,8-tetramethyl-1,3,5,7,2,4,6,8-tetrazatetrasilocane Chemical compound C(=C)N1[SiH](N([SiH](N([SiH](N([SiH]1C)C=C)C)C=C)C)C=C)C YAYVEQQGOJLBQC-UHFFFAOYSA-N 0.000 claims description 4
- JVZKVVDFQLHZBY-UHFFFAOYSA-N N1[SiH2]N[SiH2]N[SiH2]N[SiH2]1 Chemical compound N1[SiH2]N[SiH2]N[SiH2]N[SiH2]1 JVZKVVDFQLHZBY-UHFFFAOYSA-N 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 4
- BDAWXSQJJCIFIK-UHFFFAOYSA-N potassium methoxide Chemical compound [K+].[O-]C BDAWXSQJJCIFIK-UHFFFAOYSA-N 0.000 claims description 4
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 2
- WPUMTJGUQUYPIV-JIZZDEOASA-L disodium (S)-malate Chemical compound [Na+].[Na+].[O-]C(=O)[C@@H](O)CC([O-])=O WPUMTJGUQUYPIV-JIZZDEOASA-L 0.000 claims description 2
- 235000019265 sodium DL-malate Nutrition 0.000 claims description 2
- 239000001632 sodium acetate Substances 0.000 claims description 2
- 235000017281 sodium acetate Nutrition 0.000 claims description 2
- 239000001394 sodium malate Substances 0.000 claims description 2
- MYWQGROTKMBNKN-UHFFFAOYSA-N tributoxyalumane Chemical compound [Al+3].CCCC[O-].CCCC[O-].CCCC[O-] MYWQGROTKMBNKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 abstract description 23
- 230000000694 effects Effects 0.000 abstract description 4
- 230000001133 acceleration Effects 0.000 abstract description 2
- 238000007711 solidification Methods 0.000 abstract 1
- 230000008023 solidification Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 17
- 239000000945 filler Substances 0.000 description 10
- 230000032683 aging Effects 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000002329 infrared spectrum Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229910007991 Si-N Inorganic materials 0.000 description 2
- 229910006294 Si—N Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- NKRJRPDCNYYXEZ-UHFFFAOYSA-N (2-methylpropan-2-yl)oxyalumane Chemical compound CC(C)(C)O[AlH2] NKRJRPDCNYYXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910018516 Al—O Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 241000235648 Pichia Species 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 229920001558 organosilicon polymer Polymers 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/16—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers in which all the silicon atoms are connected by linkages other than oxygen atoms
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
- C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
- C08G77/398—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing boron or metal atoms
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/60—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which all the silicon atoms are connected by linkages other than oxygen atoms
- C08G77/62—Nitrogen atoms
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
- H01L2933/0008—Processes
- H01L2933/0033—Processes relating to semiconductor body packages
- H01L2933/005—Processes relating to semiconductor body packages relating to encapsulations
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The application discloses an ultraviolet LED lamp bead bonded by silazane and a preparation method thereof in the silazane field, wherein an adhesive of the ultraviolet LED lamp bead comprises the following components in parts by weight: 100 parts of polysilazane and 5-20 parts of an organic aluminum compound as a binder. The application provides a technical effect of realizing the support of a molecular structure, increasing active sites, further realizing the acceleration of the solidification speed and improving the bonding strength by carrying out thermal polymerization reaction on an organic aluminum compound and polysilazane.
Description
Technical Field
The application belongs to the technical field of silazane, and particularly relates to an ultraviolet LED lamp bead bonded by silazane and a preparation method thereof.
Background
The organic silicon binder is a common binder between the glass cover plate and the bracket in the LED lamp bead, has good weather resistance and chemical stability, and mainly comprises polysiloxane, polysilazane, polysilabozane and the like; in the process of curing the organic silicon adhesive, the molecular structure shows a shrinkage trend, and when the organic silicon adhesive is bonded, the shrinkage trend of the outermost bonding molecules contacted with the substrate is smaller and larger towards the upper layer due to the support of the substrate, so that the bonding precision is poor, the bonding strength is not high, the aging time of the adhesive is accelerated under the condition of long-time ultraviolet radiation, and the service life of the ultraviolet LED lamp beads is shortened; filler is added into the organosilicon binder, and filler particles can effectively control the degree of molecular shrinkage in the curing process of the organosilicon binder, but the addition of the filler affects the performances of the binder in all aspects; polysilazane is an organosilicon polymer with Si-N as a polymerization unit, and when the polysilazane is used for a binder, an isocyanate curing agent is usually required to be added for curing the polysilazane, active groups are introduced into the polysilazane to accelerate the curing effect of the polysilazane, the curing condition is limited, and the polysilazane is difficult to use in a large scale.
