CN108864206A - A kind of ultra-thin two-dimension spin crossover nano material and its preparation method and application - Google Patents
A kind of ultra-thin two-dimension spin crossover nano material and its preparation method and application Download PDFInfo
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000001294 propane Substances 0.000 claims abstract description 22
- 125000000339 4-pyridyl group Chemical group N1=C([H])C([H])=C([*])C([H])=C1[H] 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 20
- 238000002604 ultrasonography Methods 0.000 claims abstract description 7
- 238000005442 molecular electronic Methods 0.000 claims abstract description 6
- 239000006185 dispersion Substances 0.000 claims abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 230000001476 alcoholic effect Effects 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- 235000019441 ethanol Nutrition 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 9
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 230000001376 precipitating effect Effects 0.000 claims description 6
- 229910001914 chlorine tetroxide Inorganic materials 0.000 claims description 4
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Chemical compound [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000002071 nanotube Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 125000003349 3-pyridyl group Chemical group N1=C([H])C([*])=C([H])C([H])=C1[H] 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 125000001824 selenocyanato group Chemical group *[Se]C#N 0.000 description 5
- 239000003446 ligand Substances 0.000 description 4
- DTMHTVJOHYTUHE-UHFFFAOYSA-N thiocyanogen Chemical compound N#CSSC#N DTMHTVJOHYTUHE-UHFFFAOYSA-N 0.000 description 4
- 230000002349 favourable effect Effects 0.000 description 3
- 230000005291 magnetic effect Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000003125 aqueous solvent Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
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- 229910021389 graphene Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000012621 metal-organic framework Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
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- 238000001556 precipitation Methods 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- SSGHNQPVSRJHEO-UHFFFAOYSA-N selenocyanogen Chemical compound N#C[Se][Se]C#N SSGHNQPVSRJHEO-UHFFFAOYSA-N 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- KAESVJOAVNADME-UHFFFAOYSA-N 1H-pyrrole Natural products C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
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- 238000006555 catalytic reaction Methods 0.000 description 1
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- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
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- 238000005404 magnetometry Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 description 1
- KYEKHFSRAXRJBR-UHFFFAOYSA-M potassium;selenocyanate Chemical compound [K+].[Se-]C#N KYEKHFSRAXRJBR-UHFFFAOYSA-M 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000011896 sensitive detection Methods 0.000 description 1
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- 239000004094 surface-active agent Substances 0.000 description 1
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- 229910001428 transition metal ion Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F15/00—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic Table
- C07F15/02—Iron compounds
- C07F15/025—Iron compounds without a metal-carbon linkage
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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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Abstract
The invention discloses a kind of preparation methods of ultra-thin two-dimension spin crossover nano material, carry out ultrasound removing in a solvent by the dispersion of three-dimensional Van der Waals complex and obtain, and the structural formula of the three-dimensional Van der Waals complex is Fe (XCN)2(1,3- bis- (4- pyridyl group) propane)2, X is selected from S or Se；Also disclose the ultra-thin two-dimension spin crossover nano material and its application in the molecular electronic device that preparation is shown for information storage, molecular switch or molecule that above-mentioned preparation method is prepared.Ultra-thin two-dimension spin crossover nano material thickness of the present invention realizes the spin crossover behavior of multistep in 1-10nm or so, this ultra-thin two-dimensional structure.There is huge application prospect in terms of the molecular electronic devices such as the ultra-thin two-dimension spin crossover nano material preparation is simple, and well dispersed, performance is stablized, and stores in information, molecular switch, and molecule is shown.
Description
Technical field
The present invention relates to spin crossover materials and its preparation method and application, and in particular to a kind of ultra-thin two-dimension spin crossover
Nano material and its preparation method and application.
