CN108526457A - Titanium quantum dot and its preparation method and application - Google Patents
Titanium quantum dot and its preparation method and application Download PDFInfo
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- CN108526457A CN108526457A CN201810299354.9A CN201810299354A CN108526457A CN 108526457 A CN108526457 A CN 108526457A CN 201810299354 A CN201810299354 A CN 201810299354A CN 108526457 A CN108526457 A CN 108526457A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K41/00—Medicinal preparations obtained by treating materials with wave energy or particle radiation ; Therapies using these preparations
- A61K41/0052—Thermotherapy; Hyperthermia; Magnetic induction; Induction heating therapy
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P35/00—Antineoplastic agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y5/00—Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery
Abstract
The present invention provides a kind of titanium quantum dot, the size of the titanium quantum dot is less than or equal to 20nm.Titanium quantum dot provided by the invention have many advantages, such as environmental-friendly, biocompatibility is high, full spectrum it is strong absorption and high photothermal conversion efficiency, have excellent light thermal property.The present invention also provides a kind of preparation methods of titanium quantum dot, include the following steps:Titanium material is provided, the titanium material is removed using liquid phase stripping method, obtains titanium quantum dot, the size of the titanium quantum dot is less than or equal to 20nm.Titanium quantum dot is made by non-laminar titanium material in the method that the present invention uses liquid phase stripping for the first time, and preparation method is simple to operation.The titanium quantum dot can be used as photo-thermal therapy formulation application in oncotherapy.
Description
Technical field
The present invention relates to field of nanometer material technology, and in particular to a kind of titanium quantum dot and its preparation method and application.
Background technology
Oncotherapy is always that the mankind are difficult to overcome field.Traditional treatment means include operating on, chemotherapy, putting
It treats.But these treatment means have the characteristics that treatment time length and toxic side effect are big, and bring great pain to patient.It is red
Outer photo-thermal therapy is a kind of emerging treatment means, has the characteristics that treatment time is short and damages small.Recently, infrared photo-thermal therapy
It is even more to have started the upsurge of one treating cancer by nano material.General photo-thermal nano material includes noble metal, such as gold,
Emerging two-dimensional materials with some, including graphene, molybdenum disulfide, black phosphorus, tellurium, titanium carbide etc..
The infrared required performance of optothermal material includes that nontoxic, strong infrared absorption and high photothermal conversion efficiency etc. are special
Point.And these optothermal materials studied at present are less able to fully meet the performance of these needs.Therefore, for photo-thermal material
The exploitation of material is imperative.
Invention content
To solve the above problems, the present invention provides a kind of titanium quantum dot, the titanium quanta point biological compatibility is good, together
When light thermal property it is excellent.
First aspect present invention provides a kind of titanium quantum dot, and the size of the titanium quantum dot is less than or equal to 20nm.
Wherein, the size of the titanium quantum dot is 1-10nm.
Wherein, the light absorption wavelength ranging from 200-2000nm of the titanium quantum dot.
First aspect present invention provide titanium quantum dot have environmental-friendly, bio-compatibility, full spectrum it is strong absorb and
The advantages that higher photothermal conversion efficiency.Therefore, there is excellent light thermal property.
Second aspect of the present invention provides a kind of preparation method of titanium quantum dot, includes the following steps:
Titanium material is provided, the titanium material is removed using liquid phase stripping method, obtains titanium quantum dot, the titanium quantum
The size of point is less than or equal to 20nm.
Wherein, the liquid phase stripping method specifically includes following operation:
The titanium material is added into polar solvent, Probe Ultrasonic Searching 10-15h is used under ice bath environment;The probe
After ultrasound, then water bath sonicator is used, the water bath sonicator time is 6-15h, and the temperature of the water-bath is kept for 5-15 DEG C;Institute
After stating water bath sonicator, titanium quantum dot is centrifuged and is dried to obtain.
Wherein, the power of the Probe Ultrasonic Searching is 250-300W;The water bath sonicator power is 350-400W.
Wherein, the polar solvent includes at least one of isopropanol, ethyl alcohol, water and N-Methyl pyrrolidone.
Wherein, a concentration of 1-7mg/mL of the titanium material in the polar solvent.
Wherein, the operation of the centrifugation includes:
The centrifugal force for using 5000-8000g first, centrifuges 20-35min, takes supernatant;Then the supernatant is used
The centrifugal force of 10000-13000g continues to centrifuge 20-35min, and it is the titanium quantum dot to obtain precipitation.