The prior silazane technology mainly has the following problems: the first polysilazane binder has harsh curing conditions and longer curing time; second, polysilazane adhesives shrink in molecular structure during curing, resulting in reduced bond strength.
Disclosure of Invention
Aiming at the situation, in order to overcome the defects of the prior art, the application provides the ultraviolet LED lamp bead bonded by silazane and the preparation method thereof, and in order to solve the problems of severe curing conditions and lower bonding strength, the application provides a technical effect of realizing the support of a molecular structure, increasing active sites, further realizing the acceleration of curing speed and improving bonding strength by polymerizing silazane and organic aluminum.
In order to achieve the above purpose, the technical scheme adopted by the application is as follows: the application provides an ultraviolet LED lamp bead bonded by silazane, wherein the adhesive of the ultraviolet LED lamp bead comprises the following components in parts by weight: 100 parts of polysilazane and 5-20 parts of an organic aluminum compound.
Preferably, the polysilazane is a polymer using cyclotrisilazane and cyclotetrasilazane as polymerization monomers.
Preferably, the cyclotrisilazane comprises at least one of hexamethylcyclotrisilazane, trimethyltrivinyl cyclotrisilazane.
Preferably, the cyclotetrasilazane is at least one of octamethyl cyclotetrasilazane and tetramethyl tetravinyl cyclotetrasilazane.
Preferably, the organic aluminum compound is at least one of aluminum isopropoxide, aluminum sec-butoxide, aluminum n-butoxide, diethyl aluminum ethoxide, aluminum tert-butoxide, and aluminum acrylate.
Preferably, the binder has a polymer monomer formula of、。
Preferably, the R1 group is at least one of isopropyl, sec-butyl, n-butyl, ethyl, tert-butyl, and acrylic group.
Preferably, the R2 group is at least one of methyl and vinyl.
The application also provides a preparation method of the ultraviolet LED lamp bead bonded by silazane, which comprises the following steps:
s1, diluting polysilazane monomer with a solvent, adding a catalyst in a nitrogen atmosphere, and removing redundant solvent after reacting for 2-6 hours to obtain polysilazane;
s2, performing thermal polymerization reaction on the polysilazane prepared in the step S1 and an organic aluminum compound in a nitrogen atmosphere to obtain an adhesive of the ultraviolet LED lamp beads;
and S3, coating the ultraviolet LED lamp bead adhesive prepared in the step S2 on the top of the glass cover plate and the top of the bracket, and curing the adhesive to obtain the ultraviolet LED lamp bead.
Preferably, in S1, the catalyst is at least one of lithium hexaphenyl cyclotrisilazane, potassium methoxide, sodium acetate and sodium malate.
Preferably, in S1, the solvent is at least one of toluene, xylene, and n-hexane.
Preferably, in S2, the temperature of the thermal polymerization reaction is 300-400℃and the reaction time is 4-8 hours.
The beneficial effects obtained by the application are as follows:
according to the application, the organic aluminum compound and polysilazane are subjected to thermal polymerization reaction, so that the adhesive property and the ageing resistance of the polysilazane serving as an adhesive are effectively improved; according to the application, the organic aluminum compound is introduced into the polysilazane polymer, the Al element can effectively support the polysilazane binder, so that the shrinkage effect generated in the curing process is avoided, the interfacial densification of the binder is facilitated, the bonding strength and the ageing resistance of the binder are improved, the organic aluminum compound can increase active groups in the polysilazane, the compatibility with adhered substances is improved, the curing is easy, and the performance of the binder is improved.
Drawings
FIG. 1 is a graph showing the results of high temperature shear strength of the UV LED bead binders prepared in examples 1-5 and comparative examples 1-3 of the present application;
FIG. 2 is a graph showing the results of the bonding strength and aging resistance of the UV LED bead adhesives prepared in examples 1-5 and comparative examples 1-3 of the present application;
FIG. 3 is an SEM image of the interface of the ultraviolet LED lamp beads prepared in example 1 after curing the adhesive;
fig. 4 is an infrared spectrum of the adhesive of the uv LED lamp bead prepared in example 1 of the present application.