Background technique
Spin crossover material is one of most noticeable bistable material, it refers under the conditions of specific environmental stimuli
It is mutual between the transition metal ions high-spin that (such as temperature, pressure, light radiation, guest molecule) occurs and low spin states
Conversion.This conversion can be along with performance changes such as a series of magnetics, electronics, optics, calorifics.This excellent characteristic makes
The fields such as spin crossover material novel information memory device on a molecular scale, molecular switch, display device, sensitive detection parts tool
There is tempting application prospect (J.Am.Chem.Soc.2018,140,98-101).In order to achieve the purpose that practical application, spin is handed over
Pitching material nano is necessary approach.Wherein the factors such as nanosizing mode, nano-grade size have to pass the performance of material
Important influence.
Ultra-thin two-dimension nano material imparts its unique physics, electricity due to atomic-level thickness and two-dimensional layered structure
Son, chemistry and optical property and wide application prospect.With traditional two-dimension nano materials (graphene, graphene oxide,
Metal oxide, boron nitride etc.) it compares, ultra-thin two-dimension metal-organic framework material has adjustable structure and function (by changing
Become metal and matched type), big surface area, the hole of high-sequential and sufficiently exposed surface-active site, catalysis,
Electrochemistry, detection, gas separation, environmental monitoring etc. show huge application potential.By ultra-thin two-dimension nano material skill
Art is applied to the preparation of metal organic frame nano material, is a kind of solution of very advantageous.And it studies and leads in spin crossover
Domain, there is not been reported for the research that spin crossover metal-organic framework material and ultra-thin two-dimension nano material are combined.
Summary of the invention
Goal of the invention：In order to solve the practical application of existing spin crossover material, first aspect present invention provides one kind
Ultra-thin two-dimension spin crossover nano material, second aspect provide the preparation method of ultra-thin two-dimension spin crossover nano material, the
Three aspects provide ultra-thin two-dimension spin crossover applications to nanostructures.
Technical solution：A kind of preparation method of ultra-thin two-dimension spin crossover nano material described in first aspect present invention,
It carries out ultrasound removing in a solvent by the dispersion of three-dimensional Van der Waals complex to obtain, the structural formula of the three-dimensional Van der Waals complex is
Fe(XCN)2(1,3- bis- (4- pyridyl group) propane)2, X is selected from S or Se.
The preparation step of the three-dimensional Van der Waals complex is as follows：
(1) under nitrogen atmosphere, by Fe (ClO4)2·6H2O and KXCN are dissolved in alcoholic solvent, stir 15-60min, Gu
Liquid separation removal precipitating, obtains Fe (XCN)2Alcoholic solution；Wherein, X is selected from S or Se；It is preferred that Fe (ClO4)2·6H2O and KXCN are pressed
Molar ratio 1:2 additions；
(2) under nitrogen atmosphere, the Fe (XCN) step (1) obtained2Alcoholic solution and 1,3- bis- (4- pyridyl group) propane alcohol
Solid is precipitated in solution mixing, and suspension stirs 0.5-1h at 50-100rpm, and filtering, cleaning precipitating are to get three-dimensional Van der Waals
Complex Fe (XCN)2(1,3- bis- (4- pyridyl group) propane)2.It is preferred that Fe (XCN)2With mole of 1,3- bis- (4- pyridyl group) propane
Than being 1:2.
In step (1), the alcoholic solvent is methanol or ethyl alcohol, preferably Fe (ClO4)2·6H2The ratio of O and the alcoholic solvent
For 0.5mmol:30-35mL；In step (2), the ligand 1, the solvent in 3- bis- (4- pyridyl group) propane alcoholic solution is methanol
Or ethyl alcohol, the preferably ratio of ligand and alcoholic solvent is 1mmol:20-25mL.
Specifically, the preparation method of ultra-thin two-dimension spin crossover nano material, includes the following steps：
S1, it disperses three-dimensional Van der Waals complex in solvent, the ultrasound 30- under the conditions of 30-60 DEG C, 20-60kHz
90min；
S2, the solution that step S1 is obtained is stirred into 12-24h at 100-500rpm, is then allowed to stand 12-24h, 100-
1000rpm is centrifuged off precipitating, obtains the dindar solution of favorable dispersibility；
S3, the dindar solution that step S2 is obtained is spin-dried for, obtains ultra-thin two-dimension spin crossover nano material.
