CN113189051B - Method for preparing magneto-optical glass-based periodic nanopore magnetic plasma sensor - Google Patents
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Abstract
The invention discloses a preparation method of a magneto-optical glass based periodic nanopore magnetic plasma sensor, which is used for constructing the magnetic plasma sensor based on a nonreciprocal effect based on a periodic nanopore magnetic plasma structure of high-performance magneto-optical glass, can quickly and sensitively react to tiny changes of the refractive index or the dielectric constant of a substance to be detected, is an advanced sensing technology with high sensing efficiency, high sensitivity and low cost, and can be widely applied to the fields of biology, medical sensing, environmental monitoring and the like in the plasma sensing technology.
Description
Technical Field
The invention belongs to the field of biosensor preparation, and particularly relates to a preparation method of a magneto-optical glass-based periodic nanopore magnetic plasma sensor.
Background
Until now, the technology for manufacturing magneto-optical devices constructed by tiny optical elements and optical fiber elements has been developed and matured basically and has been successfully applied to optical sensing and optical communication networks, but these sensors are not only large in size and high in manufacturing cost, but also discrete devices cannot be applied to high-precision optical information processing chips; driven by the integration of device functions, the manufacture of a nano-structure magneto-optical device (represented by a plasma nano-structure magneto-optical sensor) becomes a main attack direction of researchers, and the advantage of nano-integration of the magneto-optical device not only greatly reduces the size of the device and reduces the cost, but also can improve the sensitivity of optical sensing.
The magnetic plasma nanostructure is a basic structural unit of the integrated magneto-optical sensor and is also the most effective platform for realizing the magneto-optical sensor, the structure can overcome the light diffraction limit, gather the light field energy to the nanometer level, not only can obviously enhance the interaction of light and substances, excite a plurality of SPR modes and enhance the magneto-optical effect, but also can effectively and accurately control the light through an external magnetic field, induce the nonreciprocal effect of substances, provide high-sensitivity magneto-optical induction for advanced fields of optical sensing, biological sensing, photocatalysis, terahertz and the like, although magnetic plasma nanostructure integration has been realized on a composite film at present, the design and manufacture of the magnetic plasma nanostructure are still not ideal enough, and the magnetic plasma nanostructure is a bottleneck realized by an integrated magneto-optical sensor (the light transmittance in a visible light region is not ideal, the resonance peak is wider, and the magneto-optical effect is limited), and mainly embodied in the following aspects:
1) the continuous (non-periodic) magnetic plasma structure is adopted, the optical absorption (especially a magnetic film) of the structure is too large to consume the resonance energy of the conducted plasma, the lost energy is quickly converted into larger resonance line width, so that the spectrum is widened and the spectral resolution is reduced, and the non-periodic structure only supports the transmission of a single resonance wave (conducted SPR), so that the sensing sensitivity is limited;
2) most of the designs of the magnetic plasma structure are based on transparent BK glass, but the refractive index of the BK glass is small (1.42), a strong resonance peak is easily caused at a gold/glass interface, thereby interfering with the spectral analysis of the conducted plasma and the localized plasma, there have been studies to solve the problem by sandwiching a high refractive index silicon nitride layer between a glass and a gold layer, the high-refractive-index silicon nitride is introduced to inhibit the oscillation amplitude and the light energy consumption of light on a metal and glass interface, so that the refractive indexes of the nano structure are better matched, and the wave spectrum can be effectively separated, however, a silicon nitride film with a high melting point is deposited on the glass, so that the cost is improved, the structural complexity is increased, the light energy consumption is increased, and even signal interference exists, with the increase of the thickness of the silicon nitride film, an optical wavelength window generates red shift, the light transmittance is extremely reduced, and the sensing application of a visible light wave band is not facilitated;
3) the magneto-optical materials used (including ferromagnetic and ferrite materials) have significant limitations: ferromagnetic materials BIG and the like have high magneto-optical activity, but the application of the ferromagnetic materials BIG and the like on optical devices is limited by the extremely high light absorption coefficient; although the ferrite magnetic material has the advantages of high magnetic optical activity and low optical absorption coefficient, the ferrite magnetic material has high cost as a single crystal, the lattice constant and the thermal expansion coefficient of the ferrite magnetic material are extremely difficult to match with glass, the obtained nonreciprocal effect is limited, the growth process of the ferrite magnetic material needs high temperature of 700 ℃, and the wide application of the ferrite magnetic material is greatly restricted;
therefore, although the magnetic plasma structure has an attractive prospect of being capable of regulating and controlling the excitation of plasma and magneto-optical effects through an external magnetic field, due to the problems of the magnetic plasma nanostructure in design and manufacture, the existing integrated magneto-optical sensor cannot meet the increasingly urgent requirements of optical communication and optical sensing systems.
