CN105462584B - Fluorescent carbon point and preparation method thereof and the filling composition of LED chip - Google Patents
Fluorescent carbon point and preparation method thereof and the filling composition of LED chip Download PDFInfo
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Abstract
The invention discloses a kind of fluorescent carbon point and preparation method thereof and the filling composition of LED chip, wherein, the preparation method includes：(1) after the cellulosic fabric containing isopropanol is burnt, ash content M1 is obtained；(2) ash content M1 and concentrated nitric acid are subjected to oxidation reaction, fluorescent carbon point is made；Wherein, the oxidizing acid is selected from nitric acid.Above-mentioned design is by the way that cellulosic fabric is burnt under conditions of containing isopropanol, then the ash content and concentrated nitric acid that are obtained after burning are subjected to oxidation reaction, so as to which fluorescent carbon point be made by this method, the filling composition of LED chip is made after fluorescent carbon point made from this method and adhesive are mixed, and it is applied in the preparation of LED chip, so that its LED chip cost obtained is relatively low, simple for process, stability is high, environmental-friendly, and light can uniformly disperse when in use.
Description
Technical field
The present invention relates to LED chip fill material fields, and in particular, to a kind of fluorescent carbon point and preparation method thereof and
The filling composition of LED chip.
Background technology
Under the dual-pressure of global energy shortage crisis and environmental pollution getting worse, low-carbon energy-saving, environmentally protective, color
Coloured silk is abundant, service life is longer, the semi-conductor LED illuminating technology of micromation is come into being.Since it is on energy saving and environmentally friendly
Double dominant is approved by the world, as universally acknowledged New Solid lighting engineering, and in energy saving green illumination
Field degree of receiving more and more attention.White LED light source has come into people’s lives, has been widely used at present at home
The fields such as illumination, screen display, lamps for vehicle, backlight of LCD and daily decoration.
Even to this day, the LED chip of lighting of existing three kinds of comparative maturities obtains the method for white light：Quantum Well technology, RGB are more
Chip technology, fluorescence transformation approach.Wherein fluorescence transformation approach is most widely used at present, and technology is most ripe, technique simplest one
The mainstream technology that kind is popularized very much.And the principle of luminosity of used fluorescence transformation approach is usually the color contamination principle of light now, is
Under the excitation of low-voltage direct, it can launch blue light (450~460nm) using InGaN light emitting diodes, be coated in so as to excite
The phosphor emission of chip top goes out visible ray, and is finally mixed into white light.And the fluorescent powder used at present mainly passes through height
The rare earth oxide of warm Solid phase synthesis reduces LED fluorescent yields between this luminescent material due to the interaction of light attracts, and
Phosphor material powder is the opaque particle of micron-sized solid, there are problems that more serious being in the light causes luminous uniformity bad；
Secondly lack feux rouges in rare earth phosphor spectral component, cause colour temperature higher, and then the reduction (example of various performances can be caused
The reduction of such as service life)；The presence in the form of suspension in packaging plastic because of fluorescent powder again, there are settlement issues, cause
Fluorescent powder coating is uneven, so as to cause non-uniform light.Furthermore rare earth phosphor has very big pollution to environment.
Therefore it provides a kind of cost is relatively low, simple for process, stability is high, environmental-friendly, and the fluorescence that can be uniformly dispersed
The problem of carbon dots and preparation method thereof and the filling composition of LED chip are urgent need to resolve of the present invention.
The content of the invention
For the above-mentioned prior art, it is an object of the invention to overcome in the prior art light-emitting phosphor uniformity it is bad,
The problem of colour temperature is higher during use, and environmental pollution is larger, so as to provide a kind of cost is relatively low, simple for process, stability is high,
It is environmental-friendly, and fluorescent carbon point that can be uniformly dispersed and preparation method thereof and the filling composition of LED chip.
To achieve these goals, the present invention provides a kind of preparation method of fluorescent carbon point, wherein, the preparation method
Including：
(1) after the cellulosic fabric containing isopropanol is burnt, ash content M1 is obtained；
(2) ash content M1 and oxidizing acid are subjected to oxidation reaction, fluorescent carbon point is made；Wherein, the oxidizing acid is selected from
Nitric acid.