The accompanying drawings are included to provide a further understanding of the application and are incorporated in and constitute a part of this specification, illustrate the application and together with the embodiments of the application, serve to explain the application.
Detailed Description
The following description of the embodiments of the present application will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the application; all other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the present application. The preferred methods and materials described herein are illustrative only and should not be construed as limiting the application.
The experimental methods in the following examples are all conventional methods unless otherwise specified; the test materials and test strains used in the examples described below, unless otherwise specified, were commercially available.
The sources of the materials used in the application are as follows:
hexamethyl cyclotrisilazane (CasNo: 1009-93-4) is available from Shanghai, inc. of medical technologies, inc., trade name: BD64079;
trimethyl trivinyl Cyclotrisilazane (CasNo: 5505-72-6) is available from Shanghai Michelin Biochemical technologies Co., ltd., brand: t865220;
octamethyl cyclotetrasilazane (CasNo: 1020-84-4) is available from Shanghai microphone Biochemical technologies Co., ltd., brand: o833879;
tetramethyl tetravinyl Cyclo-tetrasilazane (CasNo: 5162-63-0) is available from Shanghai Meilin Biochemical technologies Co., ltd., brand: t934210;
aluminum isopropoxide (CasNo: 555-31-7) was purchased from Shanghai Bi-pharmaceutical technologies Co., ltd., brand: BD113691;
aluminum sec-butoxide (CasNo: 2269-22-9) was purchased from Sigma Aldrich (Shanghai) trade Co., ltd., trade name: 201073;
diethylaluminum ethoxide (CasNo: 1586-92-1) was purchased from Shanghai Bi-pharmaceutical technologies Co., ltd., brand: BD64079;
aluminum tert-butoxide (CasNo: 556-91-2) is available from Shanghai Pichia pharmaceutical technologies Co., ltd., brand: BD113737;
aluminum acrylate (CasNo: 15743-20-1) is available from Hadamard agents Co., ltd., trade name: 27208C.
Example 1
An ultraviolet LED lamp bead bonded by silazane, wherein the adhesive of the ultraviolet LED lamp bead comprises the following components in parts by weight: 100 parts of polysilazane and 5 parts of an organic aluminum compound.
The polysilazane monomer is hexamethyl-cyclotrisilazane; the organic aluminum compound is aluminum isopropoxide.
The structural formula of the polymer monomer of the binder is。
The application also provides a preparation method of the ultraviolet LED lamp bead bonded by silazane, which comprises the following steps:
s1, diluting a hexamethyl-cyclotrisilazane monomer with n-hexane, adding lithium hexaphenyl-cyclotrisilazane salt in a nitrogen atmosphere, reacting at the temperature of-10 ℃ for 6 hours, and removing excess cyclohexane to obtain polysilazane;
s2, carrying out thermal polymerization reaction on the polysilazane prepared in the step S1 and aluminum isopropoxide in a nitrogen atmosphere, wherein the reaction temperature is 380 ℃, and the reaction time is 6 hours, so as to obtain an adhesive of the ultraviolet LED lamp beads;
and S3, coating the ultraviolet LED lamp bead adhesive prepared in the step S2 on the top of the glass cover plate and the top of the bracket, and curing the adhesive to obtain the ultraviolet LED lamp bead.
Example 2
An ultraviolet LED lamp bead bonded by silazane, wherein the adhesive of the ultraviolet LED lamp bead comprises the following components in parts by weight: 100 parts of polysilazane and 10 parts of an organic aluminum compound.
The polysilazane monomer is trimethyl trivinyl cyclotrisilazane; the organoaluminum compound is aluminum sec-butoxide.
The structural formula of the polymer monomer of the binder is。
The application also provides a preparation method of the ultraviolet LED lamp bead bonded by silazane, which comprises the following steps:
s1, diluting a trimethyl trivinyl cyclotrisilazane monomer with n-hexane, adding hexaphenyl cyclotrisilazane lithium salt in a nitrogen atmosphere, reacting at the temperature of-10 ℃ for 6 hours, and removing redundant cyclohexane to obtain polysilazane;
s2, carrying out thermal polymerization reaction on the polysilazane prepared in the step S1 and aluminum sec-butoxide in a nitrogen atmosphere, wherein the reaction temperature is 320 ℃, and the reaction time is 8 hours, so as to obtain an adhesive of the ultraviolet LED lamp beads;
and S3, coating the ultraviolet LED lamp bead adhesive prepared in the step S2 on the top of the glass cover plate and the top of the bracket, and curing the adhesive to obtain the ultraviolet LED lamp bead.