In step S1, the solvent is water or alcoholic solvent, and preferably alcoholic solvent is methanol, ethyl alcohol or propyl alcohol.The three-dimensional model
The ratio of moral China complex and solvent is 5-20mg:30-100mL.
In step S3, the temperature that is spin-dried for is 30-80 DEG C.
Second aspect of the present invention provides the ultra-thin two-dimension spin crossover nano material that above-mentioned preparation method is prepared；It is thick
Degree is 1-10nm, preferably 2-5nm；Lateral dimension is 0.5-2 μm, preferably 0.5-1 μm.
Third aspect present invention provides the ultra-thin two-dimension spin crossover nano material in preparation for information storage, molecule
The application in molecular electronic device that switch or molecule are shown.
Beneficial effect：Ultra-thin two-dimension spin crossover nano material prepared by the present invention has the following advantages that：It (1) is a kind of pure
Pure nano material is free of any surfactant；(2) ultra-thin two-dimension spin crossover nano material is equal in solution and solid state
It is stabilized, well dispersed, performance is stablized；(3) ultra-thin two-dimension spin crossover nano material can realize the spin crossover row of multistep
For；(4) preparation method simple and flexible, the two-dimension nano materials of available 1-10nm different-thickness, this ultra-thin two dimension
Structure realizes the spin crossover behavior of multistep；(5) ultra-thin two-dimension spin crossover nano material can be applicable to stores for information,
Molecular switch, molecule are shown etc. in molecular electronic devices.
Detailed description of the invention
Fig. 1 is three-dimensional Van der Waals complex Fe (XCN)2(1,3- bis- (4- pyridyl group) propane)2Crystal structure；
Fig. 2 is ultra-thin two-dimension spin crossover nano material transmission electron microscope pattern prepared by the present invention；
Fig. 3 is the susceptibility curve of ultra-thin two-dimension spin crossover nano material prepared by the present invention.
Specific embodiment
1 Fe of embodiment (SCN)2Alcoholic solution preparation
Fe (the ClO of 0.5mmol4)2·6H2The KSCN of O and 1.0mmol is dissolved in 30mL methanol in nitrogen atmosphere, is stirred
20min is mixed, the white precipitate KClO of generation is filtered to remove4, obtained filtrate is Fe (SCN)2Methanol solution.
2 Fe of embodiment (SeCN)2Alcoholic solution preparation
Fe (the ClO of 0.5mmol4)2·6H2The KSeCN of O and 1.0mmol is dissolved in 35mL ethyl alcohol in nitrogen atmosphere,
30min is stirred, the white precipitate KClO of generation is filtered to remove4, obtained filtrate is Fe (SeCN)2Ethanol solution.
3 three-dimensional Van der Waals complex Fe (SCN) of embodiment2(1,3- bis- (4- pyridyl group) propane)2Synthesis
The Fe (SCN) that embodiment 1 obtains2Methanol solution, is added to 20mL dissolved with 1.0mmol ligand 1 in nitrogen atmosphere,
In the methanol solution of 3- bis- (4- pyridyl group) propane, solution is immediately turned into glassy yellow, and along with the precipitation of bright yellow solid.Shape
At suspension solution stirring 0.5-1h after filter, obtain bright yellow solid, 10mL methanol washs obtained solid to get arriving pure three
It ties up Van der Waals complex Fe (SCN)2(1,3- bis- (4- pyridyl group) propane)2, crystal structure is shown in Fig. 1.
4 three-dimensional Van der Waals complex Fe (SeCN) of embodiment2(1,3- bis- (4- pyridyl group) propane)2Synthesis
The Fe (SeCN) that embodiment 2 obtains2Ethanol solution is added to 25mL dissolved with 1.0mmol ligand in nitrogen atmosphere
In the ethanol solution of 1,3- bis- (4- pyridyl group) propane, solution is immediately turned into dark yellow, and along with the precipitation of dark yellow solid.