Disclosure of Invention
In order to overcome the technical defects in the prior art, the invention constructs a periodic nanopore magnetic plasma structure based on high-performance magneto-optical glass, and constructs a high-sensitivity optical sensor based on the structure.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for preparing a magneto-optical glass-based periodic nanopore magnetic plasma sensor comprises the following steps:
1) preparing a magneto-optical glass prism: according to (35-40) Bi 2 O 3 -(40-45)PbO-(8-10)H 3 BO 3 -(2-5)GeO 2 (2-5) the molar ratio of BaO glass raw materials are weighed, stirred and subjected to N at the temperature of 900 ℃ and 1000 DEG C 2 Casting into prism shape after medium melting for 1-1.5 hr, annealing at 300-350 deg.C for 2-3 hr, and optically polishing the upper surface of magneto-optical glass prism to reach surface roughness<100nm, flatness>7(ASTM standard);
2) preparation of magneto-optical glass based multilayer film structure: cleaning the upper surface of the magneto-optical glass prism with deionized water, purging with ammonia gas for 2-4 min under the pressure of 5-8.0 × 10 before deposition -5 Pa, transferring the magneto-optical glass prism to a magnetron sputtering vacuum chamber, filling Ar gas to ensure that the total pressure reaches 0.6-1 Pa, the power is 60W, sputtering the gold target at the temperature of 120-150 ℃, naturally cooling to room temperature after 9-15 hours to obtain a gold film, then exchanging the sputtering target, and reducing the initial pressure to 3-5.0 x 10 -1 Pa, power of 60-80W, keeping temperature unchanged, codepositing Fe and Co in the mixed atmosphere of argon and oxygen for 6-10 hours, and cooling to obtain Fe 3 O 4 &Repeatedly sputtering a layer of gold film on the Co film, and then annealing at the temperature of 300-350 ℃ for 1-2 hours to obtain a magneto-optical glass multi-layer film structure;
3) preparing a periodic nanopore matrix by adopting a hot pressing method: aligning the prepared magneto-optical glass-based multilayer film structure and the nano-pore nickel alloy film, then placing the film structure and the nano-pore nickel alloy film into a hot-pressing vacuum cavity for fixing, setting the heating rate to be 4-6 ℃/min, applying 10-15MP pressure when the temperature reaches 350-365 ℃, keeping for 2-5 minutes, then removing the pressure, and cooling to room temperature to obtain a magneto-optical glass-based periodic nano-pore magnetic plasma structure;
4) constructing a sensing system: one end of the prepared magneto-optical glass based periodic nanopore magnetic plasma structure is connected with a laser through an optical fiber, the other end of the prepared magneto-optical glass based periodic nanopore magnetic plasma structure is connected with a spectrometer and a detector through an optical fiber, a biological sensing film is coated on the surface of the magneto-optical glass based periodic nanopore magnetic plasma structure through a spin coating method, then the magneto-optical glass based periodic nanopore magnetic plasma structure is placed in a sensing substance, when the sensing substance is adsorbed by the sensing film, the concentration is increased, the refractive index and the dielectric constant of the sensing film are changed, the plasma effect is excited, spectrum shift is generated, and biomolecule concentration information is obtained according to the spectrum shift.
Preferably, the melting in step 1) is in air or N 2 In (1).
Preferably, the gold film and Fe in step 2) 3 O 4 &The thickness of the Co film is 100-150 nm.
Preferably, the volume ratio of argon to oxygen in step 2) is 1: 1-1.2.
Preferably, the diameter of the periodic nanopores in the step 3) is 200-220nm, the pore spacing is 400-450nm, and the pore depth is 50-100 nm.
Preferably, the thickness of the biosensing membrane in step 4) is 50-80 nm.