Example 3
Ultraviolet LED lamp beads bonded by silazane, wherein the bonding of the ultraviolet LED lamp beads comprises the following components in parts by weight: 100 parts of polysilazane and 15 parts of an organic aluminum compound.
The polysilazane monomer is octamethyl-cyclotetrasilazane; the organoaluminum compound is aluminum tert-butoxide.
The structural formula of the polymer monomer of the binder is。
The application also provides a preparation method of the ultraviolet LED lamp bead bonded by silazane, which comprises the following steps:
s1, diluting an octamethyl-cyclotetrasilazane monomer with toluene, adding potassium methoxide under a nitrogen atmosphere, reacting at 250 ℃ for 6 hours, and removing redundant toluene to obtain polysilazane;
s2, carrying out thermal polymerization reaction on the polysilazane prepared in the step S1 and tert-butoxyaluminum in a nitrogen atmosphere, wherein the reaction temperature is 300 ℃, and the reaction time is 8 hours, so as to obtain an adhesive of the ultraviolet LED lamp beads;
and S3, coating the ultraviolet LED lamp bead adhesive prepared in the step S2 on the top of the glass cover plate and the top of the bracket, and curing the adhesive to obtain the ultraviolet LED lamp bead.
Example 4
An ultraviolet LED lamp bead bonded by silazane, wherein the adhesive of the ultraviolet LED lamp bead comprises the following components in parts by weight: 100 parts of polysilazane and 20 parts of an organic aluminum compound.
The polysilazane monomer is tetramethyl tetravinyl cyclotetrasilazane; the organic aluminum compound is aluminum acrylate.
The structural formula of the polymer monomer of the binder is。
The application also provides a preparation method of the ultraviolet LED lamp bead bonded by silazane, which comprises the following steps:
s1, diluting a tetramethyl tetravinyl cyclosilazane monomer with toluene, adding potassium methoxide in a nitrogen atmosphere, reacting at the temperature of 250 ℃ for 6 hours, and removing excess toluene to obtain polysilazane;
s2, carrying out thermal polymerization reaction on the polysilazane prepared in the step S1 and aluminum acrylate in a nitrogen atmosphere, wherein the reaction temperature is 380 ℃, and the reaction time is 6 hours, so as to obtain an adhesive of the ultraviolet LED lamp beads;
and S3, coating the ultraviolet LED lamp bead adhesive prepared in the step S2 on the top of the glass cover plate and the top of the bracket, and curing the adhesive to obtain the ultraviolet LED lamp bead.
Example 5
An ultraviolet LED lamp bead bonded by silazane, wherein the adhesive of the ultraviolet LED lamp bead comprises the following components in parts by weight: 100 parts of polysilazane and 10 parts of an organic aluminum compound.
The polysilazane monomer is hexamethyl-cyclotrisilazane; the organic aluminum compound is diethyl aluminum ethoxide.
The structural formula of the polymer monomer of the binder is。
The application also provides a preparation method of the ultraviolet LED lamp bead bonded by silazane, which comprises the following steps:
s1, diluting a hexamethyl-cyclotrisilazane monomer with cyclohexane, adding lithium hexaphenyl-cyclotrisilazane salt in a nitrogen atmosphere, reacting at the temperature of-10 ℃ for 6 hours, and removing excess cyclohexane to obtain polysilazane;
s2, carrying out thermal polymerization reaction on the polysilazane prepared in the step S1 and diethyl aluminum ethoxide in a nitrogen atmosphere, wherein the reaction temperature is 400 ℃, and the reaction time is 4 hours, so as to obtain the adhesive of the ultraviolet LED lamp beads;
and S3, coating the ultraviolet LED lamp bead adhesive prepared in the step S2 on the top of the glass cover plate and the top of the bracket, and curing the adhesive to obtain the ultraviolet LED lamp bead.
Comparative example 1
This comparative example provides an ultraviolet LED lamp bead bonded with silazane, which differs from example 1 in that: the polysilazane prepared in example 1 was mixed with Al powder, which was 10% by mass of the filler in the binder.
Comparative example 2
This comparative example provides an ultraviolet LED lamp bead bonded with silazane, which differs from example 1 in that: the polysilazane prepared in example 1 was mixed with Al powder, which was 5% by mass of the filler in the binder.