Second aspect of the present invention provides a kind of preparation method of titanium quantum dot, uses the method for liquid phase stripping by non-for the first time
Titanium quantum dot is made in the titanium material of stratiform, and preparation method is simple to operation.
Third aspect present invention provides a kind of titanium quantum dot as described above as answering in photo-thermal therapy preparation
With.
To sum up, advantageous effect of the present invention includes the following aspects:
1, titanium quantum dot provided by the invention have environmental-friendly, bio-compatibility, full spectrum it is strong absorb and it is higher
The advantages that photothermal conversion efficiency, has excellent light thermal property;
2, the preparation method of titanium quantum dot provided by the invention, for the first time using the method for stripping by non-laminar titanium material system
Titanium quantum dot is obtained, preparation method is simple to operation;
3, titanium quantum dot provided by the invention can be used as photo-thermal therapy formulation application.
Description of the drawings
Fig. 1 is the transmission electron microscope picture of titanium quantum dot made from embodiment 1;
Fig. 2 is the abosrption spectrogram of the liquid phase stripping process in different solvents;
Fig. 3 is the abosrption spectrogram of the liquid phase stripping process of different ultrasonic times;
Fig. 4 is the titanium quantum dot aqueous dispersions photo of various concentration;
Fig. 5 is the abosrption spectrogram of the titanium quantum dot aqueous dispersions of various concentration;
Fig. 6 is the extinction coefficient of titanium quantum dot;
Fig. 7 is the heating curve of the titanium quantum dot aqueous dispersions of various concentration;
Fig. 8 is the photothermal conversion efficiency of titanium quantum dot aqueous dispersions;
Fig. 9 is the cytotoxicity assay result figure of titanium quantum dot.
Specific implementation mode
As described below is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also considered as
Protection scope of the present invention.
" the titanium quantum dot " or " titanium " that the present invention mentions removes specified otherwise, refers to simple substance titanium.
Embodiment of the present invention first aspect provides a kind of titanium quantum dot, and the size of the titanium quantum dot is less than or equal to
20nm。
In embodiment of the present invention, the size of the titanium quantum dot is 1-10nm.Optionally, the size of the titanium quantum dot
For 10-20nm.Still optionally further, the size of the titanium quantum dot is 1-5nm.Still optionally further, the titanium quantum dot
Size is 5-10nm.Still optionally further, the size of the titanium quantum dot is 2-3nm.Still optionally further, the titanium quantum dot
Size be 1nm, 2nm, 3nm, 4nm, 5nm, 6nm, 7nm, 8nm, 9nm, 10nm, 11nm, 12nm, 13nm, 14nm, 15nm,
16nm, 17nm, 18nm, 19nm or 20nm.Optionally, the number of plies of the titanium quantum dot is not done specifically limited.It is mentioned here
What " size " of titanium quantum dot referred to is also " diameter " of titanium quantum dot.
The titanium quantum dot size that embodiment of the present invention provides is smaller, and smaller size contributes to titanium quantum dot swollen
Tumor position has preferable passive concentration effect, and is easy from internal discharge, and biocompatibility is good.Meanwhile the titanium quantum
The photo-thermal effect of point is apparent.
In embodiment of the present invention, the titanium quantum dot has the absorption from visible region to near-infrared region.Optionally,
The light absorption wavelength ranging from 200-2000nm of the titanium quantum dot.
In embodiment of the present invention, the photothermal conversion efficiency of the titanium quantum dot is more than or equal to 60%.
First aspect present invention provide titanium quantum dot have environmental-friendly, bio-compatibility, full spectrum it is strong absorb and
The advantages that higher photothermal conversion efficiency, has excellent light thermal property.
Second aspect of the embodiment of the present invention provides a kind of preparation method of titanium quantum dot, includes the following steps:
Titanium material is provided, the titanium material is removed using liquid phase stripping method, obtains titanium quantum dot, the titanium quantum
The size of point is less than or equal to 20nm.
In embodiment of the present invention, the titanium material is the non-laminar Titanium simple substance of two dimension, can be such as titanium valve, such as grain
Diameter is micron-sized titanium valve, and it is tens microns or titanium valve below to be specifically as follows grain size.May be titanium block, it is big to its
Small and shape is not particularly limited.If titanium material is the larger titanium block of grain size, first titanium block can be ground, used after grinding
It is removed in liquid phase.The titanium material can be by being commercially available.