The invention has the following beneficial effects:
firstly, the adoption of the periodic nanopore structure not only avoids the prism excitation mode, but also enables the device to be more easily miniaturized and integrated into a nanometer device, and the local plasma effect is excited, the double superposition of the local plasma effect and the surface plasma effect is realized (free electrons in the Au film continuous between holes are driven by an electromagnetic field to generate collective oscillation on the surface of the film to generate conductive SPR, and a local SPR resonance excited by the nano holes per se generates a great electromagnetic field in a dozen of nano areas on the surface of the film along with the electromagnetic field), the sensing efficiency is improved, various defects in the traditional sensing are avoided, the sensing sensitivity is greatly increased, can quickly and sensitively react to the tiny change of the refractive index or the dielectric constant of a substance to be measured, is an advanced sensing technology with high sensing efficiency, high sensitivity and low cost, the method can be widely applied to the fields of biology, medical sensing, environmental monitoring and the like in the plasma sensing technology;
secondly, the heavy metal oxide magneto-optical glass with large refractive index and good magneto-optical performance is used as a substrate, so that the light transmittance of optical energy in an optical band is effectively improved, the optical energy consumption or signal loss caused by the resonance of the optical energy at a gold film/glass interface due to the mismatch of the refractive indexes is suppressed, the spectral resolution is increased, and the magneto-optical performance of the system is greatly improved;
③ use strong magnetic Fe 3 O 4 &The Co nano composite film provides good magnetism and low absorption, realizes the magnetic plasma effect, and has strong magnetism Fe 3 O 4 &The Co nano composite film can be cooperated with magneto-optical glass (substrate) with high magneto-optical activity to increase magneto-optical effect (except Fe under the action of external magnetic field) of magnetic plasma structure 3 O 4 &The magneto-optical rotation generated by the Co magnetic film, the magneto-optical glass with high magneto-optical activity also generates magneto-optical rotation to the polarization signal, and because the magneto-optical effects are not different, the angles of the two rotations can be superposed and enhanced, so that the magneto-optical effect of the magnetic plasma structure is greatly enhanced).
Drawings
FIG. 1 is a structural diagram of a magneto-optical glass-based periodic nanopore magnetic plasma sensor in embodiment 1 of the present invention;
FIG. 2 is an electron micrograph and a photograph of periodic nanopores prepared in example 1 of the present invention;
FIG. 3 is a nanopore parameter versus Au/Fe in example 2 of the invention 3 O 4 &The plasma effect of Co/Au;
FIG. 4 shows Au/Fe in example 2 of the present invention 3 O 4 &Co/Au films versus general film refractivity.
Detailed Description
The invention is further illustrated by the following specific examples.
Example 1
1) Preparing a magneto-optical glass prism: according to 35Bi 2 O 3 -45PbO-10H 3 BO 3 -5GeO 2 Glass raw materials were weighed at a molar ratio of-5 BaO, stirred and then subjected to N at 900 deg.C 2 Casting into prism shape after medium melting for 1 hr, annealing at 350 deg.C for 3 hr, and optically polishing the upper surface of glass prism to reach surface roughness<100nm, flatness>7；
2) Preparing a multilayer film structure on the upper surface of a magneto-optical glass prism: cleaning the upper surface of the magneto-optical glass prism with deionized water, purging with ammonia gas for 2 min, and controlling the pressure before deposition to be 8.0 × 10 -5 Pa, transferring the magneto-optical glass prism to a magnetron sputtering vacuum chamber, filling Ar gas to ensure that the total pressure reaches 0.6 Pa, the power is 60W, sputtering a gold target at the temperature of 150 ℃, naturally cooling to room temperature after 12 hours to obtain a gold film with the thickness of 150nm, then exchanging the sputtering target, reducing the initial pressure to 5.0 multiplied by 10 -1 Pa, power of 80W, keeping temperature unchanged, codepositing Fe and Co for 8 hours in mixed atmosphere obtained by mixing argon and oxygen according to volume ratio of 1:1, and cooling to obtain Fe with thickness of 150nm 3 O 4 &Repeatedly sputtering a layer of gold film with the thickness of 150nm on the Co film, and then annealing for 2 hours at 350 ℃ to obtain a magneto-optical glass multi-layer film structure;
3) preparing a periodic nanopore matrix by adopting a hot pressing method: aligning the prepared magneto-optical glass-based multilayer film structure and the nano-pore nickel alloy film, then placing the aligned magneto-optical glass-based multilayer film structure and the nano-pore nickel alloy film into a hot-pressing vacuum chamber for fixing, setting the temperature rise speed to be 5 ℃/min, applying 10MP pressure when the temperature reaches 365 ℃, keeping for 2 minutes, then removing the pressure, and cooling to room temperature to obtain a magneto-optical glass-based periodic nano-pore magnetic plasma structure;
4) constructing a sensing system: one end of the prepared magneto-optical glass based periodic nanopore magnetic plasma structure is connected with a laser through an optical fiber, the other end of the magneto-optical glass based periodic nanopore magnetic plasma structure is connected with a spectrometer and a detector through an optical fiber, a biological sensing film is coated on the surface of the magneto-optical glass based periodic nanopore magnetic plasma structure by a spin coating method to be 50nm, the magneto-optical glass based periodic nanopore magnetic plasma structure is placed in a substance for sensing sulfur dioxide, when the sensing film absorbs and senses sulfur dioxide, the concentration of the sensing film is increased, the refractive index and the dielectric constant of the sensing film are changed, the plasma effect is excited, spectrum deviation is generated, and biomolecule concentration information is obtained according to the spectrum deviation; the detection result is as follows:magneto-optical glass based Au/Fe 3 O 4 &The sensing range of the Co/Au/nano-pore structure magnetic plasma biosensing on sulfur dioxide gas is 0-10ppm, the resolution of the sensing sulfur dioxide is 0.01ppm, and the sensing sensitivity is 0.5ppm SiO 2 The sensitivity was 50000 nA/ppm.
