CN106994184A - A kind of vulcanized lead tellurium composite, preparation method and its usage - Google Patents
A kind of vulcanized lead tellurium composite, preparation method and its usage Download PDFInfo
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- CN106994184A CN106994184A CN201710204866.8A CN201710204866A CN106994184A CN 106994184 A CN106994184 A CN 106994184A CN 201710204866 A CN201710204866 A CN 201710204866A CN 106994184 A CN106994184 A CN 106994184A
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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
Abstract
The present invention provides a kind of vulcanized lead tellurium composite, preparation method with and application thereof.The preparation method of vulcanized lead tellurium composite comprises the following steps：Sulfur-bearing tellurium source presoma and lead source presoma are well mixed by S1 in organic solvent, obtain presoma reaction solution；Step S1 forerunner's reaction solution is carried out two-part microwave heated constant temperature and reacted by S2, obtains vulcanized lead tellurium composite.The vulcanized lead tellurium composite of the present invention has excellent photothermal conversion performance, available for photo-thermal therapy field.
Description
Technical field
The present invention relates to a kind of vulcanized lead-tellurium composite, its preparation method with and application thereof.
Background technology
Metal sulfide receives much concern because of properties such as it is unique and enriches light, electricity, thermal and magnetics.Vulcanized lead is a kind of weight
The semiconductor of group IV-VI group is wanted, vulcanized lead has narrower energy gap (0.41ev), in lead ion sensor, light sensation performance,
Infrared probe, and area of solar cell etc. have application.
Synthesis vulcanization Al-matrixcomposites method has many kinds.For example, vulcanized lead quantum dot can pass through chemical solution method
Synthesis is obtained, and vulcanized lead/lead telluride nano material is obtained by hydro-thermal method synthesis, but synthetic method also has many defects,
Such as generated time is long, synthetic quantity very little, complex operation etc..
CN101844801A discloses a kind of monodisperse water soluble sulfide nanocrystalline cluster and preparation method thereof.This method is adopted
Solution chemical processes synthetic technology is used, lead acetate, polyacrylic acid and diglycol are mixed according to certain ratio, in nitrogen
Agitating and heating under gas shielded, rapidly injects the diglycol solution of thiocarbamide, constant reaction temperature is at 210 DEG C or so, instead
Answer 5~30 minutes, reaction product is cooled down, washed and be dried in vacuo again with water and ethanol repeatedly, monodisperse water soluble is made spherical
Sulfide nanocrystalline cluster.Resulting monodisperse pulmbous sulfide colloidal nano druse has good water solubility, and size can regulate and control
And particle has absorption in visible ray and near infrared region；Raw material is cheap and easy to get, and technique is simple, and cost is low, good process repeatability.
CN104022223A discloses a kind of core shell structure cadmium selenide/vulcanized lead nanometer corner body and preparation method thereof.It is logical
Low Temperature Thermal injection precursor solution is crossed into the second phase material of nanometer corner body surface face epitaxial growth so as to obtain core shell structure
Nanoparticles CdSe/vulcanized lead nanometer corner body.The present invention in a mild condition, can pass through the second heat injection of process control
Mode, in existing nanometer corner body surface face epitaxial growth in high quality the second phase Shell Materials, obtained core shell structure cadmium selenide/
Vulcanized lead nanometer corner body has high charge transport ability.
CN101920987A discloses a kind of chemical method for preparing lead sulfide nanoparticles.Change method by lead chloride and oil
Amine is added in the reactor with vacuum extractor, is vacuumized, and oil bath heating is stirred 0.5~2 hour to 120~180 DEG C；
Obtain uniform leucosol；Sulphur powder and oleyl amine are added in another reactor, 60~100 DEG C is heated to, obtains peony
Solution；Two solution are mixed, sampled and was rapidly injected in cold toluene centrifuge tube by 10~30 minutes, centrifugation is removed
Remove solid impurity；Supernatant in centrifuge tube is poured into beaker, then the addition ethanol precipitation vulcanized lead in beaker, then from
The heart is separated, and is removed ethanol, is obtained lead sulfide nanoparticles.The present invention obtains good dispersion, even-grained various sizes of sulphur
Change lead nano particle.Resulting materials can obtain stable near-infrared absorption spectrum.