The present invention also provides a kind of fluorescent carbon points according to made from preparation method described above.
The present invention also provides a kind of filling composition of LED chip, wherein, the filling composition is included according to above-mentioned institute
Fluorescent carbon point made from the preparation method stated or according to fluorescent carbon point and adhesive described above.
Through the above technical solutions, the present invention burns cellulosic fabric under conditions of containing isopropanol, then
The ash content and oxidizing acid that are obtained after burning are subjected to oxidation reaction, so as to which fluorescent carbon point be made by this method, by the party
The filling composition of LED chip is made after fluorescent carbon point made from method and adhesive mixing, and is applied to the preparation of LED chip
In so that its LED chip cost obtained is relatively low, simple for process, stability is high, environmental-friendly, and luminous energy when in use
It is enough homodisperse.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Description of the drawings
Attached drawing is for providing a further understanding of the present invention, and a part for constitution instruction, with following tool
Body embodiment is together for explaining the present invention, but be not construed as limiting the invention.In the accompanying drawings：
Fig. 1 is fluorescence emission spectrogram of compound of the A1 obtained under different excitation wavelengths in embodiment 1 in the present invention；
Fig. 2 be in the present invention in embodiment 1 A1 obtained ultraviolet lamp for a long time irradiate under figure of fluorescence intensity changes；
Fig. 3 is LED chip encapsulation cross-reference figure；
Fig. 4 is the fluorescence spectras of A1 obtained after packaging in embodiment 1 in the present invention；
Fig. 5 is the chromaticity coordinate figure of white light LEDs made from A1 obtained in embodiment 1 in the present invention.
Specific embodiment
The specific embodiment of the present invention is described in detail below.It is it should be appreciated that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the invention.
The present invention provides a kind of preparation method of fluorescent carbon point, wherein, the preparation method includes：
(1) after the cellulosic fabric containing isopropanol is burnt, ash content M1 is obtained；
(2) ash content M1 and oxidizing acid are subjected to oxidation reaction, fluorescent carbon point is made；Wherein, the oxidizing acid is selected from
Nitric acid.
Then above-mentioned design will be obtained by the way that cellulosic fabric is burnt under conditions of containing isopropanol after burning
Ash content and oxidizing acid carry out oxidation reaction, so as to by this method be made fluorescent carbon point.Certainly, here contain isopropyl
Alcohol cellulosic fabric burning can be immersed with isopropanol cellulosic fabric take out after burn, can also be according to alcohol
The operating method of lamp lights wick after the alcohol in alcolhol burner is changed to isopropanol, other similar modes that can be realized exist
It may be used in the present invention, do not repeat one by one herein.
The nitric acid can be the salpeter solution of any concentration, for example, in a kind of preferred embodiment of the present invention,
The nitric acid can be provided by concentration for the salpeter solution of 2-14mol/L.
The cellulosic fabric can be cellulosic fabric type commonly used in the art, for example, the one of the present invention
In kind preferred embodiment, in order to make combustion efficiency more preferable, the cellulosic fabric can be selected from cotton fabric, flaxen fiber
Fabric or bamboo fiber.
The dosage of the salpeter solution can be not construed as limiting compared with the dosage of the ash content M1, certainly, in order to enable institute
It states ash content M1 and aoxidizes the yield for completely, improving fluorescent carbon point as far as possible, in a kind of embodiment being more highly preferred to of the present invention,
Compared with the ash content M1 of 100mg, the dosage of the salpeter solution can be further defined to 100-200mL.
The oxidation reaction is operated according to this field conventional practices, for example, one kind in the present invention is preferred
In embodiment, the reaction temperature of the oxidation reaction could be provided as 100-160 DEG C, and the reaction time could be provided as 0.5-
3h。
In order to make the yield higher of fluorescent carbon point obtained, and less side products, in the preferred implementation of one kind of the present invention
It can also include ash content M1 obtained carrying out activation drying process in mode, in step (1), the activation drying process can be with
Drying means according to this field routine is operated, for example, can be high temperature drying, drying temperature and drying time can not
It is construed as limiting, for example, in a kind of embodiment being more highly preferred to of the present invention, in order to be obtained under conditions of saving energy consumption as far as possible
To preferable drying effect, can select ash content M1 being placed at 100-150 DEG C dry 0.5-1h.
