CN111204705B - Preparation method of directionally assembled core-cap heterogeneous dimer structure - Google Patents
Preparation method of directionally assembled core-cap heterogeneous dimer structure Download PDFInfo
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- 239000000539 dimer Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 125
- 239000011258 core-shell material Substances 0.000 claims abstract description 43
- 239000002086 nanomaterial Substances 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000000758 substrate Substances 0.000 claims description 62
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 38
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 38
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 38
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims description 33
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims description 33
- 238000005530 etching Methods 0.000 claims description 22
- 238000001312 dry etching Methods 0.000 claims description 17
- 239000007787 solid Substances 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 10
- 239000000833 heterodimer Substances 0.000 claims description 10
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 8
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002955 isolation Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- -1 polydimethylsiloxane Polymers 0.000 claims description 5
- 229920000642 polymer Polymers 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000000861 blow drying Methods 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 3
- 239000000710 homodimer Substances 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
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- 238000000576 coating method Methods 0.000 claims 1
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- 238000010168 coupling process Methods 0.000 abstract description 3
- 238000005859 coupling reaction Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000000523 sample Substances 0.000 abstract description 2
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 abstract description 2
- 230000001419 dependent effect Effects 0.000 abstract 1
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- 239000010931 gold Substances 0.000 description 5
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- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
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- 230000005284 excitation Effects 0.000 description 2
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- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
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- 239000000377 silicon dioxide Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
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- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
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- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
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- G01N21/552—Attenuated total reflection
- G01N21/553—Attenuated total reflection and using surface plasmons
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Abstract
The core-cap structured particle has different local surface plasmon resonance modes (LSPR) in the directions perpendicular and parallel to its symmetry axis, and this feature makes its LSPR coupling mode with other particles dependent on the position of dimer binding. For three-dimensional structures such as core caps, assembling another particle to its specific location is a great challenge. The invention discloses a preparation method of a directionally assembled core-cap heterogeneous dimer structure, and belongs to the technical field of nano-structure probes. The central apex region of the crown is automatically obtained using the core-shell nanostructured particles and the linker molecules are exposed to the outside by physical peeling to complete the attachment of the dimers. The method has the beneficial effect that one spherical nano particle is assembled to a specific region of the core cap nano structure particle, namely the central region of the cap top, so that a single dimer structure with stable structure is obtained. The method can be extended to the preparation of a homogeneous dimeric structure consisting of two core-cap particles.
Description
Technical Field
The invention belongs to the technical field of nano-structure probes, relates to nano-structure assembly, and particularly relates to a preparation method of a directionally assembled core-cap heterogeneous dimer structure.
Background
The self-assembly of the manually controlled nanoparticles has wide application potential in related fields of nanotechnology, including photoelectron, biological/medical diagnosis and treatment and the like. Two nanoparticles with surface plasmon resonance (LSPR) effect are of interest due to the electromagnetic field variation caused by the LSPR resonant coupling between them and the unique photoelectric property variation that the field acts on the surrounding material. However, it is not easy to self-assemble two nano-structured particles into a dimer structure, because in a uniformly dispersed and stable particle solution system, the surface of each particle is usually modified with a stabilizer, so that the surface of each particle is uniformly charged to keep a certain distance from each other to avoid particle agglomeration, and after surface modification, the equilibrium system is broken, which easily causes association agglomeration; in addition, after the connecting molecules enter a solution system, the connecting molecules are randomly bonded to the surfaces of the particles, so that the surfaces of the particles can obtain a plurality of bonding points, and a plurality of particles can be bonded to one particle through the bonding points to generate agglomeration and even cascade agglomeration. In order to avoid agglomeration, the number and distribution of the molecules attached to the particle surface need to be precisely controlled, and the self-assembly of dimers now occurs mainly in isotropic spherical symmetric structures. The situation becomes more complicated by the directionally assembled core cap, which is an asymmetric structure.
The core cap nanostructure is characterized in that the outer surface of the spherical core is wrapped with an unclosed continuous metal shell layer, and the depth of the cap can be smaller than, equal to or larger than a half shell (as shown in figure 1) according to the proportion of the shell layer covering the surface of the core. The structure is an axisymmetric structure, and the optical property of the structure strongly depends on the orientation between an excitation light electric field and a symmetry axis. The electric field of the excitation light causes different LSPR modes in directions parallel and perpendicular to its symmetry axis, respectively. Thus, when another particle is close to the core-cap particle, the change in optical properties resulting from the LSPR resonant coupling between the two depends on the point of bonding of the two. The core-cap heterodimer is formed by connecting a core-cap nano-structured particle A and a spherical symmetrical structure particle B, and when a binding point is positioned in the central vertex area of the outer surface of the cap of A, the assembled dimer can generate enhanced optical performance and remove the dependence on the polarization direction of exciting light. The directed assembly of B to a specific position of a is a challenge, since not only the number of attached molecules but also the position of their growth needs to be controlled. The preparation of AB heterodimers assembled via the central region of the crown of A has not been reported.