Tellurium is a kind of important low-gap semiconductor (direct band gap 0.35eV), not only with good electrical conductance,
The physical properties such as pyroelectricity, piezoelectricity and also there is preferable application in optics aspect.
CN103451599A discloses a kind of cadmium telluride/bismuth telluride one for cooperateing with the photo-thermal sent a telegraph collaboration to send a telegraph with photo-thermal
Body nano structural material and its preparation method.Its step is one layer of cadmium telluride nanometer rods of deposition on the conducting surface of conducting glass substrate
Layer, has the bismuth telluride layer that tellurium adulterates in cadmium telluride nanometer rods layer surface redeposition, constitutes the integrated nano junction of cadmium telluride/bismuth telluride
Structure material.Light and heat in solar spectrum can be converted into electric energy by the material simultaneously, realize photo-thermal collaboration using photo-thermal collaboration
The integrated nano structural material of the cadmium telluride sent a telegraph/bismuth telluride.
CN105963712A discloses a kind of nano combined drug particles of thermochemotherapy telluride copper and its construction method.Its side
Method be nano combined drug particles be the telluride copper nano particles wrapped up using oleic acid as kernel, be enclosed with one layer in kernel outer surface
Hydrophobic drug；The surface of nano combined drug particles is modified with amphipathic molecule.Send the telluride copper of bright oleic acid parcel elsewhere
Nano particle acts not only as the material of tumor thermal therapy, is effectively killed under relatively low laser intensity and relatively low concentration
Dead cancer cell；And the carrier of medicine is also used as, it is achieved thereby that the synergistic treatment of thermochemotherapy, can effectively improve tumour
Therapeutic efficiency；Therefore, telluride copper nano particles have broad application prospects in terms of medicine transmission, oncotherapy.
CN104176704A discloses a kind of mushroom cadmium sulfide-tellurium composite and its production and use.Method
It is as follows：By tellurium source presoma and the dissolving of cadmium source presoma in organic solvent, organosulfur compound and alkalescent are then added
Compound, under high pressure confined reaction；After reaction terminates, pressure release naturally cools to room temperature to normal pressure, centrifuges, consolidate
Body, the solid is washed with water, absolute ethyl alcohol successively, vacuum drying, obtains the mushroom cadmium sulfide-tellurium composite.Institute
Stating cadmium sulfide-tellurium composite has good non-uniform topographical, form controllable, and with excellent hydrogen manufacturing performance and effect, can
For photolysis water hydrogen field.
The composite of microcosmic nanostructured not only has the characteristic of original material in itself due to it, can more play different materials
Cooperative effect between material, the unique physical and chemical property not possessed with homogenous material, thus with it is very wide should
Use prospect.Based on this, design a kind of simple and environmentally-friendly method prepare the composite of vulcanized lead-tellurium have it is particularly significant
Meaning.
The content of the invention
In order to solve to vulcanize in the prior art many defects that Al-matrixcomposites exist in synthesis, of the invention is main
Purpose be to provide a kind of vulcanized lead-tellurium composite with and preparation method thereof, can quickly and easily be obtained by this method
Vulcanized lead-tellurium composite.
To achieve the above objectives, the present invention provides a kind of preparation method of vulcanized lead-tellurium composite, including following step
Suddenly：
S1：Sulfur-bearing tellurium source presoma and lead source presoma are well mixed in organic solvent, presoma reaction solution is obtained；
S2：Step S1 forerunner's reaction solution is subjected to the reaction of two-part microwave heated constant temperature, the vulcanized lead-tellurium is obtained multiple
Condensation material.
The vulcanized lead prepared by this method-tellurium composite is found to have certain photothermal conversion ability, can
For photo-thermal therapy.
Preferably, in step sl, the sulfur-bearing tellurium source presoma is tellurium diethyl dithiocarbamate, the lead source
Any one or any a variety of mixing of the presoma in lead dimethyl dithiocarbamate, lead acetate, lead dimethide
The mol ratio of thing, the sulfur-bearing tellurium source presoma and lead source presoma is 2:(1~3).