In order to enable the concentration higher of the fluorescent carbon point so that its using effect when actually preparing LED chip is more preferable,
It can also include extracting fluorescent carbon point obtained in a kind of preferred embodiment of the present invention, in step (2), make
Obtain high brightness fluorescent carbon dots.
The extracting process can be operated according to the extracting process of this field routine, and extractant can be conventional uses
Extractant type, for example, can be the conventional use of type such as n-butanol, certainly, in order to enable its content is higher, and avoid
It introduces on fluorescent carbon point influential extractant type when in use, in a kind of preferred embodiment of the present invention, extraction
Agent can be with selected as ethyl acetate.
The dosage of the extractant can not be further qualified, certainly, it is contemplated that and it is cost-effective, and still reach higher
Extraction concentration, the present invention a kind of embodiment being more highly preferred in, it is described compared with the fluorescent carbon point of 100 parts by volume
The dosage of extractant can be with selected as 10-100 parts by volume.
The present invention also provides a kind of fluorescent carbon points according to made from preparation method described above.
The present invention also provides a kind of filling composition of LED chip, wherein, the filling composition is included according to above-mentioned institute
Fluorescent carbon point made from the preparation method stated or according to fluorescent carbon point and adhesive described above.
Here adhesive can be according to curing materials commonly used in the art, it is, for example, possible to use being passed through in LED chip
Frequently with silicones and curing agent mixing, for example, what can be commonly used according to this field presses resin and curing agent volume
According to 1:5 ratio is mixed to prepare adhesive, and resin can be conventional use of epoxy resin, silica gel or silicones etc., curing agent
Or commercially available conventional such curing agent, certainly, the material of other similar effects can also use herein, at this then not
It illustrates one by one.
Certainly, the fluorescent carbon point can be used directly, certainly, in order to further improve the utilization rate of fluorescent carbon point,
In a kind of preferred embodiment of the present invention, the fluorescent carbon point can be the glimmering of 1-50 weight % by the concentration of fluorescent carbon point
Light carbon dots solution provides.
Solvent in above-mentioned fluorescent carbon point solution can be type of solvent commonly used in the art, for example, can be just
Butanol, certainly, in order to make the dispersion performance of fluorescent carbon point in the solution more preferable, and then higher using effect, in this hair
In a kind of bright embodiment being more highly preferred to, the solvent in the fluorescent carbon point solution can be further selected as acetic acid second
Ester.
The fluorescent carbon point solution and the adhesive can be not construed as limiting with magnitude relation, certainly, in order to enable in LED
There is during the use of chip better using effect, avoid causing during fluorescent carbon point excessive concentration Fluorescence quenching effect or
Be fluorescent carbon point concentration it is too low cause shine it is weaker, the present invention a kind of preferred embodiment in, the fluorescent carbon point is molten
The dosage volume ratio of liquid and the adhesive can be defined to 1：1-5.
Fluorescent carbon point solution and the adhesive are packaged in LED chip and can be carried out according to conventional packaged type, when
So, in order to avoid occurring bubble in encapsulation process, and curing rate is accelerated as far as possible, in a kind of preferred embodiment party of the present invention
In formula, which can dry 0.5-1h in 80-120 DEG C of vacuum drying chamber.As long as it is the operation of this field routine
Mode can be operated, herein herein without repeating.
The present invention will be described in detail by way of examples below.In following embodiment, the isopropanol, the nitre
Sour, described alcolhol burner and the ethyl acetate are conventional commercial products.
Embodiment 1
Ethyl alcohol in alcolhol burner is changed to isopropanol, lights wick, collects ash content M1；10mg ash contents M1 is taken to be placed in 100
DEG C baking oven in activate dry 0.5h；It measures the salpeter solution that 20ml concentration is 14mol/L and is heated to 140 DEG C, to above-mentioned heating
10mg ash contents M1 reflux operation 2h at 140 DEG C are added in salpeter solution afterwards, after natural cooling, fluorescent carbon point is made；With
Ethyl acetate is extracted, until the pH value of lower floor's water sample is 7, is discarded lower floor's liquid, is obtained fluorescent carbon point A1.
