CN110371979A - A kind of method that lye etching prepares MXene quantum dot - Google Patents
A kind of method that lye etching prepares MXene quantum dot Download PDFInfo
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- CN110371979A CN110371979A CN201910703122.XA CN201910703122A CN110371979A CN 110371979 A CN110371979 A CN 110371979A CN 201910703122 A CN201910703122 A CN 201910703122A CN 110371979 A CN110371979 A CN 110371979A
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/076—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with titanium or zirconium or hafnium
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
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- C—CHEMISTRY; METALLURGY
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- C01P2004/00—Particle morphology
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Abstract
The present invention relates to a kind of lye to etch the method for preparing MXene quantum dot, belongs to field of semiconductor materials.This method comprises: it is spare to weigh MAX phase, alkali compounds and water;Alkali compounds is dissolved in water, forms alkaline solution;MAX is added to alkaline solution, is placed under room temperature, turbid solution is formed;The turbid solution that step 3 is obtained carries out centrifugation and is filtered by filter, obtains the alkaline solution of the quantum dot containing MXene;It dialyses to the alkaline solution of the quantum dot containing MXene, removes solution neutral and alkali ion and metal ion;Organic solvent and MAX are mixed into stirring, prepare MXene quantum dot.This method preparation process is simple, environmental-friendly, at low cost, and elapsed time is short and suitable large-scale production;And passing through proof has universality for MAX material.
Description
Technical field
The invention belongs to field of semiconductor materials, and in particular to a kind of method that lye etching prepares MXene quantum dot is adopted
It is prepared with aqueous slkali soak at room temperature.
Background technique
As graphene is found, ultra-thin two-dimension nano material has obtained development at full speed, especially two-dimentional transition metal
Carbide, nitride and carbonitride.Two-dimentional MXene material is because of its excellent electric conductivity, and due to connecting above lamella
Then a large amount of-OH ,-F and oxygen-containing group, therefore MXene has good hydrophily.Due to its can by electric conductivity and
Hydrophily perfectly combines, therefore is widely applied to catalysis, energy storage, photoelectricity, the fields such as biology.But it is traditional
Most of preparation method of MXene quantum dot is all by hydro-thermal reaction by presoma MXene at high temperature under high pressure by stratiform knot
The MXene of structure is cut into quantum dot.However separating the etching agent that metal phase two-dimensional material uses from MAX phase is often with acidity
Environment system etches the Al atomic layer in MAX phase using F ion as core.But the fluorine under the HF of high concentration and acidic environment
Compound environmental pollution and human body harm are larger, therefore find a kind of no F system and prepare quantum dot and seem very significant.
MXenes is referred to as transition metal carbide or carbide, their general formula is MN+1XNTX, wherein M is transition gold
Belong to, X is nitrogen or carbon, TxFor surface group (such as hydroxyl, F ion and O ion etc.).First is produced out quantum dot
MXene material is Ti3C2, quantum dot size, which can be used, passes through reaction temperature, prepare the solvent that quantum dot uses to regulate and control.
Summary of the invention
The present invention directly passes through alkaline solution and etches away the Al atomic layer in MAX phase, and the cation in aqueous slkali can be with
Intercalation replaces out Al atom, and MAX can be broken into the quantum dot of small lamella by the strong corrosive of alkaline solution.
For existing lithographic method mostly using the system containing F of use, it is affected for the performance of quantum dot, and for
The biggish defect of the harm of environment and human body, the purpose of the present invention is to provide the preparations that quantum dot is directly prepared from MAX
Method, the method preparation process is simple, environmental-friendly, at low cost, and elapsed time is short and suitable large-scale production;And pass through
Crossing proof has universality for MAX material.
According to the first aspect of the invention, a kind of method that lye etching prepares MXene quantum dot is provided, the method is logical
It crosses soda solution grouting to perform etching amphotere Al in MAX phase, and makees by the corrosivity of alkaline solution and the intercalation of cation
With directly preparing the MXene quantum dot without containing F ion from MAX phase.
Further, which comprises
Step 1: it is spare to weigh MAX phase, alkali compounds and water;
Step 2: alkali compounds being dissolved in water, forms alkaline solution;
Step 3: MAX being added to alkaline solution, is placed under room temperature, turbid solution is formed;
Step 4: the turbid solution that step 3 is obtained carries out centrifugation and is filtered by filter, obtains the quantum dot containing MXene
Alkaline solution;
Step 5: dialyse to the alkaline solution of the quantum dot containing MXene, remove solution neutral and alkali ion and metal from
Son;
Step 6: organic solvent and MAX being mixed into stirring, prepare MXene quantum dot.