Most preferably, lead source presoma be lead dimethyl dithiocarbamate, the sulfur-bearing tellurium source presoma with
The mol ratio of lead source presoma is 1:1, the vulcanized lead now obtained-tellurium composite be that appearance structure is regular and form compared with
Good dumbbell shape.
Preferably, in step sl, the organic solvent is C1-6Alcohol, C2-6Glycol, N,N-dimethylformamide (DMF),
Any one in dimethyl sulfoxide (DMSO) (DMSO) or 1-METHYLPYRROLIDONE (NMP).It is highly preferred that the organic solvent is C2-6
Glycol.
Most preferably, the organic solvent is ethylene glycol, and the appearance structure of the vulcanized lead now obtained-tellurium composite is advised
It is whole, the dumbbell shape structure of rule is presented.
Preferably, step S2 is specially：
S2-1：In the case where power is 100~400W ultrasonic agitation, forerunner's reaction solution that step S1 is obtained is heated by room temperature
To 120 DEG C, the time is 4~6min, obtains the first reaction solution；
S2-2：By first reaction solution in power under 100~400W ultrasonic agitation, to continue to be heated to 170~190 DEG C,
Time is 4~6min, and in keeping 2~4min at this temperature, obtains the second reaction solution；
S2-3：Second reaction solution is cooled to room temperature, by gained washing of precipitate, drying after centrifugation, the sulphur is produced
Change lead-tellurium composite.
Preferably, in step S2-1, ultrasonic agitation power is 200W；In step S2-2, by first reaction solution in work(
Rate for 200W ultrasonic agitation under, continue to be heated to 180 DEG C.
Experiment finds that, when ultrasonic agitation power is that 200W, S2-2 step are heated to 180 DEG C, obtained vulcanized lead-tellurium is multiple
The regular appearance of condensation material is preferable.
The present invention also provides a kind of vulcanized lead-tellurium composite, and its microscopic appearance is dumbbell shape, and its length is 1.5~2.0
μm, a width of 250~320nm of intermediate bar, a length of 300~400nm of rib of two dumbbell structure.
The present invention also provides a kind of purposes of vulcanized lead-tellurium composite, i.e., vulcanized lead-tellurium composite is used for into photo-thermal
In treatment.Because the vulcanized lead-tellurium composite has excellent photothermal deformation performance, so as to applied to photo-thermal therapy
Field.
Brief description of the drawings
Fig. 1 is the low power scanning electron microscope (SEM) photograph of vulcanized lead-tellurium composite of embodiment 1.
Fig. 2 a are the transmission electron microscope pictures of vulcanized lead-tellurium composite of embodiment 1, and Fig. 2 b and 2c are the vulcanizations of embodiment 1
The high resolution TEM figure of lead-tellurium composite.
Fig. 3 is the power spectrum test chart of vulcanized lead-tellurium composite of embodiment 1.
Fig. 4 is the X-ray diffractogram of vulcanized lead-tellurium composite of embodiment 1.
Fig. 5 a, 5b, 5c are the ESEM of vulcanized lead-tellurium composite of embodiment 1, embodiment 2 and embodiment 3 respectively
Figure.
Fig. 6 be the embodiment 1 of various concentrations vulcanized lead-tellurium composite aqueous solution 980nm laser irradiation under temperature
Change and the graph of a relation of time.
Fig. 7 is that vulcanized lead-tellurium composite aqueous solution of the embodiment 1, embodiment 2 and embodiment 3 of same concentrations exists
The lower temperature change of 980nm laser irradiation and the graph of a relation of time.
Embodiment
Below by specific embodiment, the present invention is described in detail, but the purposes of these exemplary embodiments and
Purpose only be used for enumerate the present invention, not to the present invention real protection scope constitute it is any type of it is any limit, it is more non-will
Protection scope of the present invention is confined to this.