As shown in Figure 1, Fig. 1 is fluorescence emission spectrogram of compound of the high brightness fluorescent carbon dots A1 under different excitation wavelengths, pass through
When Fig. 1 can be seen that the excitation light wave a length of 460nm of carbon dots, transmitting fluorescence intensity is maximum, so the optimal excitation of this carbon dots
Wavelength is 460nm.The chip emission wavelength used in the present invention is just 460nm, consistent with the maximum excitation wavelength of carbon dots.
Fig. 2 is figure of fluorescence intensity changes of the high brightness fluorescent carbon dots A1 in the case where ultraviolet lamp irradiates for a long time, as seen in Figure 2,
For ultraviolet lamp for a long time under irradiation, fluorescence intensity change is little, it can be seen that it has good stabilization when in use
Property.
Embodiment 2
Ethyl alcohol in alcolhol burner is changed to isopropanol, lights wick, collects ash content M2；20mg ash contents M2 is taken to be placed in 100
DEG C baking oven in activate dry 0.5h；It measures the salpeter solution that 20ml concentration is 14mol/L and is heated to 140 DEG C, to above-mentioned heating
20mg ash contents M2 reflux operation 2h at 140 DEG C are added in salpeter solution afterwards, after natural cooling, fluorescent carbon point is made；With
Ethyl acetate is extracted, until the pH value of lower floor's water sample is 7, is discarded lower floor's liquid, is obtained fluorescent carbon point A2.
Embodiment 3
Ethyl alcohol in alcolhol burner is changed to isopropanol, lights wick, collects ash content M3；30mg ash contents M3 is taken to be placed in 100
DEG C baking oven in activate dry 0.5h；It measures the salpeter solution that 20ml concentration is 14mol/L and is heated to 140 DEG C, to above-mentioned heating
30mg ash contents M3 reflux operation 2h at 140 DEG C are added in salpeter solution afterwards, after natural cooling, fluorescent carbon point is made；With
Ethyl acetate is extracted, until the pH value of lower floor's water sample is 7, is discarded lower floor's liquid, is obtained fluorescent carbon point A3.
Embodiment 4
Ethyl alcohol in alcolhol burner is changed to isopropanol, lights wick, collects ash content M4；50mg ash contents M4 is taken to be placed in 100
DEG C baking oven in activate dry 0.5h；It measures the salpeter solution that 20ml concentration is 14mol/L and is heated to 140 DEG C, to above-mentioned heating
50mg ash contents M4 reflux operation 2h at 140 DEG C are added in salpeter solution afterwards, after natural cooling, fluorescent carbon point is made；With
Ethyl acetate is extracted, until the pH value of lower floor's water sample is 7, is discarded lower floor's liquid, is obtained fluorescent carbon point A4.
Embodiment 5
Ethyl alcohol in alcolhol burner is changed to isopropanol, lights wick, collects ash content M5；It is 14mol/ to measure 20ml concentration
The salpeter solution of L is heated to 140 DEG C, and 10mg ash contents M5 is added in into the salpeter solution after above-mentioned heating and is flowed back at 140 DEG C behaviour
Make 2h, after natural cooling, fluorescent carbon point is made；It is extracted with ethyl acetate, until the pH value of lower floor's water sample is 7, is discarded
Lower floor's liquid obtains fluorescent carbon point A5.
Embodiment 6
Ethyl alcohol in alcolhol burner is changed to isopropanol, lights wick, collects ash content M6；10mg ash contents M6 is taken to be placed in 100
DEG C baking oven in activate dry 0.5h；It measures the salpeter solution that 20ml concentration is 14mol/L and is heated to 160 DEG C, to above-mentioned heating
10mg ash contents M6 reflux operation 2h at 160 DEG C are added in salpeter solution afterwards, after natural cooling, fluorescent carbon point is made；With
Ethyl acetate is extracted, until the pH value of lower floor's water sample is 7, is discarded lower floor's liquid, is obtained fluorescent carbon point A6.