Disclosure of Invention
The invention aims to provide a method for preparing a directionally assembled core cap heterogeneous dimer structure, and provides an automatic acquisition method of a central region of a three-dimensional core cap top and a method for preparing a heterogeneous/homogeneous dimer formed by connecting the central region.
The technical scheme of the invention is as follows:
a method for preparing a directionally assembled core-cap heterogeneous dimer structure, the core-cap heterogeneous dimer structure is assembled by a core-cap nano-structure particle A and a spherical nano-structure particle B through connecting molecules, the connecting molecules are positioned in the central peak area of the cap surface of the core-cap nano-structure particle A, and the preparation method comprises the following steps:
1) the method for acquiring the center position of the connecting molecule automatic crown comprises the following steps: combining the core-shell nano-structure particles C which are spherically symmetrical with connecting molecules on a substrate randomly to obtain a combination position P, then carrying out dry etching along the reverse direction of the external normal of the substrate where the combination position P is located, removing a part of shells of the core-shell nano-structure particles C by utilizing the high anisotropy of the dry etching through directional etching, forming core-cap nano-structure particles A on the substrate, and naturally positioning the connecting molecules in the cap top central region of the core-cap nano-structure particles A;
2) the preparation method of the directionally assembled core-cap heterogeneous dimer structure comprises the following steps:
i) growing connecting molecules on a cleaned planar substrate (comprising a glass sheet, a silicon wafer and the like);
ii) immersing the substrate in the solution of core-shell nanostructured particles C, the linker molecule fixing the core-shell nanostructured particles C to the substrate;
iii) after the substrate is dried, carrying out dry etching along the reverse direction of the external normal of the substrate, removing a part of shells of the core-shell nano-structure particles C by directional etching to form core-cap nano-structure particles A, and connecting the core-cap nano-structure particles A to the substrate by connecting molecules through the cap top central region of the core-cap nano-structure particles A;
iv) covering a polymer isolation layer with a certain thickness on the substrate on which the core cap nano-structure particles A are grown;
v) continuously pouring PDMS with a certain thickness on the substrate and heating and curing the PDMS, wherein the PDMS is formed by mixing polydimethylsiloxane and a curing agent according to a proportion;
vi) tearing off the PDMS cured film from the substrate, transferring the core cap nano-structured particles A onto the PDMS cured film, and exposing the cap top central area of the core cap nano-structured particles A grown with the connecting molecules from the PDMS;
vii) immersing the PDMS prepared in step vi) in a solution containing spherical nanostructured particles B, such that the spherical nanostructured particles B are bound to the cap top central region of the core cap nanostructured particles a, forming a directionally bound core cap heterodimeric structure. The structure of the spherical nano-structure particles B comprises spherical symmetrical structures such as solid spheres, hollow sphere shells, solid core shells and the like;
the structure of the core-shell nano-structured particle C with spherical symmetry can be a hollow spherical shell or a solid core-shell structure with spherical symmetry;
the core cap nano-structured particles A are prepared by directionally etching core shell nano-structured particles C with spherical symmetry, and the shape of the cap depends on and is controlled by the etching depth;
the preparation method of the directionally combined core-cap isomeric dimer structure can be extended to the preparation of the core-cap isomeric dimer structure with the cap combined in a back-to-cap manner.
The invention has the beneficial effects that: a core-cap nano-structure particle A and a spherical nano-structure particle B are assembled into a core-cap heterogeneous dimer structure through connecting molecules, the connecting molecules are located in the central vertex area of the cap surface of the particle A, and the structure can be used for high-specificity molecular detection and identification.
Drawings
FIG. 1 is a core capped nanostructured particle, the cap being comprised of an unsealed metal shell layer wrapped around the outer surface of the core, the cap having a depth which may be less than, equal to, or greater than the half shell shape. Wherein (a) is a half shell core cap nanostructure, (b) the depth of the cap is less than the half shell, and (c) the depth of the cap is greater than the half shell.