Embodiment 1
Vulcanized lead-tellurium composite is prepared by following steps：
S1：Into appropriate organic solvent ethylene glycol, it is 1 to add mol ratio:1 tellurium diethyl dithiocarbamate
(TDEC) and lead dimethyl dithiocarbamate, it is sufficiently stirred for ultrasonic wave, is well mixed, obtains forerunner's reaction solution；
S2：Forerunner's reaction solution is subjected to the reaction of two-part microwave heated constant temperature, so as to obtain vulcanized lead-tellurium composite wood
Material, be specially：
S2-1：Under ultrasonic agitation power 200W, forerunner's reaction solution that step S1 is obtained is passed through into microwave reaction instrument
120 DEG C are heated to by room temperature, the time is 5min, obtains the first reaction solution；
S2-2：By first reaction solution under ultrasonic agitation power 200W, continue to be heated to 180 DEG C, this process needs
3min, and kept for 2 minutes at such a temperature, obtain the second reaction solution；
S2-3：Second reaction solution is naturally cooled into room temperature, and centrifuged 4 minutes with 10000rpm centrifugal speed,
Gained precipitation is successively respectively washed 2-3 times with absolute ethyl alcohol and deionized water, is then dried in vacuo, vulcanized lead-tellurium is produced and is combined
Material.
Embodiment 2
The preparation of vulcanized lead-tellurium composite is that in step sl embodiment 2 is added with reference to embodiment 1, difference
Mol ratio is 2:1 tellurium diethyl dithiocarbamate (TDEC) and lead dimethyl dithiocarbamate.
Embodiment 3
The preparation of vulcanized lead-tellurium composite is that in step sl embodiment 3 is added with reference to embodiment 1, difference
Mol ratio is 2:3 tellurium diethyl dithiocarbamate (TDEC) and lead dimethyl dithiocarbamate.
Embodiment 4
The preparation of vulcanized lead-tellurium composite is with reference to embodiment 1, and difference is in step S2-1 and S2-2 ultrasonic
The power of stirring is 100W.
Embodiment 5
The preparation of vulcanized lead-tellurium composite is in step S2-1 and S2-2 with reference to embodiment 1, difference, surpasses
The power of sound stirring is 300W.
Embodiment 6
The preparation of vulcanized lead-tellurium composite is in step S2-1 and S2-2 with reference to embodiment 1, difference, surpasses
The power of sound stirring is 400W.
Embodiment 7
The preparation of vulcanized lead-tellurium composite is in step S2-2 with reference to embodiment 1, difference, by described the
One reaction solution continues to be heated to 140 DEG C.
Embodiment 8
The preparation of vulcanized lead-tellurium composite is in step S2-2 with reference to embodiment 1, difference, by described the
One reaction solution continues to be heated to 150 DEG C.
Embodiment 9
The preparation of vulcanized lead-tellurium composite is in step S2-2 with reference to embodiment 1, difference, by described the
One reaction solution continues to be heated to 160 DEG C.
Embodiment 10
The preparation of vulcanized lead-tellurium composite is in step S2-2 with reference to embodiment 1, difference, by described the
One reaction solution continues to be heated to 170 DEG C.
Embodiment 11
The preparation of vulcanized lead-tellurium composite is in step S2-2 with reference to embodiment 1, difference, by described the
One reaction solution continues to be heated to 190 DEG C.
Embodiment 12-18
The preparation of vulcanized lead-tellurium composite is with reference to embodiment 1, and difference is in step sl, by organic solvent
Replace with 1,3- propane diols (embodiment 12), 1,4- butanediols (embodiment 13), ethanol (embodiment 14), just respectively by ethylene glycol
Butanol (embodiment 15), DMF (embodiment 16), DMSO (embodiment 17) and NMP (embodiment 18).
The vulcanized lead obtained to embodiment 1-tellurium composite carries out microscopic sdIBM-2+2q.p.approach, as a result as follows：
1st, from Fig. 1 low power scanning electron microscope (SEM) photograph (SEM), the vulcanized lead-tellurium composite pattern is homogeneous, structure is new
Grain husk, is dumbbell shape structure, and the external diameter of these dumbbell shape structures is highly identical, and length is 1.5~2.0 μm, intermediate bar a width of 250~
320nm, two a length of 300~400nm of dumbbell structure rib.