Embodiment 7
Ethyl alcohol in alcolhol burner is changed to isopropanol, lights wick, collects ash content M7；10mg ash contents M7 is taken to be placed in 100
DEG C baking oven in activate dry 0.5h；It measures the salpeter solution that 20ml concentration is 14mol/L and is heated to 180 DEG C, to above-mentioned heating
10mg ash contents M7 reflux operation 2h at 180 DEG C are added in salpeter solution afterwards, after natural cooling, fluorescent carbon point is made；With
Ethyl acetate is extracted, until the pH value of lower floor's water sample is 7, is discarded lower floor's liquid, is obtained fluorescent carbon point A7.
Embodiment 8
Ethyl alcohol in alcolhol burner is changed to isopropanol, lights wick, collects ash content M8；10mg ash contents M8 is taken to be placed in 100
DEG C baking oven in activate dry 0.5h；It measures the salpeter solution that 20ml concentration is 14mol/L and is heated to 120 DEG C, to above-mentioned heating
10mg ash contents M8 reflux operation 2h at 120 DEG C are added in salpeter solution afterwards, after natural cooling, fluorescent carbon point is made；With
Ethyl acetate is extracted, until the pH value of lower floor's water sample is 7, is discarded lower floor's liquid, is obtained fluorescent carbon point A8.
Embodiment 9
Ethyl alcohol in alcolhol burner is changed to isopropanol, lights wick, collects ash content M9；10mg ash contents M9 is taken to be placed in 100
DEG C baking oven in activate dry 0.5h；It measures the salpeter solution that 20ml concentration is 14mol/L and is heated to 100 DEG C, to above-mentioned heating
10mg ash contents M9 reflux operation 2h at 100 DEG C are added in salpeter solution afterwards, after natural cooling, fluorescent carbon point is made；With
Ethyl acetate is extracted, until the pH value of lower floor's water sample is 7, is discarded lower floor's liquid, is obtained fluorescent carbon point A9.
Embodiment 10
It is prepared by the preparation method according to embodiment 1, unlike, the concentration of nitric acid is 10mol/L, and fluorescent carbon is made
Point A10.
Embodiment 11
It is prepared by the preparation method according to embodiment 1, unlike, the concentration of nitric acid is 5mol/L, and fluorescent carbon is made
Point A11.
Embodiment 12
It is prepared by the preparation method according to embodiment 1, unlike, the concentration of nitric acid is 3mol/L, and fluorescent carbon is made
Point A12.
Embodiment 13
It is prepared by the preparation method according to embodiment 1, unlike, the time of reflux operation is 0.5h, and fluorescence is made
Carbon dots A13.
Embodiment 14
It is prepared by the preparation method according to embodiment 1, unlike, the time of reflux operation is 1h, and fluorescent carbon is made
Point A14.
Embodiment 15
It is prepared by the preparation method according to embodiment 1, unlike, the time of reflux operation is 1.5h, and fluorescence is made
Carbon dots A15.
Embodiment 16
It is prepared by the preparation method according to embodiment 1, unlike, the time of reflux operation is 2.5h, and fluorescence is made
Carbon dots A16.
Embodiment 17
It is prepared by the preparation method according to embodiment 1, unlike, the time of reflux operation is 3h, and fluorescent carbon is made
Point A17.
Embodiment 18
It is prepared by the preparation method according to embodiment 1, unlike, it is extracted with n-butanol, fluorescent carbon point is made
A18。
Embodiment 19
It is prepared by the preparation method according to embodiment 1, unlike, it is extracted with benzene, fluorescent carbon point A19 is made.
Embodiment 20
It is prepared by the preparation method according to embodiment 1, unlike, it is extracted with n-hexane, fluorescent carbon point is made
A20。
Comparative example 1
The accurate 10mg graphite that weighs is placed in the dry 0.5h of activation in 100 DEG C of baking oven；It is 14mol/L nitre to measure 20ml concentration
Acid solution is heated to 140 DEG C, and 10mg graphite reflux operation 2h at 140 DEG C is added in into the salpeter solution after above-mentioned heating, is treated
After natural cooling, fluorescent carbon point is made；It is extracted with ethyl acetate, until the pH value of lower floor's water sample is 7, discards subnatant
Body obtains fluorescent carbon point D1.
