CN109097024A - A kind of preparation method of vermiculite fluorescence membrane composite material - Google Patents
A kind of preparation method of vermiculite fluorescence membrane composite material Download PDFInfo
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Abstract
The present invention provides a kind of methods for preparing the ultra-thin film composite material of transparent fluorescent using exfoliated vermiculite material and organic fluorescence molecular material, it is prepared by the method for Supramolecular Assembling, so that the ultra-thin film composite material of organic-inorganic fluorescence obtained overcomes the defect of simple organic material and simple inorganic material, and the advantages of having both the two, the assembling of anion Yu anion body is realized simultaneously, fluorescence composite material obtained has longer fluorescence lifetime, have the characteristics that the transparency and solid state, has highly application value.
Description
Technical field
The present invention relates to a kind of preparation methods of fluorescent material, and in particular to a kind of system of vermiculite fluorescence membrane composite material
Preparation Method belongs to inorganic non-metallic pit wood material processing technique field.
Background technique
The definition of Supramolecular Assembling (Supramolecular assembly) is the polymolecular being combined by non-covalent bond
Group, it can be simply to two molecular compositions, they can be spherical shape, stick or sheet sample, research Supramolecular Assembling be for
Obtain a series of new materials, what Supramolecular Assembling was studied, which construct primitive, is mostly focused on molecule and nanoscale or micron
And assembling between micron scale above object etc., the performance of new material can be effectively controlled, realizes leaping for product quality.
Vermiculite is one of the nonmetallic minerals that there are preferable resource perspective and potential advantages in China, is a kind of important nonmetallic
The secondary metamorphic mineral of water aluminosilicate containing magnesium of mineral and a kind of layer structure belongs to phyllosilicate, cheap and easy to get；Energy
High temperature resistant is the non-conductor of heat, has good electrical insulating property；Expanded vermiculite is easy to water imbibition and hygroscopicity；It is swollen under high temperature
It is swollen, it is easily peeled off, and there is preferable interlayer cation exchange capacity, swelliong power, adsorption capacity, sound-proofing, thermal insulation, resistance to
The features such as fire, freexing tolerance, and chemical property is stablized, not soluble in water, nontoxic, tasteless, without side-effects, industrial mainly benefit
With its good absorption property and ion-exchange performance processing waste water containing heavy metal and organic cation, prepare anti-biotic material and
Thermal insulation material, vermiculite filter aid, cleanser and Organized Vermiculite etc..In fact, passing through how by preparing micron or nano-powder
Assembling goes to construct new composite material, is one of the mark achievement for improving vermiculite research level.But vermiculite be typical yin from
Sub- clay, itself is negatively charged, it is difficult to be self-assembly of orderly body, how be to expand vermiculite by assembling building new material therefore
The critical issue of basic research application.And organic cation fluorophor is widely used substance in LED product, but because its
There is a problem of that the service life is short for organism, and then largely effects on the performance of LED product.
Therefore how to assemble vermiculite material and organic cation fluorophor to form one using supermolecule package technique
Kind vermiculite fluorescence composite material and then the defect for overcoming organic cation phosphor lifetime short, construct vermiculite optical material, are these
Field technical staff's urgent problem to be solved.
Summary of the invention
Insufficient and short organic cation phosphor lifetime problem is developed and used for vermiculite, it is an object of the invention to
A kind of preparation method of vermiculite fluorescence membrane composite material is provided, combines the vermiculite of macroscopic view with organic cation fluorophor to be formed
A kind of composite material.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of preparation method of vermiculite fluorescence membrane composite material, comprising the following steps:
(1) add the removing of water Ultrasonic Heating to crush vermiculite, centrifuge washing separation, precipitating ultrasonic disperse after centrifugation to go from
In sub- water, nanometer sheet vermiculite solution is obtained；
(2) fluorescent molecule ultrasonic disperse is dissolved, obtains fluorescent molecule solution；
(3) transparency silica glass or PET film are handled, obtains hydrophily quartz glass or PET film；
(4) treated in the step (3) quartz glass or PET film are impregnated in fluorescent molecule solution, uses clear water
Washes clean is impregnated in vermiculite colloidal solution later, is impregnated with clear water washes clean, then in fluorescent molecule solution, is repeated to soak
Bubble process obtains the transparent composite material ultrathin membrane of vermiculite and the assembling of organic fluorescence molecule.