In embodiment of the present invention, the liquid phase stripping method specifically includes following operation:
The titanium material is added into polar solvent, Probe Ultrasonic Searching 10-15h is used under ice bath environment;The probe
After ultrasound, then water bath sonicator is used, the water bath sonicator time is 6-15h, and the temperature of the water-bath is kept for 5-15 DEG C;Institute
After stating water bath sonicator, titanium quantum dot is centrifuged and is dried to obtain.
Optionally, the polar solvent includes at least one in isopropanol, ethyl alcohol, water and N-Methyl pyrrolidone (NMP)
Kind.Optionally, the polar solvent includes at least one of isopropanol, ethyl alcohol and N-Methyl pyrrolidone (NMP).The present invention
The solvent of use can remove titanium material, and titanium quantum dot is made.
Optionally, a concentration of 1-7mg/mL of the titanium material in the polar solvent.
Optionally, the power of the Probe Ultrasonic Searching is 250-300W.Still optionally further, the power of the Probe Ultrasonic Searching is
250W, 260W, 270W, 280W, 290W or 300W.
Optionally, the time of the Probe Ultrasonic Searching is 10h, 11h, 12h, 13h, 14h or 15h.
Optionally, the Probe Ultrasonic Searching is non-continuous ultrasound, and it is 2/4s to select the ultrasonic ON/OFF time, i.e., first ultrasound 2s, so
Ultrasonic probe is closed afterwards and keeps 4s, is continuing ultrasound 2s, and so on.
Optionally, the water bath sonicator power is 350-400W.Still optionally further, the water bath sonicator power is
350W, 360W, 370W, 380W, 390W or 400W.
Optionally, the time of the water bath sonicator is 10-15h.Specifically, the time of the water bath sonicator be 6h, 7h,
8h, 9h, 10h, 11h, 12h, 13h, 14h or 15h.
Optionally, the bath temperature is kept for 10 DEG C.
Optionally, it after ultrasound, is centrifuged, the operation of the centrifugation includes:The centrifugal force of 5000-8000g is used first,
20-35min is centrifuged, supernatant is taken;Then the supernatant is continued to centrifuge 20- using the centrifugal force of 10000-13000g
35min, it is the titanium quantum dot to obtain precipitation.Optionally, the mode of the drying is unlimited, may be, for example, vacuum drying.The
The slow-speed of revolution centrifugation of one step is to detach the larger-size part titanium quantum dot of removal, and second step is centrifuged at a high speed i.e.
The titanium quantum dot of size needed for obtaining.
Prior art generally use liquid phase stripping method is used for removing two-dimensional layer material.And the present invention uses liquid phase stripping method
The non-laminar metal material of stripping two dimension, and it is successful.
Second aspect of the present invention provides a kind of preparation method of titanium quantum dot, uses the method for liquid phase stripping by non-for the first time
Titanium quantum dot is made in the titanium material of stratiform, and preparation method is simple to operation.
Third aspect present invention provides a kind of titanium quantum dot as described above as answering in photo-thermal therapy preparation
With.
Since the titanium quantum dot of the present invention has good biocompatibility and photothermal conversion performance, it can be very
It is used as photo-thermal therapy preparation for treating disease well.
Embodiment 1:
A kind of preparation method of titanium quantum dot, includes the following steps:
(1) titanium valve of 500mg is added in the isopropanol of 100mL.Then selection Probe Ultrasonic Searching 250W, ultrasonic 15h.Selection
The ultrasonic ON/OFF time is 2/4s, and is that ultrasound is carried out under ice bath environment.After Probe Ultrasonic Searching is complete, water bath sonicator is then used.
Water bath sonicator power is 360W.Ultrasonic time is 12h.Bath temperature is kept for 10 DEG C;
(2) the metal simple-substance titanium quantum dot that ultrasound is needed using the method for centrifugation later.First use 5000g from
Mental and physical efforts centrifuge 35min.Supernatant is taken, then continues to centrifuge 25min using 12000g by supernatant, be precipitated, after vacuum drying i.e.
Obtain titanium quantum dot.
Fig. 1 is the Electronic Speculum shape appearance figure of metal simple-substance titanium quantum dot.As shown in Figure 1, the size of titanium quantum dot is less than 10nm.Cause
This can separate Titanium quantum dot really by the observation of transmission electron microscope by liquid phase stripping method.