FIG. 2 is a heterogeneous dimeric structure of a semi-shell shaped nano-structured particle connected with a solid nanogold sphere through a central region of a shell top;
FIG. 3 is a homodimeric structure of one core-capped nanostructured particle back-coupled to another core-capped nanostructured particle through the central apex region of the cap top;
FIG. 4 is a heterodimeric structure of core-capped nanostructured particles connected to core-shell nanostructured particles through the central apex region of the cap top.
Detailed Description
The preferred embodiments will be described in detail below with reference to the accompanying drawings. It should be emphasized that the following description is merely exemplary in nature and is not intended to limit the scope of the invention or its application.
Example 1:
the preparation method of the directionally assembled core-cap heterodimer structure is characterized in that the core-cap heterodimer structure is composed of a half-shell core-shell nanoparticle A1 (the core is SiO)2Sphere, Au half shell) and a solid gold sphere nanoparticle B1 were assembled via linker molecules (see fig. 2) located in the central apex region of the half shell surface of particle a1, the preparation method being characterized by: 1) the method for acquiring the center position of the automatic shell top of the connecting molecule comprises the following steps: core-shell nanostructured particles C1 (SiO) with spherical symmetry2@ Au, core of SiO2Ball, the outer surface of which is 100% covered with Au shell) is randomly combined with connecting molecules on the substrate to obtain a combination point P1, then dry etching is carried out along the reverse direction of the outer normal of the substrate where the combination position P1 is located, a part of the shell of C1 is removed by directional etching by utilizing the high anisotropy of the dry etching, a half-shell-shaped core-shell nanoparticle A1 is formed on the substrate, and the connecting molecules are naturally located in the shell top central region of the particle A1; 2) the preparation method of the directionally assembled A1 and B1 isomeric dimer structure is characterized by the following steps,
i) cleaning a glass slide, immersing the glass slide in a polyvinylpyrrolidone (PVP) alcohol solution overnight to grow a connecting molecule PVP on the glass slide;
ii) immersing the substrate in a solution of particles C1, the linking molecules immobilizing C1 to the substrate;
iii) passing the substrate through N2After blow-drying, carrying out dry etching along the reverse direction of the external normal of the substrate, carrying out directional etching to remove a half shell of C1 to form half-shell core-shell structure particles A1, and connecting molecules connect A1 on the substrate through the central region of the shell top of A1;
iv) covering a substrate grown with A1 with a polymer isolation layer with the thickness of 5 nm;
v) continuously pouring PDMS with a certain thickness on the substrate and heating and curing, wherein the PDMS is formed by mixing polydimethylsiloxane and a curing agent according to a ratio of 10: 1;
vi) tearing off the PDMS cured film from the substrate, transferring the semi-shell core-shell structure particles onto the PDMS cured film, and exposing the PDMS from the cap top region of the particles A1 with the connecting molecules;
vii) dipping the PDMS prepared in step vi) into a solution containing B1, such that B1 binds to the central region of the top of the a1 cap, forming a directionally bound core-cap heterodimeric structure.
The preparation method of the oriented combined core-cap heterogeneous dimer structure is characterized in that the structure of the spherical symmetric nano-structure particles B1 comprises a solid sphere, a hollow spherical shell, a solid core shell and the like;
the preparation method of the directionally combined core-cap heterodimer structure is characterized in that the core-shell nano-structured particle C1 with spherical symmetry has a structure of a spherical-symmetric hollow spherical shell or solid core-shell structure;
the preparation method of the directionally combined core-cap heterogeneous dimer structure is characterized in that the core-cap nano-structured particles A1 are prepared by directionally etching core-shell nano-structured particles C1 with spherical symmetry, and the shape of the cap depends on and is controlled by the depth of etching;
example 2:
a method for preparing directionally assembled core-cap heterodimer structure can be extended to the preparation of core-cap homodimer structure with cap combined with back cap, and the structure is characterized in that the core-cap heterodimer structure is composed of a cap-shaped core-shell nanoparticle A2 (the core is SiO)2A sphere, a cap Au shell less than, equal to, or greater than the depth of the half shell) and another cap core shell nanoparticle B2 are assembled via linker molecules (see fig. 3), the two particles being connected via the cap top central region, the caps facing away from each other, the method of preparation being characterized in that: 1) the method for acquiring the center position of the connecting molecule automatic crown comprises the following steps: core-shell nanostructured particles C2 (SiO) with spherical symmetry2@ Au, core of SiO2Ball, outer surface 100% covered Au shell) is randomly combined with the connecting molecules on the substrate to obtain a combination point P2, then dry etching is carried out along the reverse direction of the outer normal of the substrate where the combination position P2 is located, a part of the shell of C2 is removed by directional etching by utilizing the high anisotropy of the dry etching, core-cap nano-structured particles A2 are formed on the substrate, and the core-cap nano-structured particles A2 are connected with the connecting moleculesThe linker molecule is naturally located in the central region of the crown of particle a 2; 2) the preparation method of the directionally assembled A2B 2 isomeric dimer structure is characterized by the following steps,