Further, the alkali compounds is KOH, NaOH, LiOH or ammonium hydroxide.
Further, the step 3 at room temperature in placement process auxiliary with stirring operation.
Further, centrifugal condition is that 1000~5000rpm is centrifuged 5~20min in the step 4.
Further, filter pore size is 0.22~0.80 μm in the step 4.
Further, condition of dialysing in the step 5 is in the bag filter of 3500Da~7000Da dialysis 3~5 days.
Further, organic solvent is dimethyl sulfoxide, n,N-Dimethylformamide or ethyl alcohol, temperature in the step 6
It is 50~110 DEG C, mixing time is 0.5~2h.
Further, the MAX phase includes Ti3AlC2、Ti2AlN、Cr2AlC、Ti2AlC。
According to the second aspect of the invention, a kind of MXene quantum dot is provided, the MXene quantum dot uses more than
It is prepared by the method that the lye etching of either side prepares MXene quantum dot.
Beneficial effects of the present invention:
(1) raw material needed for MAX phase used in preparation method of the present invention prepares quantum dot is few, and can be by anti-
Temperature and the concentration of solution are answered to shorten the time required for reaching certain quantum dot concentration.The present invention is at low cost simultaneously, closes
Not high at technical requirements, reaction condition is easily controllable, environmental-friendly, is suitble to produce in enormous quantities;
(2) the MXene quantum dot of this experiment preparation is not due to using the acid condition containing F ion, without removing
MXene two-dimensional material, but directly by alkaline solution for the etching of amphotere Al in MAX phase, and it is molten by alkalinity
The corrosivity of liquid and the special adsorption of cation directly prepare the MXene quantum dot without containing F ion from MAX phase.
(3) it is prepared while being passed through by using different solvents and change reaction temperature, substantially increase the concentration of quantum dot.
Detailed description of the invention
Fig. 1 is the preparation method flow chart of MXene quantum dot according to the present invention.
Fig. 2 is the preparation flow figure for preparing aqueous slkali and preparing MXene quantum dot.
Fig. 3 is the 100nm transmission electron microscope picture of (aqueous solvent) of MXene quantum dot prepared by embodiment 1.
Fig. 4 is the 10nm transmission electron microscope picture of (aqueous solvent) of MXene quantum dot prepared by embodiment 1.
Fig. 5 is the PL map for the MXene quantum dot that embodiment 1 uses KOH to prepare as etching agent.
Fig. 6 is the PL map for the MXene quantum dot that embodiment 1 uses NaOH to prepare as etching agent.
Fig. 7 is the PL map for the MXene quantum dot that embodiment 1 uses LiOH to prepare as etching agent.
Fig. 8 is that the MXene quantum dot solution that embodiment 2 uses DMSO to prepare as organic solvent has Tyndall effect.
Specific embodiment
The invention discloses a kind of methods that middle highly basic prepares MXene quantum dot in common solvents.This method pass through by
Method, which will pass through, two-dimentional transition metal carbide or nitride (MAX) addition aqueous slkali (molar concentration >=0.001M/L) to exist on a small quantity
Centrifuging and taking supernatant liquor after placement a few hours at room temperature, and be the quantum dot solution prepared after filtering.Change can be passed through
Reaction temperature realizes the rate for adjusting the output of MXene quantum dot.Solvent can be replaced in this test and change temperature to come
Realize the preparation of high concentration MXene quantum dot.The conventional presoma MXene bis- for preparing MXene quantum dot is not used in this invention
Material is tieed up, but MXene quantum dot is directly prepared from raw material by one-step method.It is etched in experiment without using routine Al element
Agent, without harmful elements such as F, so that it is gathered around and have broad application prospects in biology and electron storage capability realm.
As shown in Figs. 1-2, the preparation method of MXene quantum dot according to the present invention, the method comprises the following steps:
Step 101. weighs 0.1g MAX phase, and 0.56g KOH measures 10ml water.
The KOH of weighing is dissolved in after 10mL water by step 102. is directly added into MAX in alkaline solution, places under room temperature
4h (or longer time) can be assisted simultaneously to stir.
After the turbid solution that step 103. obtains step 102 is centrifuged 5min with 3500rpm, the mistake for being 0.22 μm with aperture
Filter filters, and obtains MXene quantum dot.
The quantum dot prepared under step 104. aqueous solvent can dialyse 3-5 days in the bag filter of 3500Da, can remove big
The alkaline solution of amount and it is dissolved in water Al ion, that is, prepares MXene quantum dot;
Step 105. mixes stirring 1h by the way that its ionized water is changed to organic solvent DMSO at 90 DEG C with MAX, can
To prepare the MXene quantum dot of high concentration, and there is good dispersibility.
