CN106350000A - Preparing method of TiO2 enhanced glow transparent organic silica gel - Google Patents
Preparing method of TiO2 enhanced glow transparent organic silica gel Download PDFInfo
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- CN106350000A CN106350000A CN201610750124.0A CN201610750124A CN106350000A CN 106350000 A CN106350000 A CN 106350000A CN 201610750124 A CN201610750124 A CN 201610750124A CN 106350000 A CN106350000 A CN 106350000A
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- Prior art keywords
- silica gel
- organic silica
- transparent organic
- preparation
- butyl titanate
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09J183/04—Polysiloxanes
- C09J183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
-
- 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
- C08K3/08—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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
-
- 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
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Luminescent Compositions (AREA)
- Led Device Packages (AREA)
Abstract
The invention provides a preparing method of TiO2 enhanced glow transparent organic silica gel, which uses the characteristics of scattering and secondary excitation of titanium dioxide nanoparticles for enhancing the optical excitation and reducing the light attenuation. The smaller energy band width can directly absorb energy wavelengths with less energy for secondary excitation. This invention further adopts the central ion luminescence properties of Pt quantum dots, and the conduction band and valence band of TiO2 and energy band of Pt quantum dots have ladder differences, which can further enhance the secondary excitation of light.
Description
Technical field
The present invention relates to a kind of transparent silica gel field, a kind of tio of specific design2Strengthen the preparation of luminescence transparent organic silica gel
Method.
Background technology
, because having the features such as life-span length, energy-efficient, environmental protection in terms of illumination, led is as new photograph for quasiconductor led
Mingguang City source substitutes conventional illumination sources and has sizable potentiality, is to solve one of effective way of current energy crisis.With
The constantly improve of power type white light led manufacturing technology, its luminous efficiency, brightness and power are all improved largely.Therefore, led
Encapsulating material starts to face huge challenge, prepares with high refractive index, high resistance to ultraviolet ability and heat-proof aging ability, low
Stress, the encapsulating material of high heat conductance, it is expected to improve optical output power and the service life of illuminating device.Data show, led
Light source is than electric filament lamp economize on electricity 87%, ratio fluorescent lamp economize on electricity 50%, and the life-span is longer 20～30 times than electric filament lamp, longer 10 times than fluorescent lamp.
LED light source is because having that energy-saving and environmental protection, long-life, safety, response be fast, small volume, rich color, a series of uniquenesses such as controlled are excellent
Point is it is considered to be the optimal realization means of energy consumption drop in economize on electricity.Cob encapsulation is a kind of chip directly placed technology, is by bare chip
It is affixed directly on printed circuit board (PCB), then carry out wire bonding, then technique chip and lead encapsulating protected with organic gel.
Cob-led light source has the advantages such as high efficiency, low-loss, long-life, light colour purity, vibration resistance, fast response time.When led face light
When source adopts cob technique productions, abandon the metal rack encapsulation mode of straw hat pipe and paster lamp bead, can be directly by chip attachment
On the splendid metal basal board of heat conductivility, radiating efficiency improves tens times than lamp bead formula LED light source, and led will be greatly lowered
The light decay of light source, is effectively ensured the service life of LED lamp.Led area source is the encapsulation of whole face, and advanced technique will perfectly solve
The certainly uneven problem of led lamp beads coloured light, whole face goes out light, and the equal light effect of illumination is good, be following room lighting energy-conserving light source not
Two choosing.
In general, the encapsulating material of led have several as follows: epoxy resin, silica gel, silicones.But in conjunction with current city
From the point of view of three kinds of led encapsulating materials of field main flow, although epoxy resin encapsulating material has advantage in light transmission and cost,
Show slightly not enough at brightness decay, anti-uv, the aspect such as heat-resisting.Silicones are in the performance ratio of the aspect such as heat-resisting, anti-uv and brightness decay
Epoxy resin is eager to excel, and and epoxy resin combine to obtain preferable no interface problem, compare and be suitable for use in white light and some low decay will
In the encapsulation asked (as display screen, wiring board, rosette etc.), but weak point is the Gao Gong being unsuitable to apply to more than more than 0.5w
On rate product, price is relatively also costly.Silica gel relative to for the above two, has larger in anti-uv, heat-resisting and brightness decay
Advantage, be particularly suited for use in high-power LED product and partly on low decay and white light product, but shortcoming to be adhesion poor,
Combine easy generation interface problem, easy moisture absorption with epoxy, dust tightness is poor.