Magneto-optical glass based Au/Fe in example 1 3 O 4 &The structure of the magnetic plasma biosensor with the Co/Au/nanopore structure is shown in figure 1, and the periodic nanopore prepared in example 1 is shown in figure 2, so that the magnetic plasma biosensor has the advantages of small surface damage area to a gold film, uniform pore diameter, consistent depth and good periodicity.
Example 2
1) Preparing a magneto-optical glass prism: according to 40Bi 2 O 3 -40PbO-10H 3 BO 3 -3GeO 2 Glass raw materials were weighed at a molar ratio of-7 BaO, stirred and then N was added at 950 ℃ 2 Casting into prism shape after medium melting for 1 hr, annealing at 300 deg.C for 2 hr, and optically polishing the upper surface of glass prism to reach surface roughness<100nm, flatness>7；
2) Preparing a multilayer film structure on the upper surface of the magneto-optical glass prism: cleaning the upper surface of the magneto-optical glass prism with deionized water, purging with ammonia gas for 3 minutes, wherein the pressure before deposition is 6.0 × 10 -5 Pa, transferring the sample to a magnetron sputtering vacuum chamber, filling Ar gas to ensure that the total pressure reaches 0.6 Pa, the power is 60W, sputtering a gold target at the temperature of 120 ℃, naturally cooling to room temperature after 12 hours to obtain a gold film with the thickness of 120nm, then exchanging the sputtering target, and reducing the initial pressure to 5.0 multiplied by 10 -1 Pa, power of 80W, keeping temperature unchanged, codepositing Fe and Co for 8 hours in mixed atmosphere obtained by mixing argon and oxygen according to volume ratio of 1:1, and cooling to obtain Fe with thickness of 80nm 3 O 4 &Repeatedly sputtering a layer of gold film with the thickness of 120nm on the Co film, and then annealing for 2 hours at 350 ℃ to obtain a magneto-optical glass multi-layer film structure;
3) preparing a periodic nanopore matrix by adopting a hot pressing method: aligning the prepared magneto-optical glass based multilayer film structure and the nanopore nickel alloy film, then placing the aligned magneto-optical glass based multilayer film structure and the nanopore nickel alloy film into a hot-pressing vacuum cavity for fixing, setting the heating speed to be 5 ℃/min, applying 10MP pressure when the temperature reaches 355 ℃, keeping for 2 minutes, then removing the pressure, and cooling to room temperature to obtain a magneto-optical glass based periodic nanopore magnetic plasma structure;
4) constructing a sensing system: one end of the prepared magneto-optical glass based periodic nanopore magnetic plasma structure is connected with a laser through an optical fiber, the other end of the magneto-optical glass based periodic nanopore magnetic plasma structure is connected with a spectrometer and a detector through an optical fiber, a biological sensing film is coated on the surface of the magneto-optical glass based periodic nanopore magnetic plasma structure by a spin coating method to be 60nm, the magneto-optical glass based periodic nanopore magnetic plasma structure is placed in a substance for sensing sulfur dioxide, when the sensing film absorbs and senses sulfur dioxide, the concentration of the sensing film is increased, the refractive index and the dielectric constant of the sensing film are changed, the plasma effect is excited, spectrum shift is generated, and biomolecule concentration information is obtained according to the spectrum shift; the detection result is as follows: magneto-optical glass based Au/Fe 3 O 4 &The sensing range of the Co/Au/nano-pore structure magnetic plasma biosensing on sulfur dioxide gas is 0-9ppm, the resolution of the sensing sulfur dioxide is 0.02ppm, and the sensing sensitivity is 0.44ppm SiO 2 The sensitivity was 46000 nA/ppm.