The invention will be further elaborated combined with specific embodiments below (with alkaline solution 1M/L, prepares Ti3C2For
It is bright).
Embodiment one
Weigh 0.1g Ti3AlC2, KOH is dissolved in 10mL deionized water that (alkalinity for being made into 1mol is molten by 0.56g KOH
Liquid), glass beaker is sealed with preservative film, 6h is placed at room temperature and assists with magnetic agitation, by resulting turbid 3500rpm from
After heart 5min, supernatant liquor is taken, what the filter membrane for the use of aperture being 0.22 μm filtered obtains flaxen clear solution.It obtains
The bag filter (3500Da) of solution is dialysed 3 days, is removed solution neutral and alkali ion and metal ion, is obtained Ti3C2Quantum dot.
(KOH is changed into the solution of highly basic in other, repeats the above steps to obtain identical faint yellow clear solution.)
The obtained quantum dot of preparation is tested as follows:
High-resolution-ration transmission electric-lens characterization, as can be seen that the quantum dot prepared from the high-resolution-ration transmission electric-lens figure of Fig. 3-4
Favorable dispersibility, and there is apparent lattice fringe.It is 0.263nm is Ti by measurement spacing of lattice3C2(0, -1,1,0)
Crystal face.The solution after part is dialysed is taken out from Fig. 5-7 is put into measurement PL map in quartz colorimetric utensil.
Embodiment two
Weigh 0.2g Ti3AlC2, KOH is dissolved in 10ml and goes in DMSO to be heated to 90 DEG C to make its dissolution by 0.56g KOH
(alkaline solution for being made into 1mol/L) seals glass beaker with preservative film, places 6h at room temperature and assists to stir, by gained
Turbid 3500rpm centrifugation 5min after, take supernatant liquor to obtain dark-brown clear solution.(it is organic molten to change DMSO into other
Agent repeats the available similar dark solution of above procedure.) upper layer uniform solution will be gone to be packed into glass after the solution centrifugation of preparation
In bottle, discovery Tyndall phenomenon is irradiated with laser pen, illustrates to form uniform colloidal solution, reference can be made to Fig. 8.
The present invention includes but is not limited to above embodiments, it is all carried out under the principle of spirit of that invention it is any equivalent
Replacement or local improvement, all will be regarded as within protection scope of the present invention.
Claims (10)
1. a kind of lye etches the method for preparing MXene quantum dot, which is characterized in that the method is by soda solution grouting to MAX phase
Middle amphotere Al is performed etching, and by the corrosivity of alkaline solution and the special adsorption of cation, is directly made from MAX phase
It is standby to go out not containing the MXene quantum dot of F ion.
2. the method according to claim 1, wherein the described method includes:
Step 1: it is spare to weigh MAX phase, alkali compounds and water;
Step 2: alkali compounds being dissolved in water, forms alkaline solution;
Step 3: MAX being added to alkaline solution, is placed under room temperature, turbid solution is formed;
Step 4: the turbid solution that step 3 is obtained carries out centrifugation and is filtered by filter, obtains the alkalinity of the quantum dot containing MXene
Solution;
Step 5: dialysing to the alkaline solution of the quantum dot containing MXene, remove solution neutral and alkali ion and metal ion;
Step 6: organic solvent and MAX being mixed into stirring, prepare MXene quantum dot.
3. according to the method described in claim 2, it is characterized in that, the alkali compounds is KOH, NaOH, LiOH or ammonium hydroxide.
4. according to the method described in claim 2, it is characterized in that, the step 3 assists in placement process at room temperature
With stirring operation.
5. according to the method described in claim 2, it is characterized in that, in the step 4 centrifugal condition be 1000~5000rpm from
5~20min of the heart.
6. according to the method described in claim 2, it is characterized in that, filter pore size is 0.22~0.80 μm in the step 4.
7. according to the method described in claim 2, it is characterized in that, in the step 5 dialyse condition be 3500Da~
The bag filter of 7000Da is dialysed 3~5 days.
8. according to the method described in claim 2, it is characterized in that, organic solvent is dimethyl sulfoxide, N, N- in the step 6
Dimethylformamide or ethyl alcohol, temperature are 50~110 DEG C, and mixing time is 0.5~2h.
9. the method according to claim 1, wherein the MAX phase includes Ti3AlC2、Ti2AlN、Cr2AlC、
Ti2AlC。
10. a kind of MXene quantum dot, which is characterized in that the MXene quantum dot is using according to claim 1 to any one of 9
It is prepared by the method that the lye etching prepares MXene quantum dot.