However, silica gel packaging body has decay and certain absorption, the decay that can reduce light is excited to ask by secondary light
How topic, strengthen photoemissive secondary excitation, improves decay of luminescence problems demand and solves.
Content of the invention
The problem existing for prior art, it is an object of the invention to provide a kind of tio2Strengthen luminescence transparent organosilicon
The preparation method of glue, the specifically comprising the following steps that of the method
A. weigh butyl titanate, ethanol, water, glacial acetic acid according to the ratio of required formulation components, and carry out mix and blend, heating
Annealing 2h obtains nanometer level titanium dioxide powder, and described butyl titanate, ethanol, water, the mass ratio of glacial acetic acid are 1:9:2:
9；
B. above-mentioned prepared nanometer level titanium dioxide powder is mixed in butyl titanate, carries out magnetic agitation and obtain presoma
Solution, the weight of nanometer level titanium dioxide powder and butyl titanate is than for 1:100 to 2:100；
C. above-mentioned a certain amount of precursor solution is added in a certain amount of organic silica gel；The addition of precursor solution with
Described organic silica gel mass ratio between the two is 10:100 to 20:100；It is thoroughly mixed, be obtained and there is nano titanium oxide
Organic silicon packaging glue；
D. firming agent and catalyst are added in prepared having in the organic silicon packaging glue of nano titanium oxide, through being sufficiently stirred for mixing
After conjunction, vacuum distillation aerofluxuss are steeped, after drained bubble, cold curing 10-25 h；Or it is heated to 110～150 DEG C of solidifications 60
Min, the tio2 finally giving solidification strengthens luminescence transparent organic silica gel.
According to embodiments of the invention, wherein, in stepb, also include pt quantum dot being dispensed into metatitanic acid four fourth simultaneously
In ester.
According to embodiments of the invention, wherein, the particle diameter of described pt quantum dot is in below 20nm.
According to embodiments of the invention, wherein, in step a, the time of described stirring is more than 1 hour, described heating
Temperature be 1000 DEG C -1500 DEG C.
According to embodiments of the invention, wherein, organic silica gel is α, alpha, omega-dihydroxy polydimethyl siloxane, α, ω-dihydroxy
Any one in base poly dimethyl hexichol siloxanes.
According to embodiments of the invention, wherein, described firming agent is methyl 3 third (fourth) ketoximinosilanes and vinyl three
Third (fourth) ketoximinosilanes, described catalyst is dibutyl tin laurate；The addition of described firming agent and catalyst is by having
On the basis of the quality of machine silica gel；
According to embodiments of the invention, wherein, firming agent is 5:100 to 10:100 with the mass ratio of organic silica gel；Catalyst with
The mass ratio of organic silica gel is 0.5:100 to 1:100.
Compared with prior art, the mechanism of the inventive method and feature are as described below:
The present invention utilizes the scattering of titania nanoparticles and the characteristic of secondary excitation, strengthens light and excites, reduces optical attenuation, its
The light wave that less bandwidth can directly absorb less energy carries out secondary excitation.The present invention also adopts the center of pt quantum dot
Ion Luminescence Properties, and, the conduction band of titanium dioxide and valence band have ladder difference with the energy band of pt quantum dot, can increase further
The secondary excitation of high light.
Specific embodiment
The invention will be further described with the following Examples.
Embodiment 1:
The tio2 that the present invention provides strengthens the preparation method of luminescence transparent organic silica gel, the specifically comprising the following steps that of the method
A. weigh butyl titanate, ethanol, water, glacial acetic acid according to the ratio of required formulation components, and carry out mix and blend, heating
Obtain nanometer level titanium dioxide powder, described butyl titanate, ethanol, water, the mass ratio of glacial acetic acid to 1500 DEG C of annealing 2h
For 1:9:2:9；
B. above-mentioned prepared nanometer level titanium dioxide powder and pt quantum dot are mixed in butyl titanate, carry out magnetic force and stir
Mix and obtain precursor solution, the weight of nanometer level titanium dioxide powder and butyl titanate is than for 1:100；
C. above-mentioned a certain amount of precursor solution is added in a certain amount of organic silica gel；The addition of precursor solution with
Described organic silica gel mass ratio between the two is 10:100；It is thoroughly mixed, the organosilicon encapsulation with nanometer tio2 is obtained
Glue；
D. firming agent and catalyst are added in prepared having in the organic silicon packaging glue of nanometer tio2, through being thoroughly mixed
Afterwards, vacuum distillation aerofluxuss bubble, after drained bubble, cold curing 25 h；Or it is heated to 150 DEG C of solidification 60 min, finally give
The tio2 of solidification strengthens luminescence transparent organic silica gel.