It is filtered after the suspension solution stirring 0.5-1h of formation, obtains dark yellow solid, 15mL ethanol washing obtained solid is pure to get arriving
Three-dimensional Van der Waals complex Fe (SeCN)2(1,3- bis- (4- pyridyl group) propane)2。
The preparation of 5 ultra-thin two-dimension spin crossover nano material of embodiment
The three-dimensional Van der Waals complex Fe (SCN) prepared with embodiment 32(1,3- bis- (4- pyridyl group) propane)2For material,
Ultra-thin two-dimension spin crossover nano material is prepared, specific step is as follows：
S1, by 10mg three-dimensional Van der Waals complex Fe (SCN)2(1,3- bis- (4- pyridyl group) propane)2, in 100mL beaker
It is scattered in 50mL aqueous solvent, at 40 DEG C, ultrasound 60min under the conditions of 50kHz；
The solution that S2, step S1 are obtained stirs for 24 hours at 500 rpm, is then allowed to stand 12h, and 1000rpm is centrifuged off sedimentation
Object obtains the dindar solution of favorable dispersibility；
S3, above-mentioned dindar solution is spin-dried at 40-60 DEG C, obtains light green color ultra-thin two-dimension spin crossover nano material；
With a thickness of 2nm, lateral dimension is 0.5 μm.
The preparation of 6 ultra-thin two-dimension spin crossover nano material of embodiment
The three-dimensional Van der Waals complex Fe (SeCN) prepared with embodiment 42(1,3- bis- (4- pyridyl group) propane)2For material,
Ultra-thin two-dimension spin crossover nano material is prepared, specific step is as follows：
S1, by 8mg three-dimensional Van der Waals complex Fe (SeCN)2(1,3- bis- (4- pyridyl group) propane)2, in 100mL beaker
It is scattered in 60mL aqueous solvent, at 30 DEG C, ultrasound 90min under the conditions of 40kHz；
The solution that S2, step S1 are obtained stirs for 24 hours at 300 rpm, is then allowed to stand 12h, and 1000rpm is centrifuged off sedimentation
Object obtains the dindar solution of favorable dispersibility；
S3, above-mentioned dindar solution is spin-dried at 40-60 DEG C, obtains light green color ultra-thin two-dimension spin crossover nano material；
With a thickness of 5nm, lateral dimension is 1 μm.
Embodiment 7
Preparation method is with embodiment 5, the difference is that by 5mg three-dimensional Van der Waals complex Fe (SCN)2((the 4- pyridine of 1,3- bis-
Base) propane)2, it is scattered in 100mL beaker in 30mL methanol solvate.
Embodiment 8
Preparation method is with embodiment 5, the difference is that by 20mg three-dimensional Van der Waals complex Fe (SCN)2((the 4- pyrrole of 1,3- bis-
Piperidinyl) propane)2, it is scattered in 200mL beaker in 100mL alcohol solvent.
9 ultra-thin two-dimension spin crossover appearance of nano material of embodiment characterization
The pattern of ultra-thin two-dimension spin crossover nano material prepared by embodiment 5 is characterized by transmission electron microscope, Fig. 2
Show that TEM image of the ultra-thin two-dimension nano material under 0.5 μm of scale, image clearly show the regular ultrathin membrane of bulk.
The test of 10 variable temperature magnetic susceptibility of embodiment
The light green color ultra-thin two-dimension spin crossover nano material for taking 10mg embodiment 5 to be spin-dried for is strong in the magnetic field 2000Oe
It spends, has carried out magnetic susceptibility measurement, rate of temperature fall 2K/min within the temperature range of 320-5K.Susceptibility curve (the χ of samplemTvs
T) as shown in figure 3, multistep spin crossover behavior has occurred in all nanotube samples.These results indicate that obtained by the method for the present invention
Ultra-thin two-dimension spin crossover nano material can be applicable to and stored for information, molecular switch, molecule such as shows at the molecular electronics device
In part.