Comparative example 3
This comparative example provides an ultraviolet LED lamp bead bonded with silazane, which differs from example 1 in that: the polysilazane prepared in example 1 was mixed with Al powder, which was 15% by mass of the filler in the binder.
Experimental example
1. The adhesive samples were tested for shear strength according to standard astm d905-89 at a loading speed of 0.2mm/min.
2. Testing the bonding strength of the ultraviolet LED lamp bead adhesive according to the ISO4624-2002 standard, polishing a spindle by using a full-automatic drawing instrument, cleaning and drying by alcohol, bonding a test piece coated by the adhesive with the spindle, and testing after curing; the ultraviolet LED lamp beads prepared in the above examples 1 to 5 and comparative examples 1 to 3 were subjected to ultraviolet aging for 500 hours under ultraviolet conditions, and then the bonding strength of the ultraviolet LED lamp beads was measured.
3. Scanning electron microscope analysis: the microscopic morphology of the section of the bonded sample was observed and analyzed using a scanning electron microscope.
4. Infrared spectrum information of the adhesive prepared in example 1 was tested using an infrared spectrometer. The KBr tabletting method is adopted, and the test range is 4000-500cm -1 。
Analysis of results
Fig. 1 is a graph showing the results of high temperature shear strength of the uv LED lamp bead adhesives prepared in examples 1 to 5 and comparative examples 1 to 3 according to the present application, as shown in the graph, the examples 1 to 5 show higher shear strength than the comparative examples 1 to 3 at 200 ℃ and at 1000 ℃, and the comparative examples 1 to 3 can effectively improve the shear strength by adding Al powder as an active filler to the adhesive by using a conventional method, whereas the adhesive prepared in examples 1 to 5 according to the present application is more uniformly dispersed than the adhesive prepared in comparative examples except that the active filler only plays a physical role by organically forming Al element and combining it with polysilazane through thermal polymerization reaction.
FIG. 2 is a graph showing the results of the bonding strength and aging resistance of the ultraviolet LED bead adhesives prepared in examples 1-5 and comparative examples 1-3, wherein the bonding strength is significantly higher at 200℃and 1000℃as compared with comparative examples 1-3, and the reactive filler is directly added to the adhesive, and the reactive filler has a tendency to migrate to the lower layer of the adhesive during curing of the adhesive, so that the adhesive prepared in comparative examples 1-3 has poor bonding properties; after 500h of ultraviolet ageing, the strength of the adhesive prepared in the examples and the comparative examples is reduced, but the ultraviolet LED lamp bead adhesive prepared in the examples still has higher adhesive performance.
Fig. 3 is an SEM image of the interface of the ultraviolet LED lamp bead prepared in example 1 after the adhesive is cured, as shown in the figure, the density of the adhesive interface is higher, the effective acting area at the interface is higher, and the adhesive performance is better.
FIG. 4 is an infrared spectrum of the adhesive for UV LED beads prepared in example 1 of the present application, as shown in the graph, at 3500-3400cm -1 The absorption peak corresponding to N-H bond is 1950-1850cm -1 The absorption peak of the corresponding Al-O bond is 3000-2900cm -1 The sum 1300-1250cm < -1 > corresponds to Si-CH 3 Is 3100-3050cm -1 The absorption peak of C-O is 1380-1350cm -1 The absorption peak of Si-O is 1150-1050cm -1 The position corresponds to the absorption peak of Si-N; the above-described absorption peak type and position substantially correspond to those of the binder prepared in example 1.
Although embodiments of the present application have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the application, the scope of which is defined in the appended claims and their equivalents.
The application and its embodiments have been described above with no limitation, and the application is illustrated in the figures of the accompanying drawings as one of its embodiments, without limitation in practice. In summary, those skilled in the art, having benefit of this disclosure, will appreciate that the application can be practiced without the specific details disclosed herein.