Embodiment 2:
The present invention also provides another kind of tio2 to strengthen the preparation method of luminescence transparent organic silica gel, and the concrete steps of the method are such as
Under:
A. weigh butyl titanate, ethanol, water, glacial acetic acid according to the ratio of required formulation components, and carry out mix and blend, heating
Obtain nanometer level titanium dioxide powder to 1000 DEG C of annealing 2h, described butyl titanate, ethanol, water, the mass ratio of glacial acetic acid are
1:9:2:9；
B. above-mentioned prepared nanometer level titanium dioxide powder is mixed in butyl titanate, carries out magnetic agitation and obtain presoma
Solution, the weight of nanometer level titanium dioxide powder and butyl titanate is than for 2:100；
C. above-mentioned a certain amount of precursor solution is added in a certain amount of organic silica gel；The addition of precursor solution with
Described organic silica gel mass ratio between the two is 20:100；It is thoroughly mixed, the organosilicon encapsulation with nanometer tio2 is obtained
Glue；
D. firming agent and catalyst are added in prepared having in the organic silicon packaging glue of nanometer tio2, through being thoroughly mixed
Afterwards, vacuum distillation aerofluxuss bubble, after drained bubble, cold curing 10 h；Or it is heated to 150 DEG C of solidification 60 min, finally give
The tio2 of solidification strengthens luminescence transparent organic silica gel.
Embodiment 3:
The present invention also provides another tio2 to strengthen the preparation method of luminescence transparent organic silica gel, and the concrete steps of the method are such as
Under:
A. weigh butyl titanate, ethanol, water, glacial acetic acid according to the ratio of required formulation components, and carry out mix and blend, heating
Obtain nanometer level titanium dioxide powder, described butyl titanate, ethanol, water, the mass ratio of glacial acetic acid to 1200 DEG C of annealing 2h
For 1:9:2:9；
B. above-mentioned prepared nanometer level titanium dioxide powder is mixed in butyl titanate, carries out magnetic agitation and obtain presoma
Solution, the weight of nanometer level titanium dioxide powder and butyl titanate is than for 1.5:100；
C. above-mentioned a certain amount of precursor solution is added in a certain amount of organic silica gel；The addition of precursor solution with
Described organic silica gel mass ratio between the two is 20:100；It is thoroughly mixed, the organosilicon encapsulation with nanometer tio2 is obtained
Glue；
D. firming agent and catalyst are added in prepared having in the organic silicon packaging glue of nanometer tio2, through being thoroughly mixed
Afterwards, vacuum distillation aerofluxuss bubble, after drained bubble, cold curing 10 h；Or it is heated to 110 DEG C of solidification 60 min, finally give
The tio2 of solidification strengthens luminescence transparent organic silica gel.
According to embodiments of the invention, wherein, the particle diameter of described pt quantum dot is in below 20nm.
According to embodiments of the invention, wherein, in step a, the time of described stirring is more than 1 hour, described heating
Temperature be 1000 DEG C -1500 DEG C.
According to embodiments of the invention, wherein, organic silica gel is α, alpha, omega-dihydroxy polydimethyl siloxane, α, ω-dihydroxy
Any one in base poly dimethyl hexichol siloxanes.
According to embodiments of the invention, wherein, described firming agent is methyl 3 third (fourth) ketoximinosilanes and vinyl three
Third (fourth) ketoximinosilanes, described catalyst is dibutyl tin laurate；The addition of described firming agent and catalyst is by having
On the basis of the quality of machine silica gel；
According to embodiments of the invention, wherein, firming agent is 5:100 to 10:100 with the mass ratio of organic silica gel；Catalyst with
The mass ratio of organic silica gel is 0.5:100 to 1:100.
It is last that it is noted that obvious, above-described embodiment is only intended to clearly illustrate example of the present invention, and simultaneously
The non-restriction to embodiment.For those of ordinary skill in the field, can also do on the basis of the above description
Go out change or the variation of other multi-forms.There is no need to be exhaustive to all of embodiment.And thus drawn
Obvious change that Shen goes out or change among still in protection scope of the present invention.