The beneficial effect of above scheme is: the vermiculite of molecular level and organic fluorescence molecule being passed through Supramolecular Assembling, and attached
On quartz glass or PET film, form a kind of ultra-thin film composite material of vermiculite fluorescence.
Preferably, 1-1000 nanometers of vermiculite partial size of nanometer sheet of gained, nanometer sheet vermiculite solution concentration are in the step (1)
0.001-1g/ml。
Preferably, step (1) supersonic frequency is 20Hz-1000MHz, and heating temperature is 40-350 DEG C, centrifugal rotational speed
For 8000-230000rpm.
The beneficial effect of above-mentioned optimal technical scheme is: by controlling centrifugal rotational speed, guaranteeing the leech in vermiculite colloidal solution
Stone is conducive to the progress of Supramolecular Assembling process in subsequent reactions in molecular level.
Further, the fluorescent molecule in the step (2) is pyrrole Luo Hong, rhodamine B 6G, cadmiumsulfide quantum dot, selenizing
One of cadmium quantum dot or cadmium telluride quantum dot.
Preferably, the cadmiumsulfide quantum dot, CdSe quantum dots and cadmium telluride quantum dot are living by cationic surface
Property agent modification be prepared into positively charged quantum dot.
Preferably, the cationic surfactant be cetyl ammonium bromide or bromohexadecane base trimethylpyridine or
Brocide or dodecylpyridinium bromide.
The beneficial effect of above-mentioned optimal technical scheme is: rhodamine B 6G and pyrrole Luo Hong itself are cationic fluorescent body, and
Cadmiumsulfide quantum dot, CdSe quantum dots and cadmium telluride quantum dot may carry anion, by modification, may be implemented
The layer assembly of anion and anion overcomes the defect that cannot be assembled with identical charges.
Preferably, the PET film in the step (3) or quartz glass processing are using radio-frequency power 0-5000W, radio frequency
The plasma of frequency 5-1000MHz and the ultraviolet light of uitraviolet intensity 0-3000uW/cm are handled, and time 1-30 points of processing
Clock.
The beneficial effect of above-mentioned optimal technical scheme is: plasma and ultraviolet while being handled, and destroys quartz glass
Or pet sheet face structure, make quartz glass or pet sheet face hydroxylating, water-wetted surface is become from hydrophobic surface, it is real by the method
It is now quick and easy, effectively, overcome the modified disadvantage of organic chemistry.
Preferably, fluorescent molecule and vermiculite soaking time are 0.1-60min in the step (4)；Washing time is 0.1-
30min。
Preferably, the number of occurrence is 2 times -100000 times in the step (4).
The beneficial effect of above-mentioned optimal technical scheme is: by repeatedly washing by soaking repeatedly, guarantee vermiculite molecule with it is organic
Fluorescent molecule forms Supramolecular Assembling composite material.
In conclusion the beneficial effects of the present invention are: provide a kind of preparation method of vermiculite fluorescence membrane composite material,
So that vermiculite and organic fluorescence molecular material are acted on by Supramolecular Assembling and are covered on shape in modified quartz glass or PET film
At a kind of fluorescence membrane composite material, vermiculite is typical inorganic object, and fluorescent molecule is organic matter, and shining with negative electrical charge is gathered
It closes object and is replaced assembling layer by layer with stratified material, form inorganic/organic composite ultrathin membrane, realize light emitting polymer molecule and exist
Interlayer generates orientation effect, to realize the microcosmic controllable of light functional polymer intermolecular distance, keeps it evenly dispersed in interlayer,
The luminous quenching phenomenon for effectively inhibiting the accumulation of photoactive molecules and generating, the characteristics of luminescence of acquisition not red shift, not wideization；Together
When also advantageously improve the physics and chemical stability of light emitting polymer, solve present in organic luminescence polymer device
The problem that stability is poor, service life is short has very high application value in field of light emitting materials, it is important that the present invention is logical
The modified control for crossing micellar structure, realizes the assembling of electronegative vermiculite Yu electronegative fluorescence quantum.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 attached drawing is the nature that material made from the embodiment of the present invention 2 acts on fluorescence membrane group based on electrostatic alternating sorbent
Light (a) and fluorescence (b) figure；
Fig. 2 attached drawing is material made from the embodiment of the present invention 2 based on the ultraviolet of electrostatic alternating sorbent effect fluorescence membrane group
Spectrogram；
Fig. 3 attached drawing is that material made from the embodiment of the present invention 2 is based on electrostatic alternating sorbent effect fluorescence membrane group in difference
Linear fit under wavelength；
Fig. 4 attached drawing is that material made from the embodiment of the present invention 2 is based on electrostatic alternating sorbent effect fluorescence membrane group fluorescence hair
Penetrate spectrogram；
Fig. 5 attached drawing is that material made from the embodiment of the present invention 2 is strong based on electrostatic alternating sorbent effect fluorescence membrane group fluorescence
Spend linear fit.