Claims (4)
1. An ultraviolet LED lamp bead bonded by silazane, which is characterized in that: the adhesive of the ultraviolet LED lamp bead comprises the following components in parts by weight: 100 parts of polysilazane and 5-20 parts of an organic aluminum compound;
the polysilazane is a polymer taking cyclotrisilazane and cyclotetrasilazane as polymerization monomers;
the organic aluminum compound is at least one of aluminum isopropoxide, aluminum sec-butoxide, aluminum n-butoxide, diethyl aluminum ethoxide, aluminum tert-butoxide and aluminum acrylate;
the preparation method of the ultraviolet LED lamp bead bonded by silazane specifically comprises the following steps:
s1, diluting polysilazane monomer with a solvent, adding a catalyst in a nitrogen atmosphere, and removing redundant solvent after reacting for 2-6 hours to obtain polysilazane;
s2, carrying out thermal polymerization reaction on the polysilazane prepared in the step S1 and an organic aluminum compound in a nitrogen atmosphere, wherein the temperature of the thermal polymerization reaction is 300-400 ℃ and the reaction time is 4-8 hours, so as to obtain an adhesive of the ultraviolet LED lamp beads;
and S3, coating the ultraviolet LED lamp bead adhesive prepared in the step S2 on the tops of the glass cover plate and the bracket, and curing the adhesive to obtain the ultraviolet LED lamp bead.
2. The uv LED lamp bead bonded with silazane according to claim 1, wherein: the cyclotrisilazane comprises at least one of hexamethylcyclotrisilazane and trimethyltrivinyl cyclotrisilazane.
3. The uv LED lamp bead bonded with silazane according to claim 2, wherein: the cyclotetrasilazane is at least one of octamethyl cyclotetrasilazane and tetramethyl tetravinyl cyclotetrasilazane.
4. The uv LED lamp bead bonded with silazane according to claim 3, wherein: in S1, the catalyst is at least one of lithium hexaphenyl cyclotrisilazane, potassium methoxide, sodium acetate and sodium malate; the solvent is at least one of toluene, xylene and n-hexane.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63191832A (en) * | 1986-09-26 | 1988-08-09 | Toa Nenryo Kogyo Kk | Production of new polyaluminopolysilazane |
| US4886860A (en) * | 1988-03-23 | 1989-12-12 | Toa Nenryo Kogyo Kabushiki Kaisha | Polymetalosilazane and process for preparing same |
| KR20130072990A (en) * | 2011-12-22 | 2013-07-02 | 한국세라믹기술원 | Encapsulant for uvled device, uvled device using the same and manufacturing method thereof |
| CN107417177A (en) * | 2017-06-22 | 2017-12-01 | 安徽省德邦瓷业有限公司 | A kind of high-temperature Resistance Adhesives used in domestic ceramics manufacturing process |
| CN108641672A (en) * | 2018-06-01 | 2018-10-12 | 湖北新海鸿化工有限公司 | A kind of anti-oxidant LED packaging plastics of high transparency |
| CN109406038A (en) * | 2018-11-26 | 2019-03-01 | 闽南师范大学 | A kind of flat membrane structure SiAlCN wireless and passive pressure sensor and preparation method thereof |
| CN109627447A (en) * | 2019-01-31 | 2019-04-16 | 倍晶生物科技（上海）有限公司 | A kind of preparation method and application of polysilazane material |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2022168729A (en) * | 2021-04-26 | 2022-11-08 | 信越化学工業株式会社 | Glassy adhesive |
-
2023
- 2023-06-29 CN CN202310779406.3A patent/CN116515455B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63191832A (en) * | 1986-09-26 | 1988-08-09 | Toa Nenryo Kogyo Kk | Production of new polyaluminopolysilazane |
| US4886860A (en) * | 1988-03-23 | 1989-12-12 | Toa Nenryo Kogyo Kabushiki Kaisha | Polymetalosilazane and process for preparing same |
| KR20130072990A (en) * | 2011-12-22 | 2013-07-02 | 한국세라믹기술원 | Encapsulant for uvled device, uvled device using the same and manufacturing method thereof |
| CN107417177A (en) * | 2017-06-22 | 2017-12-01 | 安徽省德邦瓷业有限公司 | A kind of high-temperature Resistance Adhesives used in domestic ceramics manufacturing process |
| CN108641672A (en) * | 2018-06-01 | 2018-10-12 | 湖北新海鸿化工有限公司 | A kind of anti-oxidant LED packaging plastics of high transparency |
| CN109406038A (en) * | 2018-11-26 | 2019-03-01 | 闽南师范大学 | A kind of flat membrane structure SiAlCN wireless and passive pressure sensor and preparation method thereof |
| CN109627447A (en) * | 2019-01-31 | 2019-04-16 | 倍晶生物科技（上海）有限公司 | A kind of preparation method and application of polysilazane material |
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