2nd, there is dumbbell shape structure from Fig. 2 a transmission electron microscope picture (TEM), figure, from high resolution transmission electron microscopy
It can be seen that gem-pure lattice fringe, is primarily present a variety of lattice fringes of 0.209nm, 0.223nm two in (Fig. 2 b and 2c)
Width, PbS (220) and Te (110) crystal face are correspond to respectively.
3rd, the test result from Fig. 3 power spectrums (EDX) is found out：Contain tri- kinds of elements of Pb, S, Te in sample, illustrate the mute of preparation
Bell type shape composite contains tri- kinds of elements of Pb, S, Te (wherein Cu elements come from the Cu nets specimen holder needed for test sample).
4th, from Fig. 4 X-ray diffractogram (XRD), it is main it is corresponding be PbS and Te diffraction maximum, by comparing this
A little diffraction maximums, it is known that the present invention successfully synthesizes PbS-Te composites.
The vulcanized lead obtained to embodiment 1-tellurium composite carries out the test of photothermal conversion performance, and method of testing is：Will
Vulcanized lead-tellurium composite is distributed in high purity water is configured to 0 μ g/mL, 5 μ g/mL, 10 μ g/mL, 25 μ g/mL, 50 μ g/ respectively
ML, 100 μ g/mL solution, the solution prepared absorption 1mL is added in quartz colorimetric utensil, irradiated with 980nm laser
10min records temperature change.Fig. 6 shows the pass of solution temperature change and the time under the irradiation of 980nm laser of various concentrations
System's figure, under 50 μ g/mL mass concentration, laser irradiation 10min, its temperature rise is higher than pure water about 9.5 DEG C, shows that it has
Excellent light thermal property.
According to Fig. 5 a, 5b, 5c, the form of comparative example 1, embodiment 2 and the product of embodiment 3, it can be deduced that, it is used as original
The sulphur tellurium source presoma of material has conclusive influence with the mol ratio of lead source presoma on the form of final product, when both
Mol ratio is 1:When 1, the best dumbbell shape structure of form can be obtained.The vulcanized lead obtained to embodiment 1,2,3-tellurium composite wood
Material carries out photothermal conversion performance test, and now method is the same, and solution concentration is 100 μ g/mL.From figure 7 it can be seen that embodiment 1
Product photothermal conversion ability it is best, it is seen that the appearance structure of vulcanized lead-tellurium composite closer to regular dumbbell shape, its
Photothermal conversion ability is better.
SEM sign discoveries are carried out to the product of embodiment 4, embodiment 5 and embodiment 6, although obtained vulcanized lead-tellurium is multiple
The form of condensation material is similar dumbbell shape, but pattern systematicness is poor.It can be seen that ultrasonic agitation power influences the rule of composite
Then property, when ultrasonic agitation power is 200W, can obtain the preferable vulcanized lead of pattern systematicness-tellurium composite.
SEM sign discoveries are carried out to the product of 7~embodiment of embodiment 11, embodiment 7, embodiment 8 and embodiment 9 fail
The dumbbell shape structure of formation rule, and there is bulk presoma assembly, the pattern of embodiment 10 and embodiment 11 is presented substantially
Dumbbell shaped, but pattern systematicness is poor.It can be seen that second segment microwave heating outlet temperature have to the regularity of composite compared with
Big influence, when second segment microwave heat outlet temperature be 180 DEG C when, can obtain the preferable vulcanized lead of pattern systematicness-
Tellurium composite.
SEM sign discoveries are carried out to the product of 12~embodiment of embodiment 18, the composite pattern of gained is not presented
The dumbbell shape structure of rule, it is seen that organic solvent also has large effect to the pattern of composite.
Claims (10)
1. the preparation method of a kind of vulcanized lead-tellurium composite, it is characterised in that comprise the following steps：
S1：Sulfur-bearing tellurium source presoma and lead source presoma are well mixed in organic solvent, presoma reaction solution is obtained；
S2：Step S1 forerunner's reaction solution is subjected to the reaction of two-part microwave heated constant temperature, the vulcanized lead-tellurium is obtained multiple
Condensation material.
2. preparation method according to claim 1, it is characterised in that in step sl, the sulfur-bearing tellurium source presoma is
Tellurium diethyl dithiocarbamate, lead source presoma is selected from lead dimethyl dithiocarbamate, lead acetate, dimethyl
Any one in lead or any a variety of mixture, the mol ratio of the sulfur-bearing tellurium source presoma and lead source presoma is
2:(1~3).