Claims (10)
1. a kind of preparation method of ultra-thin two-dimension spin crossover nano material, which is characterized in that it is by three-dimensional Van der Waals complex
Dispersion carries out ultrasound removing in a solvent and obtains, and the structural formula of the three-dimensional Van der Waals complex is Fe (XCN)2(bis- (4- of 1,3-
Pyridyl group) propane)2, X is selected from S or Se.
2. preparation method according to claim 1, which is characterized in that the preparation step of the three-dimensional Van der Waals complex is such as
Under：
(1) under nitrogen atmosphere, by Fe (ClO4)2·6H2O and KXCN are dissolved in alcoholic solvent, stir 15-60min, solid-liquid point
It leaves away except precipitating, obtains Fe (XCN)2Alcoholic solution；Wherein, X is selected from S or Se；
(2) under nitrogen atmosphere, the Fe (XCN) step (1) obtained2Alcoholic solution and 1,3- bis- (4- pyridyl group) propane alcoholic solution
Solid is precipitated in mixing, and suspension stirs 0.5-1h, and filtering, cleaning precipitating are to get three-dimensional Van der Waals complex Fe (XCN)2(1,
3- bis- (4- pyridyl group) propane)2。
3. preparation method according to claim 2, which is characterized in that alcoholic solvent described in step (1) be methanol or ethyl alcohol,
Solvent in 1,3- bis- described in step (2) (4- pyridyl group) propane alcoholic solution is methanol or ethyl alcohol.
4. preparation method according to claim 1, which is characterized in that include the following steps：
S1, it disperses three-dimensional Van der Waals complex in solvent, the ultrasound 30-90min under the conditions of 30-60 DEG C, 20-60kHz；
S2, the solution that step S1 is obtained is stirred into 12-24h at 100-500rpm, is then allowed to stand 12-24h, 100-1000rpm
It is centrifuged off precipitating, obtains dindar solution；
S3, the dindar solution that step S2 is obtained is spin-dried for, obtains ultra-thin two-dimension spin crossover nano material.
5. the preparation method according to claim 4, which is characterized in that solvent described in step S1 is water or alcoholic solvent.
6. the preparation method according to claim 4, which is characterized in that three-dimensional Van der Waals complex described in step S1 and molten
The ratio of agent is 5-20mg:30-100mL.
7. the preparation method according to claim 4, which is characterized in that being spin-dried for temperature described in step S3 is 30-80 DEG C.
8. the ultra-thin two-dimension spin crossover nano material that preparation method described in claim 1-7 any one is prepared.
9. ultra-thin two-dimension spin crossover nano material according to claim 8, which is characterized in that the ultra-thin two-dimension spin
Crossing nanotube material with a thickness of 1-10nm, lateral dimension is 0.5-2 μm.
10. ultra-thin two-dimension spin crossover nano material described in claim 8 is in preparation for information storage, molecular switch or molecule
Application in the molecular electronic device of display.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111073630A (en) * | 2019-12-02 | 2020-04-28 | 东南大学 | Near-infrared light triggered three-dimensional spin cross nano composite material and preparation and application thereof |
| CN111073630B (en) * | 2019-12-02 | 2022-03-08 | 东南大学 | Near-infrared light triggered three-dimensional spin cross nano composite material and preparation and application thereof |
| CN111252803A (en) * | 2020-01-15 | 2020-06-09 | 东南大学 | Square AgCl nanoparticles and preparation method and application thereof |
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| CN111282545B (en) * | 2020-02-10 | 2022-03-11 | 东南大学 | Two-dimensional van der waals heterojunction and application thereof |
| CN113354841A (en) * | 2021-05-27 | 2021-09-07 | 东南大学 | Three-dimensional spin cross gel material, preparation method and application |
| CN113354841B (en) * | 2021-05-27 | 2022-06-28 | 东南大学 | Three-dimensional spin cross gel material, preparation method and application |
| CN114524947A (en) * | 2022-03-10 | 2022-05-24 | 淮阴师范学院 | Complex molecular switch based on cis-trans isomerization of olefin and application thereof |
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