i) after being cleaned, the glass slide is immersed in a polyvinylpyrrolidone (PVP) alcohol solution for overnight so as to grow the connecting molecule PVP on the glass slide;
ii) immersing the substrate in a solution of particles C2, the linking molecules immobilizing C2 to the substrate;
iii) passing the substrate through N2After blow-drying, carrying out dry etching along the reverse direction of the external normal of the substrate, removing a part of shells of C2 by directional etching to form core cap nano-structure particles A2, and connecting molecules to A2 on the substrate through the cap top central region of A2;
iv) covering a substrate grown with A2 with a polymer isolation layer with the thickness of 5 nm;
v) continuously pouring PDMS with a certain thickness on the substrate and heating and curing, wherein the PDMS is formed by mixing polydimethylsiloxane and a curing agent according to a ratio of 10: 1;
vi) tearing off the PDMS cured film from the substrate, transferring the semi-shell core-shell structure particles onto the PDMS cured film, and exposing the PDMS from the cap top region of the particles A2 with the connecting molecules;
vii) dipping the PDMS prepared in step vi) into a solution containing C2 so that C2 binds to the central region of the crown of a2 (see fig. 4);
viii) dry etching is performed in the opposite direction of the substrate outer normal, directional etching removes a part of the shell of C2 grown from the previous step, forming core-capped nano-structured particles B2, and linker molecules link B2 to the substrate via the cap top central region of a2, the caps of both facing away from each other.
The preparation method of the directionally combined core-cap heterodimer structure is characterized in that the core-shell nano-structured particle C2 with spherical symmetry has a structure of a spherical-symmetric hollow spherical shell or solid core-shell structure;
the preparation method of the directionally combined core-cap heterodimer structure is characterized in that the core-cap nano-structured particles A2 are prepared by directionally etching core-shell nano-structured particles C2 with spherical symmetry, and the shape of the cap depends on and is controlled by the depth of etching.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the technical scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.
Claims (7)
1. A method for preparing a directionally assembled core-cap heterogeneous dimer structure is characterized in that the core-cap heterogeneous dimer structure is assembled by a core-cap nano-structure particle A and a spherical nano-structure particle B through connecting molecules, and the connecting molecules are positioned in the central vertex area of the cap surface of the core-cap nano-structure particle A, and the method for preparing the core-cap heterogeneous dimer structure comprises the following steps:
1) the method for acquiring the center position of the connecting molecule automatic crown comprises the following steps: combining the core-shell nano-structure particles C which are spherically symmetrical with connecting molecules on a substrate randomly to obtain a combination position P, then carrying out dry etching along the reverse direction of the outer normal of the substrate where the combination position P is located, removing a part of shells of the core-shell nano-structure particles C by utilizing the anisotropy of the dry etching through directional etching, forming core-cap nano-structure particles A on the substrate, and naturally positioning the connecting molecules in the cap top central region of the core-cap nano-structure particles A;
2) the preparation method of the directionally assembled core-cap heterogeneous dimer structure comprises the following steps:
i) growing connecting molecules on the cleaned planar substrate;
ii) immersing the substrate in the solution of core-shell nanostructured particles C, the linker molecule fixing the core-shell nanostructured particles C to the substrate;
iii) after the substrate is dried, carrying out dry etching along the reverse direction of the external normal of the substrate, removing a part of shells of the core-shell nano-structure particles C by directional etching to form core-cap nano-structure particles A, and connecting the core-cap nano-structure particles A to the substrate by connecting molecules through the cap top central region of the core-cap nano-structure particles A;
iv) covering a polymer isolation layer on the substrate on which the core cap nano-structure particles A grow;
v) continuously pouring PDMS on the substrate and heating and curing the PDMS, wherein the PDMS is formed by mixing polydimethylsiloxane and a curing agent according to a proportion;
vi) tearing off the PDMS cured film from the substrate, transferring the core cap nano-structured particles A onto the PDMS cured film, and exposing the cap top central area of the core cap nano-structured particles A grown with the connecting molecules from the PDMS; vii) immersing the PDMS prepared in step vi) in a solution containing spherical nanostructured particles B, such that the spherical nanostructured particles B are bound to the cap top central region of the core cap nanostructured particles a, forming a directionally bound core cap heterodimeric structure.