As shown in FIG. 3, the nanopore parameter pair prepared in inventive example 2 is Au/Fe 3 O 4 &The plasma effect of Co/Au influences, and the hole depth of the periodic nano-holes influences the strength and peak position of magnetic plasma, and the plasma performance of the holes with the depth of 70 nm is optimal; FIG. 4 shows Au/Fe in example 2 of the present invention 3 O 4 &The refraction ratios of the Co/Au film and the general film are compared, and Au/Fe can be seen 3 O 4 &The Co/Au film has sharp and symmetrical refractivity and has a sensitive reaction capability to the sensing substance.
The foregoing detailed description is intended to illustrate and not limit the invention, which is intended to be within the spirit and scope of the appended claims, and any changes and modifications that fall within the true spirit and scope of the invention are intended to be covered by the following claims.
Claims (5)
1. A method for preparing a magneto-optical glass-based periodic nanopore magnetic plasma sensor is characterized by comprising the following steps of:
1) preparing a magneto-optical glass prism: according to (35-40) Bi 2 O 3 -(40-45)PbO-(8-10)H 3 BO 3 -(2-5)GeO 2 (2-5) weighing glass raw materials according to the BaO molar ratio, stirring, melting at the temperature of 900 ℃ and 1000 ℃ for 1-1.5 hours, casting into a prism shape, annealing at the temperature of 300 ℃ and 350 ℃ for 2-3 hours, and optically polishing the upper surface of the magneto-optical glass prism to achieve surface roughness<100nm, flatness>7；
2) Preparation of magneto-optical glass based multilayer film structure: cleaning the upper surface of the magneto-optical glass prism with deionized water, purging with ammonia gas for 2-4 min under the pressure of 5-8.0 × 10 before deposition -5 Pa, transferring the magneto-optical glass prism to a magnetron sputtering vacuum chamber, filling Ar gas to ensure that the total pressure reaches 0.6-1 Pa, the power is 60W, sputtering the gold target at the temperature of 120-150 ℃, naturally cooling to room temperature after 9-15 hours to obtain a gold film, then exchanging the sputtering target, and reducing the initial pressure to 3-5.0 x 10 -1 Pa, power of 60-80W, keeping temperature unchanged, codepositing Fe and Co in the mixed atmosphere of argon and oxygen for 6-10 hours, and cooling to obtain Fe 3 O 4 &Repeatedly sputtering a layer of gold film on the Co film, and then annealing at the temperature of 300-350 ℃ for 1-2 hours to obtain a magneto-optical glass multi-layer film structure;
3) preparing a periodic nanopore matrix by adopting a hot pressing method: aligning the prepared magneto-optical glass-based multilayer film structure and the nano-pore nickel alloy film, then placing the film structure and the nano-pore nickel alloy film into a hot-pressing vacuum cavity for fixing, setting the heating rate to be 4-6 ℃/min, applying 10-15MP pressure when the temperature reaches 350-365 ℃, keeping for 2-5 minutes, then removing the pressure, and cooling to room temperature to obtain a magneto-optical glass-based periodic nano-pore magnetic plasma structure;
4) constructing a sensing system: one end of the prepared magneto-optical glass based periodic nanopore magnetic plasma structure is connected with a laser through an optical fiber, the other end of the prepared magneto-optical glass based periodic nanopore magnetic plasma structure is connected with a spectrometer and a detector through an optical fiber, a biological sensing film is coated on the surface of the magneto-optical glass based periodic nanopore magnetic plasma structure through a spin coating method, then the magneto-optical glass based periodic nanopore magnetic plasma structure is placed in a sensing substance, when the sensing substance is adsorbed by the sensing film, the concentration is increased, the refractive index and the dielectric constant of the sensing film are changed, the plasma effect is excited, spectrum shift is generated, and biomolecule concentration information is obtained according to the spectrum shift.
2. The method of claim 1, wherein: the melting in the step 1) is carried out in air or N 2 In (1).
3. The method of claim 1, wherein: gold film and Fe in step 2) 3 O 4 &The thickness of the Co film is 100-150 nm.
4. The method of claim 1, wherein: the volume ratio of the argon to the oxygen in the step 2) is 1: 1-1.2.
5. The method of claim 1, wherein: the thickness of the biological sensing film in the step 4) is 50-80 nm.
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