As shown in Fig. 2, respectively removed in isopropanol (IPA) and water, the absorption spectrum of the titanium quantum dot of same concentrations.
It is obvious that the absorption spectrum for the titanium quantum dot removed in IPA has the slope of higher absorption value and bigger (i.e. in Fig. 2 above
A curve).This illustrates fully remove bigger titanium particle at smaller titanium quantum dot in IPA.Further, than
Compared with the absorption value (as shown in Figure 3) of different splitting times (referring to the water bath sonicator time), the increasing with splitting time is found
Add, absorption spectrum is being continuously increased, and will appear the state of a saturation.
Embodiment 2:
A kind of preparation method of titanium quantum dot, includes the following steps:
(1) titanium valve of 500mg is added in the N-Methyl pyrrolidone of 100mL.Then Probe Ultrasonic Searching 300W, ultrasound are selected
10h.It is 2/4s to select the ultrasonic ON/OFF time, and is that ultrasound is carried out under ice bath environment.After Probe Ultrasonic Searching is complete, then use
Water bath sonicator.Water bath sonicator power is 350W.Ultrasonic time is 15h.Bath temperature is kept for 15 DEG C;
(2) the metal simple-substance titanium quantum dot that ultrasound is needed using the method for centrifugation later.First use 8000g from
Mental and physical efforts centrifuge 20min.Supernatant is taken, then continues to centrifuge 35min using 10000g by supernatant, be precipitated, after vacuum drying i.e.
Obtain titanium quantum dot.
Embodiment 3:
A kind of preparation method of titanium quantum dot, includes the following steps:
(1) titanium valve of 500mg is added in the ethyl alcohol of 100mL.Then selection Probe Ultrasonic Searching 280W, ultrasonic 12h.Selection is super
The sound ON/OFF time is 2/4s, and is that ultrasound is carried out under ice bath environment.After Probe Ultrasonic Searching is complete, water bath sonicator is then used.Water
Bath ultrasonic power is 400W.Ultrasonic time is 6h.Bath temperature is kept for 5 DEG C;
(2) the metal simple-substance titanium quantum dot that ultrasound is needed using the method for centrifugation later.First use 7000g from
Mental and physical efforts centrifuge 25min.Supernatant is taken, then continues to centrifuge 20min using 13000g by supernatant, be precipitated, after vacuum drying i.e.
Obtain titanium quantum dot.
Effect example
(1) test of absorption spectrum and light thermal property
Prepare the aqueous dispersions absorbance spectrum and light thermal property of various concentration.Absorption spectrum is using ultraviolet-light splitting light
Degree meter measures.Photo-thermal tests us and uses 808nm laser.The titanium quantum dot aqueous dispersions of 10,25,50 and 100ppm are prepared respectively
(as shown in Figure 4).The aqueous dispersions of preparation are respectively charged into quartz colorimetric utensil, is put into ultraviolet specrophotometer card slot and measures
Trap.The absorption curve of various concentration is as shown in Figure 5.The delustring system of titanium quantum dot can be obtained according to the absorption at 808nm
Number is 17.6Lg-1cm-1(as shown in Figure 6).The value is higher than black phosphorus (14.8Lg-1cm-1) extinction coefficient.For photo-thermal experiment
It measures, takes the titanium quantum dot aqueous dispersions of 1mL various concentrations to be added in cuvette, be irradiated using 808nm laser, and simultaneously
Temperature curve is recorded with thermocouple.The temperature of the titanium quantum dot of various concentration is shown with the heating of laser irradiation time in Fig. 7
Figure.By quantitative calculating, the photothermal conversion efficiency that can obtain titanium quantum dot is 65.4% (as shown in Figure 8).
The photothermal conversion efficiency (65.4%) of the titanium quantum dot of present invention highest in the light thermit powder being had been reported that, higher than biography
The gold nano grain (21%) of system and emerging two-dimentional light thermit powder:Including MoS2(24.4%), black phosphorus quantum dot (28.4%),
Ti3C2Nanometer sheet (30.6%) and antimony quantum dot (45.5%), therefore, titanium quantum dot light thermal conversion efficiency value are apparently higher than other
The current light thermit powder studied.
Therefore, titanium quantum dot produced by the present invention has the absorption of full spectrum and higher photothermal conversion efficiency, photo-thermal
It can be good.