Comparative example 2
The accurate 10mg activated carbons that weigh are placed in the dry 0.5h of activation in 100 DEG C of baking oven；It is 14mol/L to measure 20ml concentration
Salpeter solution be heated to 140 DEG C, into the salpeter solution after above-mentioned heating add in 10mg activated carbons reflux operation at 140 DEG C
After natural cooling, fluorescent carbon point is made in 2h；It is extracted with ethyl acetate, until the pH value of lower floor's water sample is 7, is discarded down
Layer liquid, obtains fluorescent carbon point D2.
Comparative example 3
The accurate 10mg ground coffees that weigh are placed in the dry 0.5h of activation in 100 DEG C of baking oven；It is 14mol/L to measure 20ml concentration
Salpeter solution be heated to 140 DEG C, into the salpeter solution after above-mentioned heating add in 10mg ground coffees reflux operation at 140 DEG C
After natural cooling, fluorescent carbon point is made in 2h；It is extracted with ethyl acetate, until the pH value of lower floor's water sample is 7, is discarded down
Layer liquid, obtains fluorescent carbon point D3.
Comparative example 4
The accurate 10mg benzene burning ashes that weigh are placed in the dry 0.5h of activation in 100 DEG C of baking oven；Measuring 20ml concentration is
The salpeter solution of 14mol/L is heated to 140 DEG C, and 10mg benzene is added in into the salpeter solution after above-mentioned heating and is flowed back at 140 DEG C
2h is operated, after natural cooling, fluorescent carbon point is made；It is extracted with ethyl acetate, until the pH value of lower floor's water sample is 7, is abandoned
Sub-cloud liquid obtains fluorescent carbon point D4.
Application examples 1
By 10ml A1 obtained above, obtained fluorescent carbon point solution is dissolved in 50ml ethyl acetate, by above-mentioned fluorescent carbon
(silicones and silicones curing agent here routinely makes for this field for point solution, 60ml silicones and 180ml silicones curing agent
Type plays the role of adhesive jointly after mixing, other types commonly used in the art can also use, herein not
Repeat more) mixing after respectively packaging LED chips, be subsequently placed in 100 DEG C of vacuum drying chamber and place 1h, after being encapsulated
LED chip Y1.
Application examples 2
It is prepared in the way of application examples 1, unlike, the above-mentioned A1 used is changed to D4, after encapsulation is made
LED chip Y2.
Test case
By A1-A20 obtained above and D1-D4 respectively at room temperature, with fluorescein (QY=0.95) for reference substance, pass through
It is close or equal to measure the absorbance of carbon dots and reference substance, and absorbance is less than under conditions of 0.05, carbon dots is in identical exciting light
Lower integral fluorescence area as shown in Figure 4 and Figure 5, is examined so as to calculate fluorescence quantum yield by the integrated value of above-mentioned fluorescence area
The fluorescence quantum yield of carbon determination point, obtains that the results are shown in Table 1.Y1 obtained above and Y2 is reached into photoelectricity by Wuhu moral person of outstanding talent's profit
Its photoelectric properties detects by distant place spectral analysis software in scientific and technological limited semiconductor company, and obtained result is as follows.
The testing result of Y1 is as follows：
X=0.2502 y=0.2082
Luminous flux phi=21.325lm colour temperature Tc=7642K colour rendering indexs Ra=74.3
The testing result of Y2 is as follows：
X=0.1703 y=0.0775
Luminous flux phi=1.2312lm colour temperature Tc=10000K colour rendering indexs Ra=0.4
It can be seen that by above-mentioned testing result for Y2, Y1 chromaticity coordinates tend to white light field, and light leads to
Amount significantly increases, and colour temperature is relatively low, and colour rendering index significantly improves.
Table 1
By upper table as can be seen that the carbon dots fluorescence quantum yield highest being prepared according to the method for embodiment 1, different
, when carbon source quality increase, nitric acid amount remains unchanged, and carbon dots cannot get sufficient oxide etch, when reaction temperature raises
When, since concentrated nitric acid is easy to the generation NO that itself decomposesx, concentration is caused to reduce.When the temperature is low, concentrated nitric acid is not shown
Strong oxide etch effect.Wherein, the optimal reacting dose of the fluorescence quantum yield highest of A1 illustrates in A1-A4 isopropanol ash is
10mg.Two groups of description of test of A1 and A5：Activation process is conducive to the synthesis of fluorescent carbon point, and A5, can due to not carrying out activation process
It can so that carbon source activity is relatively low, is unfavorable for the generation of fluorescent carbon point.A6-A9：Illustrate that optimum temperature prepared by reaction is 140 DEG C.