Specific embodiment
A specific embodiment of the invention is described further below.
Unless otherwise instructed, raw material employed in the present invention is commercially available or commonly used in the art.
Vermiculite is combined to form one by a kind of preparation method of vermiculite fluorescence membrane composite material with organic cation fluorophor
Kind composite material, specifically adopts the following technical scheme that, comprising the following steps:
(1) vermiculite is added into water 20Hz-1000MHz ultrasound and is heated to 40-350 DEG C of removing and crushed, use 8000- later
The revolving speed centrifuge washing of 230000rpm separates, and the precipitating ultrasonic disperse after centrifugation obtains 1-1000 nanometers into deionized water
Nanometer sheet vermiculite solution, and nanometer sheet vermiculite solution concentration is 0.001-1g/ml；
(2) by pyrrole Luo Hong or rhodamine B 6G or cadmiumsulfide quantum dot or CdSe quantum dots or cadmium telluride quantum dot ultrasound
Dispersing and dissolving obtains fluorescent molecule solution；
(3) transparency silica glass or PET film are used into radio-frequency power 0-5000W, rf frequency 5-1000MHz it is equal from
The ultraviolet light of daughter and uitraviolet intensity 0-3000uW/cm are handled, and are handled time 1-30 minutes, are obtained hydrophily quartz glass
Glass or PET film；
(4) treated in step (3) quartz glass or PET film are impregnated into 0.1-60min in fluorescent molecule solution, used
Clear water washs 0.1-30min, impregnates 0.1-60min in vermiculite colloidal solution later, washs 0.1-30min with clear water, then
Fluorescent molecule solution impregnates 0.1-60min, repeats immersion and washing process 2-100000 times, obtains vermiculite and organic fluorescence molecule
The transparent composite material ultrathin membrane of assembling.
In order to advanced optimize above scheme, cadmiumsulfide quantum dot, CdSe quantum dots and cadmium telluride quantum dot pass through
Cationic surfactant modification is prepared into positively charged quantum dot, and cationic surfactant be cetyl ammonium bromide or
Bromohexadecane base trimethylpyridine or brocide or dodecylpyridinium bromide.
Specific embodiment is as follows shown in each embodiment.
Embodiment 1
A kind of preparation method of vermiculite fluorescence membrane composite material, comprising the following steps:
(1) vermiculite is added into water 20Hz ultrasound and is heated to 40 DEG C of removings and crushed, centrifuge divides in the case where revolving speed is 10000rpm
From mixture, the precipitation solid redisperse after centrifugation obtains nanometer sheet vermiculite solution into pure water；
(2) by rhodamine B 6G ultrasonic dissolution, rhodamine B 6G fluorescent molecule solution is obtained；
(3) ultraviolet light that the plasma and intensity for being 5MHz with rf frequency by clear PET film are 3000uW/cm into
Row processing, obtains hydrophily PET film；
(4) treated in step (3) PET film is impregnated 10 minutes in rhodamine B 6G fluorescent molecule solution, uses clear water
Washing 3 minutes, impregnates 10 minutes in vermiculite colloidal solution later, is washed 3 minutes with clear water, then in rhodamine B 6G fluorescence point
Sub- solution impregnates 5 minutes, 32 times repeatedly, obtains the transparent composite material film of vermiculite and fluorescent molecule assembling.
