CN101936899A - Long-range surface plasma resonance sensor and preparation method thereof - Google Patents
Long-range surface plasma resonance sensor and preparation method thereof Download PDFInfo
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- CN101936899A CN101936899A CN 201010239204 CN201010239204A CN101936899A CN 101936899 A CN101936899 A CN 101936899A CN 201010239204 CN201010239204 CN 201010239204 CN 201010239204 A CN201010239204 A CN 201010239204A CN 101936899 A CN101936899 A CN 101936899A
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Abstract
The invention discloses a long-range surface plasma resonance sensor and a preparation method thereof. The sensor is formed by bonding a BK7 prism and a glass slide through cedar oil, wherein the outer surface of the glass slide is plated with a magnesium fluoride thin film, a silver film and a gold film in turn; the gold film is directly contacted with biological solution to be detected and is used for detecting the biological solution in a mode of angle modulation; magnesium fluoride with the refractive index of about 1.38, which is close to that of the biological solution, can form approximatively symmetric structures on two sides of a metal conductive layer so as to ensure that surface plasmas on the two sides of the metal conductive layer are coupled to form the long-range surface plasma; compared with other metals, the metal silver used as the conductive layer has a narrower half band width of a resonance absorption peak, but has unsteady chemical properties; a conductive layer gold film can make a resonance angle generate a greater transition along with the change of the refractive index of the biological solution to be detected; simultaneously, the conductive layer gold film has stable chemical properties and high biological affinity. The specific multilayer film structure can integrate the advantages of each film and effectively improve the sensitivity of biological sensors.
Description
Technical field
The present invention relates to biology sensor and preparation thereof, specifically a kind of long-range surface plasma resonance sensor and preparation method.
Background technology
Compare with traditional biochemical analysis method, the surface plasma body resonant vibration biosensor technique have highly sensitive and need not mark, can be in real time, characteristics such as original position continuous detecting, be widely used in fields such as food security, environmental monitoring, pharmacy, chemistry, biology in recent years.At present, this technology has been subjected to common attention, and is able to fast development.
In theory, the halfwidth of the spread length of surface plasma wave and surface plasma body resonant vibration absorption peak exists reciprocal relation.Therefore, the sensitivity of decision spr sensor and the key issue of resolution are the spread lengths of surface plasma wave.Traditional surface plasma body resonant vibration biosensor technique utilizes the surface plasma body resonant vibration effect that results from metal level and the analyte interphase usually.Because surface plasma strong attenuation in metal causes propagation distance shorter, has influenced the sensitivity and the resolution of sensor.When metal level is overmolding to sandwich structure by the medium symmetry, the metal level both side surface is the excitating surface plasma wave respectively, these two surface waves intercouple in metal, electric field is violated the pattern that is symmetrically distributed, the shared component of field intensity is less in metal, and electromagnetic energy mainly concentrates in the medium on both sides, and is less relatively by the caused loss of metal, this surface wave can be propagated very long distance, Here it is so-called long-range surface plasma.With respect to the conventional surface plasma resonance sensor, has higher sensitivity and resolution based on the long-range surface plasma resonance sensor.
In existing long-distance surface plasma resonance sensor, most Teflon AF (n=1.31) of employing or Cytop (n=1.34) do dielectric layer material [3,4-7,8] to form the membrane structure of refractive index symmetry.But TeflonAF has toxicity after heating is disagreed by academia always.Under the plasma wave effect its whether to have potential safety hazard be a problem must considering.MgF2 is a kind of optical filming material of function admirable, and its refractive index is 1.38, satisfies the condition of refractive index symmetry substantially, particularly its have safety non-toxic, chemical stability good, be easy to advantages such as preparation.Therefore, do the dielectric layer material, have using value with MgF2.
Argent is compared with other metals as conducting stratum, and the half-peak breadth of resonance absorbing peak is narrower, but its unstable chemcial property.Conducting stratum gold film can make resonance angle that bigger migration takes place with biological solution variations in refractive index to be measured, and its chemical property is stable simultaneously, bioaffinity good [9].Plate the very thin golden film of one deck on the surface of conducting stratum silverskin, this double-metal layer structure has kept and the thin narrow advantage of the corresponding absorption peak of silverskin well, has had the chemical stability of golden film and the compatibility of biomolecule simultaneously concurrently.
Summary of the invention
The purpose of this invention is to provide the membrane structure that a kind of safety non-toxic, good stability are easy to prepare, can form the long-range surface plasma pattern, reach the sensor and the preparation method that improve sensitivity and resolution, its sensor has thermometal conducting stratum structure, this double-metal layer structure has kept and the thin narrow advantage of the corresponding absorption peak of silverskin well, has had the chemical stability of golden film and the compatibility of biomolecule simultaneously concurrently; Its preparation method is simple, and is easy to operate.
The concrete technical scheme that realizes the object of the invention is:
A kind of long-range surface plasma resonance sensor, this sensor are to be matrix and to constitute by cedar oil stickup microslide that with the BK7 prism outside surface of described microslide is coated with magnesium fluoride film, silverskin and golden film successively on matrix.