2. The method for preparing the directionally assembled core-cap heterodimer structure of claim 1, wherein the spherical nanostructured particles B have a structure of solid spheres, hollow spherical shells or solid core shells.
3. The method for preparing the directionally assembled core-cap heterodimer structure as claimed in claim 1 or 2, wherein the core-shell nanostructure particles C with spherical symmetry have a structure of a hollow spherical shell or a solid core-shell structure with spherical symmetry.
4. The method for preparing a directionally assembled core-cap heterodimeric structure according to claim 1 or 2, wherein the core-cap nanostructured particles a are prepared by directionally etching core-shell nanostructured particles C which are spherically symmetric, and the shape of the cap is determined and controlled by the depth of the etching.
5. The method for preparing a directionally assembled core-cap heterodimeric structure as claimed in claim 3, wherein the core-cap nanostructured particles A are prepared by directionally etching core-shell nanostructured particles C which are spherically symmetric, and the shape of the cap is determined and controlled by the depth of the etching.
6. The method of claim 1, 2 or 5, wherein the substrate is a glass sheet or a silicon sheet.
7. A method for preparing a directionally assembled core-cap homodimer structure is characterized in that the method can be extended to the preparation of core-cap homodimer structures with caps assembled back to caps; the structure is characterized in that the core cap isomorphic dimer structure is formed by assembling a core cap nano-structured particle A2 and another core cap nano-structured particle B2 through connecting molecules, the two particles are connected through a cap top central area, and caps are back to each other, and the preparation method is characterized in that: 1) the method for acquiring the center position of the connecting molecule automatic crown comprises the following steps: randomly combining core-shell nano-structured particles C2 which are spherically symmetrical with connecting molecules on a substrate to obtain a combination point P2, then carrying out dry etching along the reverse direction of the external normal of the substrate where the combination position P2 is located, and utilizing the anisotropy of the dry etching to remove a part of shells of the core-shell nano-structured particles C2 by directional etching so as to form core-cap nano-structured particles A2 on the substrate, wherein the connecting molecules are naturally located in the cap top central region of the core-cap nano-structured particles A2; 2) the preparation method of the directionally assembled core-capped nano-structured particles A2 and B2 isomorphic dimer structure is characterized by the following steps,
i) cleaning a glass slide, immersing the glass slide in a polyvinylpyrrolidone alcohol solution overnight to grow a connecting molecule PVP on the glass slide;
ii) immersing the substrate in the core-shell nanostructured particle C2 solution, the linker molecule fixing the core-shell nanostructured particle C2 to the substrate;
iii) passing the substrate through N2After blow-drying, performing dry etching along the reverse direction of the external normal of the substrate, performing directional etching to remove a part of shells of the core-shell nano-structured particles C2 to form core-cap nano-structured particles A2, and connecting the core-cap nano-structured particles A2 to the substrate through the cap top central region of the core-cap nano-structured particles A2 by connecting molecules;
iv) coating a substrate on which the core cap nano-structured particles A2 are grown with a polymer isolation layer with a thickness of 5 nm;
v) continuously pouring PDMS on the substrate and heating and curing the PDMS, wherein the PDMS is formed by mixing polydimethylsiloxane and a curing agent according to a ratio of 10: 1;
vi) tearing off the PDMS cured film from the substrate, transferring the core cap nano-structured particles A2 to the PDMS cured film, and exposing the PDMS from the cap top region of the core cap nano-structured particles A2 grown with the connecting molecules;
vii) dipping the PDMS prepared in step vi) into a solution containing the core shell nanostructured particles C2 such that the core shell nanostructured particles C2 are bound to the cap top central region of the core cap nanostructured particles a 2;
viii) dry etching in the reverse direction of the substrate outer normal, directional etching to remove a part of the shell of the core-shell nanostructured particle C2 grown in the previous step to form the core-cap nanostructured particle B2, and a linker molecule to link the core-cap nanostructured particle B2 to the substrate via the cap top central region of the core-cap nanostructured particle a2, the caps of both facing away from each other.
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