Embodiment 2
A kind of preparation method of vermiculite fluorescence membrane composite material, comprising the following steps:
(1) vermiculite is added into water 200Hz ultrasound and is heated to 100 DEG C of removings and crushed, centrifuge is in the case where revolving speed is 15000rpm
Separating mixture, the precipitation solid redisperse after centrifugation obtain nanometer sheet vermiculite solution into pure water；
(2) by the modified cadmiumsulfide quantum dot ultrasonic dissolution of bromohexadecane base trimethylpyridine, cadmium sulfide amount is obtained
Son point fluorescent molecule solution；
(3) be 100W with radio-frequency power by transparency silica glass, the plasma that rf frequency is 200MHz is handled,
Obtain hydrophily quartz glass；
(4) treated in step (3) quartz glass is impregnated 10 minutes in cadmiumsulfide quantum dot fluorescent molecule solution, is used
Clear water washs 5 minutes, impregnates 10 minutes, is washed 5 minutes with clear water, then in cadmiumsulfide quantum dot in vermiculite colloidal solution later
Fluorescent molecule solution impregnates, and 36 times repeatedly, obtains the transparent composite material film of vermiculite and fluorescent molecule assembling.
Embodiment 3
A kind of preparation method of vermiculite fluorescence membrane composite material, comprising the following steps:
(1) vermiculite is added into water 400Hz ultrasound and is heated to 150 DEG C of removings and crushed, centrifuge is in the case where revolving speed is 20000rpm
Separating mixture, the precipitation solid redisperse after centrifugation obtain nanometer sheet vermiculite solution into pure water；
(2) by the modified cadmium telluride quantum dot ultrasonic dissolution of cetyl ammonium bromide, cadmium telluride quantum dot fluorescence is obtained
Molecular solution；
(3) be 300W with radio-frequency power by clear PET film, the plasma that rf frequency is 400MHz and intensity are
The ultraviolet light of 2000uW/cm is handled, and hydrophily PET film is obtained；
(4) treated in step (3) PET film is impregnated 10 minutes in cadmium telluride quantum dot fluorescent molecule solution, is used
Clear water washs 10 minutes, impregnates 10 minutes, is washed 10 minutes with clear water, then in cadmium telluride quantum in vermiculite colloidal solution later
Point fluorescent molecule solution impregnates, and 40 times repeatedly, obtains the transparent composite material film of vermiculite and fluorescent molecule assembling.
Embodiment 4
A kind of preparation method of vermiculite fluorescence membrane composite material, comprising the following steps:
(1) vermiculite will be added to water 1000Hz ultrasound and be heated to 350 DEG C of removings and crushed, centrifuge is 23000rpm in revolving speed
Lower separating mixture, the precipitation solid redisperse after centrifugation obtain nanometer sheet vermiculite solution into pure water；
(2) by pyrrole Luo Hong ultrasonic dissolution, pyrrole Luo Hong fluorescent molecule solution is obtained；
(3) be 500W with radio-frequency power by clear PET film, the plasma that rf frequency is 1000MHz and intensity are
The ultraviolet light of 3000uW/cm is handled, and hydrophily PET film is obtained；
(4) treated in step (3) PET film is impregnated 12 minutes in pyrrole Luo Hong fluorescent molecule solution, is washed with clear water
It washs 5 minutes, impregnates 12 minutes in vermiculite colloidal solution, washed 5 minutes with clear water later, then in pyrrole Luo Hong fluorescent molecule solution
It impregnates, 50 times repeatedly, obtains the transparent composite material film of vermiculite and fluorescent molecule assembling.