Claims (7)
1. a kind of tio2Strengthen the preparation method of luminescence transparent organic silica gel it is characterised in that specifically comprising the following steps that of the method
A. weigh butyl titanate, ethanol, water, glacial acetic acid according to the ratio of required formulation components, and carry out mix and blend, heating
Annealing 2h obtains nanometer level titanium dioxide powder, and described butyl titanate, ethanol, water, the mass ratio of glacial acetic acid are 1:9:2:9；
B. above-mentioned prepared nanometer level titanium dioxide powder is mixed in butyl titanate, carries out magnetic agitation and obtain presoma
Solution, the weight of nanometer level titanium dioxide powder and butyl titanate is than for 1:100 to 2:100；
C. above-mentioned a certain amount of precursor solution is added in a certain amount of organic silica gel；The addition of precursor solution with
Described organic silica gel mass ratio between the two is 10:100 to 20:100；It is thoroughly mixed, be obtained and there is nano titanium oxide
Organic silicon packaging glue；
D. firming agent and catalyst are added in prepared having in the organic silicon packaging glue of nano titanium oxide, through being sufficiently stirred for mixing
After conjunction, vacuum distillation aerofluxuss are steeped, after drained bubble, cold curing 10-25 h；Or it is heated to 110～150 DEG C of solidifications 60
Min, the tio2 finally giving solidification strengthens luminescence transparent organic silica gel.
2. tio according to claim 12The preparation method strengthening luminescence transparent organic silica gel is it is characterised in that in step b
In, also include pt quantum dot being dispensed in butyl titanate simultaneously.
3. tio according to claim 22The preparation method strengthening luminescence transparent organic silica gel is it is characterised in that described pt
The particle diameter of quantum dot is in below 20nm.
4. tio according to claim 12The preparation method strengthening luminescence transparent organic silica gel is it is characterised in that in step a
In, the time of described stirring is more than 1 hour, and the temperature of described heating is 1000 DEG C -1500 DEG C.
5. tio according to claim 12The preparation method strengthening luminescence transparent organic silica gel is it is characterised in that organosilicon
Glue is α, alpha, omega-dihydroxy polydimethyl siloxane, α, any one in alpha, omega-dihydroxy polydimethyl hexichol siloxanes.
6. tio according to claim 12The preparation method strengthening luminescence transparent organic silica gel is it is characterised in that described solid
Agent is methyl 3 third (fourth) ketoximinosilanes and vinyl 3 third (fourth) ketoximinosilanes, and described catalyst is tin dilaurate two
Butyl tin；On the basis of the addition of described firming agent and catalyst presses the quality of organic silica gel.
7. tio according to claim 62The preparation method strengthening luminescence transparent organic silica gel is it is characterised in that firming agent
Mass ratio with organic silica gel is 5:100 to 10:100；Catalyst is 0.5:100 to 1:100 with the mass ratio of organic silica gel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610750124.0A CN106350000A (en) | 2016-08-30 | 2016-08-30 | Preparing method of TiO2 enhanced glow transparent organic silica gel |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610750124.0A CN106350000A (en) | 2016-08-30 | 2016-08-30 | Preparing method of TiO2 enhanced glow transparent organic silica gel |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115185020A (en) * | 2022-08-04 | 2022-10-14 | 江西麦帝施科技有限公司 | Diffusion medium and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101580628A (en) * | 2009-06-05 | 2009-11-18 | 华东师范大学 | Quantum dot luminescence transparent casting glue composite material |
| CN102876281A (en) * | 2012-09-13 | 2013-01-16 | 上海大学 | Preparation method for nano TiO2 modified high-refractive index organic silica gel for chip on board-light emitting diode (COB-LED) pressing strip |
-
2016
- 2016-08-30 CN CN201610750124.0A patent/CN106350000A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101580628A (en) * | 2009-06-05 | 2009-11-18 | 华东师范大学 | Quantum dot luminescence transparent casting glue composite material |
| CN102876281A (en) * | 2012-09-13 | 2013-01-16 | 上海大学 | Preparation method for nano TiO2 modified high-refractive index organic silica gel for chip on board-light emitting diode (COB-LED) pressing strip |
Non-Patent Citations (2)
| Title |
|---|
| 王杏等: "《纳米二氧化钛的生产与应用》", 31 July 2014, 贵州科技出版社 * |
| 蔡定建等: "《无机化学实验》", 31 August 2013, 华中科技大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115185020A (en) * | 2022-08-04 | 2022-10-14 | 江西麦帝施科技有限公司 | Diffusion medium and preparation method thereof |
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Application publication date: 20170125 |