It is synthesized higher or lower than fluorescent carbon point is unfavorable for.A1 and D1-D4 comparative illustrations：Isopropanol ash is optimal carbon source selection.From
Fluorescence quantum yield can be seen that the fluorescent quantum yield highest of A1, be optimal selection.A1 is compared with A10-A12
Bright identical carbon source concentration of nitric acid is bigger, is more conducive to the raising of fluorescence quantum yield, when A1 and A13-A17 comparative illustrations are reacted
Between be less than 2h when, fluorescence quantum yield with the reaction time increase and increase, illustrate fluorescent carbon point constantly synthesize in；During reaction
Between be more than 2h after, continuously decreased as the time increases fluorescence quantum yield, illustrate that nitric acid has fluorescent carbon point certain effect of corroding,
So that bulky grain carbon dots becomes smaller, little particle carbon dots is corroded, thus reduces the concentration of fluorescent carbon point.A1 and A18-
A20 comparisons show that ethyl acetate for optimal extractant, illustrates that the ethyl acetate is more advantageous to the fluorescent emission of carbon dots, according to document
Report is related to the polarity of solution.By above-mentioned experiment we determined that the optimal experimental program of this experiment：Activated different of 10mg
Propyl alcohol ashes are the nitric acid reflux 2h of 14mol/L in 20ml concentration, and ethyl acetate is as extractant.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail, within the scope of the technical concept of the present invention, a variety of simple variants can be carried out to technical scheme, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that the specific technical features described in the above specific embodiments, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (14)
1. a kind of preparation method of fluorescent carbon point, which is characterized in that the preparation method includes：
(1) after the cellulosic fabric containing isopropanol is burnt, ash content M1 is obtained；
(2) ash content M1 and oxidizing acid are subjected to oxidation reaction, fluorescent carbon point is made；Wherein, the oxidizing acid is selected from nitric acid.
2. preparation method according to claim 1, wherein, the nitric acid is carried by the salpeter solution that concentration is 2-14mol/L
For.
3. preparation method according to claim 2, wherein, the cellulosic fabric is selected from cotton fabric, flaxen fiber is knitted
Object or bamboo fiber.
4. preparation method according to claim 2, wherein, compared with the ash content M1 of 100mg, the salpeter solution
Dosage is 100-200mL.
5. preparation method according to claim 1 or 2, wherein, the reaction temperature of the oxidation reaction is 100-160 DEG C,
Reaction time is 0.5-3h.
6. preparation method according to claim 1 or 2, wherein, it is further included in step (1) and ash content M1 obtained lives
Change drying process, the activation drying process is that ash content M1 is placed at 100-150 DEG C dry 0.5-1h.
7. preparation method according to claim 1 or 2, wherein, it is further included in step (2) and carries out fluorescent carbon point obtained
High brightness fluorescent carbon dots is made in extraction.
8. preparation method according to claim 7, wherein, extractant is ethyl acetate.
9. preparation method according to claim 8, wherein, compared with the fluorescent carbon point of 100 parts by volume, the extractant
Dosage is 10-100 parts by volume.
10. fluorescent carbon point made from the preparation method in a kind of 1-9 according to claim described in any one.
11. a kind of filling composition of LED chip, which is characterized in that the filling composition includes appointing according in claim 1-9
Fluorescent carbon point or fluorescent carbon point according to claim 10 and adhesive made from preparation method described in meaning one.
12. filling composition according to claim 11, wherein, the fluorescent carbon point is 1-50 by the concentration of fluorescent carbon point
The fluorescent carbon point solution of weight % provides.
13. filling composition according to claim 12, wherein, the solvent in the fluorescent carbon point solution is acetic acid second
Ester.
14. filling composition according to claim 12, wherein, the dosage of the fluorescent carbon point solution and the adhesive
Volume ratio is 1：1-5.
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