3. preparation method according to claim 2, it is characterised in that lead source presoma is DMDS for amino
The mol ratio of lead formate, the sulfur-bearing tellurium source presoma and lead source presoma is 1:1.
4. according to any described preparation methods of claim 1-3, it is characterised in that in step sl, the organic solvent is
C1-6Alcohol, C2-6In glycol, N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO) (DMSO) or 1-METHYLPYRROLIDONE (NMP)
Any one.
5. preparation method according to claim 4, it is characterised in that the organic solvent is ethylene glycol.
6. according to any described preparation methods of claim 1-5, it is characterised in that step S2 is specially：
S2-1：In the case where power is 100~400W ultrasonic agitation, forerunner's reaction solution that step S1 is obtained is heated by room temperature
To 120 DEG C, the time is 4~6min, obtains the first reaction solution；
S2-2：By first reaction solution in power under 100~400W ultrasonic agitation, to continue to be heated to 170~190 DEG C,
Time is 4~6min, and in keeping 2~4min at this temperature, obtains the second reaction solution；
S2-3：Second reaction solution is cooled to room temperature, by gained washing of precipitate, drying after centrifugation, the sulphur is produced
Change lead-tellurium composite.
7. preparation method according to claim 6, it is characterised in that in step S2-1, ultrasonic agitation power is 200W；Step
In rapid S2-2, by first reaction solution in the case where power is 200W ultrasonic agitation, continue to be heated to 180 DEG C.
8. a kind of pass through vulcanized lead-tellurium composite made from any described preparation methods of claim 1-7.
9. a kind of vulcanized lead-tellurium composite, it is characterised in that its microscopic appearance is dumbbell shape structure, the length of the structure is
1.5~2.0 μm, a width of 250~320nm of intermediate bar, a length of 300~400nm of rib of two dumbbell structure.
10. vulcanized lead-tellurium composite described in claim 8 or 9 is in the application in photo-thermal therapy field.
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| CN109399581A (en) * | 2018-10-29 | 2019-03-01 | 温州大学新材料与产业技术研究院 | A kind of cuprous sulfide-tellurium nano material and preparation method thereof |
| CN109453374A (en) * | 2018-10-24 | 2019-03-12 | 温州大学 | A kind of tellurium-cuprous sulfide heterojunction composite and its preparation method and application |
| CN109467061A (en) * | 2018-10-23 | 2019-03-15 | 温州大学新材料与产业技术研究院 | A kind of PbS-Te nano particle of carried noble metal and preparation method thereof |
| CN112763419A (en) * | 2021-01-27 | 2021-05-07 | 福州大学 | Hydrogen sulfide photo-thermal detection method of perovskite nano composite material modified based on SBE-beta-CD |
| WO2023082215A1 (en) * | 2021-11-13 | 2023-05-19 | 广东暨创硒源纳米研究院有限公司 | Radiotherapy sensitizer having selenium-tellurium dumbbell heterostructure, preparation method therefor and use thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109467061A (en) * | 2018-10-23 | 2019-03-15 | 温州大学新材料与产业技术研究院 | A kind of PbS-Te nano particle of carried noble metal and preparation method thereof |
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| CN109399581A (en) * | 2018-10-29 | 2019-03-01 | 温州大学新材料与产业技术研究院 | A kind of cuprous sulfide-tellurium nano material and preparation method thereof |
| CN109399581B (en) * | 2018-10-29 | 2021-10-15 | 温州大学新材料与产业技术研究院 | Cuprous sulfide-tellurium nano material and preparation method thereof |
| CN112763419A (en) * | 2021-01-27 | 2021-05-07 | 福州大学 | Hydrogen sulfide photo-thermal detection method of perovskite nano composite material modified based on SBE-beta-CD |
| WO2023082215A1 (en) * | 2021-11-13 | 2023-05-19 | 广东暨创硒源纳米研究院有限公司 | Radiotherapy sensitizer having selenium-tellurium dumbbell heterostructure, preparation method therefor and use thereof |
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