Embodiment 5
A kind of preparation method of graphene fluorescence membrane composite material, comprising the following steps:
(1) by graphene add water supersonic frequency be 20Hz-1000MHz, heating temperature be 40-350 DEG C under conditions of into
Row dispersion, obtains graphene colloidal solution；
(2) by pyrrole Luo Hong, rhodamine B 6G, cetyl ammonium bromide or bromohexadecane base trimethylpyridine or bromination pyrrole
The modified cadmium telluride quantum dot of pyridine, CdSe quantum dots or cadmiumsulfide quantum dot ultrasonic dissolution, obtain fluorescent molecule solution；
(3) transparency silica glass or PET film are used into radio-frequency power 0-5000W, rf frequency 5-1000MHz it is equal from
The ultraviolet light of daughter and uitraviolet intensity 0-3000uW/cm are handled, and are handled the time 30 minutes, are obtained hydrophily quartz glass
Or PET film；
(4) treated in step (3) quartz glass or PET film are impregnated 11 minutes in organic fluorescence molecular solution,
It is washed 6 minutes with clear water, impregnates 11 minutes, washed 6 minutes with clear water, then in organic fluorescence in graphene colloidal solution later
Molecular solution impregnates, and 32 times repeatedly, obtains the transparent composite material film of graphene and fluorescent molecule assembling.
Embodiment 6
A kind of preparation method of molybdenum sulfide fluorescence membrane composite material, comprising the following steps:
(1) by molybdenum sulfide add water supersonic frequency be 20Hz-1000MHz, heating temperature be 40-350 DEG C under conditions of point
It dissipates, obtains molybdenum sulfide colloidal solution；
(2) by pyrrole Luo Hong or rhodamine B 6G or cetyl ammonium bromide or bromohexadecane base trimethylpyridine or bromination
The modified cadmium telluride quantum dot of pyridine or cadmiumsulfide quantum dot ultrasonic dissolution, obtain organic fluorescence molecular solution；
(3) transparency silica glass or PET film are used into radio-frequency power 0-5000W, rf frequency 5-1000MHz it is equal from
The ultraviolet light of daughter and uitraviolet intensity 0-3000uW/cm are handled, and are handled the time 30 minutes, are obtained hydrophily quartz glass
Or PET film；
(4) treated in step (3) quartz glass or PET film are impregnated 10 minutes in organic fluorescence molecular solution,
It is washed 4 minutes with clear water, impregnates 10 minutes, washed 4 minutes with clear water, then in organic fluorescence in molybdenum sulfide colloidal solution later
Molecular solution impregnates, and 32 times repeatedly, obtains the transparent composite material film of molybdenum sulfide and fluorescent molecule assembling.
Comparative example 1
This programme is the simple fluorescent molecule material without supramolecular assembly.
Performance test
Ultraviolet and fluorescence detection is carried out to fluorescence membrane composite material made from embodiment 2, analyzes the assembling of the number of plies
Quantity, the imparted relationship degree of fitting of film is 0.99 or more, and fluorescence linear relationship degree of fitting is also 0.99 or more.Its is glimmering
The light service life improves about 13 times.As a result as shown in attached drawing 1-5: from Fig. 1 (a) as can be seen that assembled quartz glass is too
Be under sunlight it is colorless and transparent, from Fig. 1 (b) as can be seen that assembled quartz glass is hair red fluorescence under ultraviolet light.
Fig. 1 shows to realize the preparation of transparent vermiculite and fluorescent molecule material.Fig. 2 and Fig. 3 be vermiculite under the fluorescent molecule difference number of plies
Ultraviolet spectra, Fig. 2 show the increase with the number of plies, and absorbance gradually increases, and Fig. 3 is at wavelength 360nm, 500nm and 700nm
Matched curve, degree of fitting illustrates that the vermiculite number of plies is effectively controlled all 0.99 or more.Fig. 4 and Fig. 5 is vermiculite and fluorescence point
Fluorescence spectrum under the sub- difference number of plies, Fig. 4 show that its wave spectrum is gradually increased with the increase of the number of plies, fluorescence absorbance, and Fig. 5 is in wave
Matched curve under long 617.5nm, degree of fitting illustrate that the fluorescent molecule number of plies is effectively controlled also 0.99 or more.The above reality
It tests and shows to assemble by the vermiculite colloidal solution and fluorescent molecule of preparation, and its fluorescence lifetime greatly improves, and realizes vermiculite
The preparation of transparent fluorescent film.