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Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111187619A (en) * | 2020-02-27 | 2020-05-22 | 北京科技大学 | MXene quantum dot fluorescence enhancement method |
CN111232981A (en) * | 2020-01-17 | 2020-06-05 | 北京理工大学 | High lithium storage capacity Ti3C2TxMechanochemical preparation method of |
CN111248224A (en) * | 2020-03-04 | 2020-06-09 | 北京科技大学 | Preparation method and antibacterial activity test method of antibacterial agent based on MXene quantum dots |
CN111944523A (en) * | 2020-08-24 | 2020-11-17 | 安徽师范大学 | MXene quantum dot with peroxide mimic enzyme property, preparation method thereof and method for detecting glutathione |
CN113248738A (en) * | 2021-06-24 | 2021-08-13 | 西南科技大学 | Two-dimensional material modified epoxy resin composite material and preparation method thereof |
CN113735124A (en) * | 2021-07-27 | 2021-12-03 | 深圳技术大学 | Preparation method and application of MXene two-dimensional material |
CN114031078A (en) * | 2021-11-19 | 2022-02-11 | 徐州纳烯新材料研究院有限公司 | Preparation method of fluorine-free MXene two-dimensional nanosheet |
CN114316971A (en) * | 2021-12-15 | 2022-04-12 | 吉林大学 | Preparation method of fluorine-free MXene quantum dots |
CN114804105A (en) * | 2022-05-13 | 2022-07-29 | 西安睿电生物科技有限公司 | Novel Ti 2 CO 2 Preparation method of two-dimensional MXene quantum dot material |
CN115282786A (en) * | 2022-01-21 | 2022-11-04 | 浙江师范大学 | MXene modified composite separation membrane and preparation method and application thereof |
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CN111232981B (en) * | 2020-01-17 | 2020-12-29 | 北京理工大学 | High lithium storage capacity Ti3C2TxMechanochemical preparation method of |
CN111187619A (en) * | 2020-02-27 | 2020-05-22 | 北京科技大学 | MXene quantum dot fluorescence enhancement method |
CN111248224B (en) * | 2020-03-04 | 2021-03-16 | 北京科技大学 | Preparation method and antibacterial activity test method of antibacterial agent based on MXene quantum dots |
CN111248224A (en) * | 2020-03-04 | 2020-06-09 | 北京科技大学 | Preparation method and antibacterial activity test method of antibacterial agent based on MXene quantum dots |
CN111944523B (en) * | 2020-08-24 | 2022-08-30 | 安徽师范大学 | MXene quantum dot with peroxide mimic enzyme property, preparation method thereof and method for detecting glutathione |
CN111944523A (en) * | 2020-08-24 | 2020-11-17 | 安徽师范大学 | MXene quantum dot with peroxide mimic enzyme property, preparation method thereof and method for detecting glutathione |
CN113248738A (en) * | 2021-06-24 | 2021-08-13 | 西南科技大学 | Two-dimensional material modified epoxy resin composite material and preparation method thereof |
CN113248738B (en) * | 2021-06-24 | 2022-07-01 | 西南科技大学 | Two-dimensional material modified epoxy resin composite material and preparation method thereof |
CN113735124A (en) * | 2021-07-27 | 2021-12-03 | 深圳技术大学 | Preparation method and application of MXene two-dimensional material |
CN114031078A (en) * | 2021-11-19 | 2022-02-11 | 徐州纳烯新材料研究院有限公司 | Preparation method of fluorine-free MXene two-dimensional nanosheet |
CN114031078B (en) * | 2021-11-19 | 2024-04-12 | 徐州纳烯新材料研究院有限公司 | Preparation method of fluorine-free MXene two-dimensional nanosheets |
CN114316971A (en) * | 2021-12-15 | 2022-04-12 | 吉林大学 | Preparation method of fluorine-free MXene quantum dots |
CN114316971B (en) * | 2021-12-15 | 2023-01-24 | 吉林大学 | Preparation method of fluorine-free MXene quantum dots |
CN115282786A (en) * | 2022-01-21 | 2022-11-04 | 浙江师范大学 | MXene modified composite separation membrane and preparation method and application thereof |
CN115282786B (en) * | 2022-01-21 | 2023-12-08 | 浙江师范大学 | MXene modified composite separation membrane and preparation method and application thereof |
CN114804105A (en) * | 2022-05-13 | 2022-07-29 | 西安睿电生物科技有限公司 | Novel Ti 2 CO 2 Preparation method of two-dimensional MXene quantum dot material |
CN114804105B (en) * | 2022-05-13 | 2023-08-08 | 补钰煜 | Novel Ti 2 CO 2 Preparation method of two-dimensional MXene quantum dot material |
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