(2) parameter in bio kinetic model of titanium quantum dot
The titanium quantum dot of different quality is scattered in cell culture medium, then is incubated altogether from different cells, then measures cell
Vigor.Hepatocellular carcinoma cells SMMC-7721 is taped against in 96 orifice plates first, after cell adherent (about 12 hours), is prepared
For testing.With the titanium amount that DMEM high glucose mediums difference compound concentration is 0,10,20,50,100,200 and 400 mg/litres
Son point dispersion liquid.100 microlitres of dispersion liquids are taken, the culture medium in aforementioned 96 orifice plate is replaced, after being incubated 24 hours, use CCK8
The vigor of cell, 3 parallel holes of each group of experimental setup inside each hole of kit measurement.As shown in figure 9, with titanium quantum dot
The raising (mg/litre from 0 to 400) of concentration, and do not add negative control group (Mock) comparison of titanium quantum dot, cell viability is simultaneously
Decline without apparent.This illustrates that titanium quantum dot does not have apparent cytotoxicity.
In conclusion titanium quantum dot shows its biocompatibility and safe and non-toxic advantage.
To sum up, titanium quantum dot produced by the present invention has good light thermal property, has both good biocompatibility, light
Fuel factor can be used for cell killing and the oncotherapy based on cellkilling capacity.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
Cannot the limitation to the scope of the claims of the present invention therefore be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of titanium quantum dot, which is characterized in that the size of the titanium quantum dot is less than or equal to 20nm.
2. titanium quantum dot as described in claim 1, which is characterized in that the size of the titanium quantum dot is 1-10nm.
3. titanium quantum dot as described in claim 1, which is characterized in that the light absorption wavelength ranging from 200- of the titanium quantum dot
2000nm。
4. a kind of preparation method of titanium quantum dot, which is characterized in that include the following steps:
Titanium material is provided, the titanium material is removed using liquid phase stripping method, obtains titanium quantum dot, the titanium quantum dot
Size is less than or equal to 20nm.
5. the preparation method of titanium quantum dot as claimed in claim 4, which is characterized in that the liquid phase stripping method specifically include with
Lower operation:
The titanium material is added into polar solvent, Probe Ultrasonic Searching 10-15h is used under ice bath environment;The Probe Ultrasonic Searching
After, then water bath sonicator is used, the water bath sonicator time is 6-15h, and the temperature of the water-bath is kept for 5-15 DEG C;The water
After bath ultrasound, titanium quantum dot is centrifuged and is dried to obtain.
6. the preparation method of titanium quantum dot as claimed in claim 5, which is characterized in that the power of the Probe Ultrasonic Searching is 250-
300W;The water bath sonicator power is 350-400W.
7. the preparation method of titanium quantum dot as claimed in claim 5, which is characterized in that the polar solvent include isopropanol,
At least one of ethyl alcohol, water and N-Methyl pyrrolidone.
8. the preparation method of titanium quantum dot as claimed in claim 5, which is characterized in that the titanium material is in the polar solvent
In a concentration of 1-7mg/mL.
9. the preparation method of titanium quantum dot as claimed in claim 5, which is characterized in that the operation of the centrifugation includes:
The centrifugal force for using 5000-8000g first, centrifuges 20-35min, takes supernatant;Then the supernatant is used
The centrifugal force of 10000-13000g continues to centrifuge 20-35min, and it is the titanium quantum dot to obtain precipitation.
10. a kind of titanium quantum dot as claimed in any one of claims 1-3 is as the application in photo-thermal therapy preparation.
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WO2019184201A1 (en) * | 2018-03-30 | 2019-10-03 | 张晗 | Titanium quantum dot-based nano titanium photo-thermal preparation and preparation method therefor |
CN109439323A (en) * | 2018-09-28 | 2019-03-08 | 深圳大学 | Beta oxidation Asia lead quantum dot and preparation method thereof, photodetector and preparation method thereof |
CN109439323B (en) * | 2018-09-28 | 2021-11-12 | 深圳大学 | Beta-lead protoxide quantum dot and preparation method thereof, photoelectric detector and preparation method thereof |
CN111423768A (en) * | 2020-04-15 | 2020-07-17 | 广东康烯科技有限公司 | Titanium quantum dot doped graphene-based conductive ink and preparation method and application thereof |
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