Fluorescent material life test:
Fluorescence membrane composite material obtained in above-described embodiment 1-6 and the fluorescent molecule material of comparative example 1 are sent out
Light life test, the result is as follows:
As can be seen from the above test results that fluorescence membrane composite material obtained by technical solution provided by the invention is taken to have
There is longer fluorescence lifetime, has highly application value in fluorescent material field.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.
Claims (10)
1. a kind of preparation method of vermiculite fluorescence membrane composite material, which comprises the following steps:
(1) removing of water Ultrasonic Heating is added to crush vermiculite, centrifuge washing separates, the precipitating ultrasonic disperse after centrifugation to deionized water
In, obtain nanometer sheet vermiculite solution；
(2) fluorescent molecule ultrasonic disperse is dissolved, obtains fluorescent molecule solution；
(3) transparency silica glass or PET film are handled, obtains hydrophily quartz glass or PET film；
(4) treated in the step (3) quartz glass or PET film are impregnated in fluorescent molecule solution, is washed with clear water
Completely, it impregnates, is impregnated with clear water washes clean, then in fluorescent molecule solution, repetition was impregnated in vermiculite colloidal solution later
Journey obtains the transparent composite material ultrathin membrane of vermiculite and the assembling of organic fluorescence molecule.
2. a kind of preparation method of vermiculite fluorescence membrane composite material according to claim 1, which is characterized in that the step
Suddenly 1-1000 nanometers of vermiculite partial size of nanometer sheet of gained in (1), nanometer sheet vermiculite solution concentration are 0.001-1g/ml.
3. a kind of preparation method of vermiculite fluorescence membrane composite material according to claim 1, which is characterized in that the step
Suddenly supersonic frequency is 20Hz-1000MHz in (1), and heating temperature is 40-350 DEG C, centrifugal rotational speed 8000-230000rpm.
4. a kind of preparation method of vermiculite fluorescence membrane composite material according to claim 1, which is characterized in that the step
Suddenly the fluorescent molecule in (2) is in pyrrole Luo Hong, rhodamine B 6G, cadmiumsulfide quantum dot, CdSe quantum dots or cadmium telluride quantum dot
One kind.
5. a kind of preparation method of vermiculite fluorescence membrane composite material according to claim 4, which is characterized in that the sulphur
Cadmium quantum dot, CdSe quantum dots and cadmium telluride quantum dot are prepared by cationic surfactant modification positively charged
Quantum dot.
6. a kind of preparation method of vermiculite fluorescence membrane composite material according to claim 5, which is characterized in that the sun
Ionic surface active agent is cetyl ammonium bromide or bromohexadecane base trimethylpyridine or brocide or ten
Dialkyl group pyridinium bromide.
7. a kind of preparation method of vermiculite fluorescence membrane composite material according to claim 1, which is characterized in that the step
Suddenly the PET film in (3) or quartz glass processing are using radio-frequency power 0-5000W, the plasma of rf frequency 5-1000MHz
The ultraviolet light of body and uitraviolet intensity 0-3000uW/cm are handled, and are handled time 1-30 minutes.
8. a kind of preparation method of vermiculite fluorescence membrane composite material according to claim 1, which is characterized in that the step
Suddenly fluorescent molecule and vermiculite soaking time are 0.1-60mi n in (4)；Washing time is 0.1-30mi n.
9. a kind of preparation method of vermiculite fluorescence membrane composite material according to claim 1, which is characterized in that the step
Suddenly the number of occurrence is 2 times -100000 times in (4).
10. a kind of vermiculite fluorescence membrane composite material, which is characterized in that be made using the method for any one of claim 1-9.
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| JP2009161642A (en) * | 2007-12-28 | 2009-07-23 | National Institute Of Advanced Industrial & Technology | Flexible fluorescent film containing clay as principal component |
| US20120107624A1 (en) * | 2009-04-07 | 2012-05-03 | Inbio Prof. Jurgen Buddefeld Dr. Peter Klauth Prof. Manfred Rietz | Modification of layered silicates for luminescence activation |
| CN106634943A (en) * | 2016-12-14 | 2017-05-10 | 塔里木大学 | Method of preparing thermochromic sensing material from vermiculite |
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