The preparation method of the sensor comprises following concrete steps:
A, to select the BK7 prism for use be described sensor base;
B, selection and the identical microslide of BK7 prism material, the size of microslide is slightly less than the bottom surface of BK7 prism;
C, to the microslide plated film
I) ground floor magnesium fluoride film
Adopt magnetron sputtering method that microslide is plated magnesium fluoride film, the vacuum tightness of vacuum chamber is 5 * 10
-4Pa, partial pressure of ar gas are 0.5Pa, and sputtering voltage is radio frequency 700～750V, and frequency is 13.56MHz, and sputtering current is 0.18～0.23A, and sputtering power is 85～117W, and self-bias is 400～440V, and sputtering time is 38～52 minutes; The thickness of magnesium fluoride film is 650nm;
Ii) second layer silver film
Adopt magnetron sputtering method to the microslide silver plating film, the vacuum tightness of vacuum chamber is 5 * 10
-4Pa, partial pressure of ar gas are 0.6Pa, and sputtering voltage is direct current 297～310V, and electric current is 0.04～0.06A, and the time is 2 minutes 15 seconds～3 minutes and 30 seconds; The thickness of silverskin is 35nm;
Iii) the 3rd layer of gold thin film
Adopt magnetron sputtering method to the microslide gold coated films, the vacuum tightness of vacuum chamber is 5 * 10
-4Pa, partial pressure of ar gas are 0.6Pa, and sputtering voltage is direct current 297～310V, and electric current is 0.04～0.06A, and the time is 1 minute 5 seconds～1 minute and 40 seconds; The gold film thickness is 15nm;
D, will be bonded together through the microslide and the BK7 prism of plated film with cedar oil; Wherein: the refractive index of cedar oil and prismatic refraction rate coupling.
The present invention is a high-sensitivity biological sensor, under the pattern of angular modulation, biological solution is detected.Adopt magnetron sputtering plating quality of forming film height, thickness can accurately be controlled, and combination closely between microslide, magnesium fluoride film, silverskin and the golden film.The easy deposit of magnesium fluoride, good stability, the refractive index of its refractive index and biological solution is approaching, can form the near symmetrical structure in the both sides of metal conductive layers, thereby makes the surface plasma coupling of metal conductive layers both sides form long-range surface plasma.Incident light obviously reduces than conventional surface plasma resonance absorption peak with the half-peak breadth of the resonance absorbing peak that long-range surface plasma resonance forms.Argent is compared with other metals as conducting stratum, and the half-peak breadth of resonance absorbing peak is narrower, but its unstable chemcial property.Conducting stratum gold film can make resonance angle that bigger migration takes place with biological solution variations in refractive index to be measured, and its chemical property is stable simultaneously, and bioaffinity is good.This specific multi-layer film structure can be comprehensively separately advantage, the sensitivity that improves biology sensor effectively.
Description of drawings
Fig. 1 is the structural representation of sensor of the present invention
Fig. 2 is the resonance absorbing peak figure of sensor of the present invention when being determinand with water
Embodiment
Embodiment 1
Consult Fig. 1, sensor of the present invention is made of by cedar oil and microslide 2 are bonding BK7 prism 1, and the outside surface of microslide 2 is coated with magnesium fluoride film 3, silverskin 4 and golden film 5 successively; Gold film 5 directly contacts with biological solution to be measured; Total reflection takes place at the interface of microslide 2 and magnesium fluoride film 3 in the P polarized light 6 of incident, and reflected light 7 is received by detector.
Preparation process:
Three-layer thin-film on the microslide 2 all adopts the method for magnetron sputtering to be coated with, to guarantee coating quality and accurately to control thickness; At first plate magnesium fluoride film 3 on microslide, the vacuum tightness of vacuum chamber is 5 * 10
-4Pa, partial pressure of ar gas are 0.5Pa, and sputtering voltage is radio frequency 700V (frequency is 13.56MHz), and sputtering current is 0.18A, and sputtering power is 85W, and self-bias is 400V, and sputtering time is 52 minutes; The thickness that plates out magnesium fluoride film 3 is 650nm; Follow electroplate film 4 at magnesium fluoride film 3; The vacuum tightness of vacuum chamber is 5 * 10
-4Pa, partial pressure of ar gas are 0.6Pa, and sputtering voltage is direct current 297V, and electric current is 0.04A, and the time is 3 minutes and 30 seconds; The thickness of silverskin 4 is 35nm; Last surface gold-plating film 5 at silver-colored film 4; The vacuum tightness of vacuum chamber is 5 * 10
-4Pa, partial pressure of ar gas are 0.6Pa, and sputtering voltage is direct current 297V, and electric current is 0.04A, and the time is 1 minute and 40 seconds; The thickness of gold film 5 is 15nm.
Cedar oil with refractive index and prismatic refraction rate coupling will be bonded together with BK7 prism 1 through the microslide 2 of plated film.
Sensor construction is with embodiment 1.
Preparation process:
Three-layer thin-film on the microslide all adopts the method for magnetron sputtering to be coated with, to guarantee coating quality and accurately to control thickness.At first plate magnesium fluoride film 3 on microslide, the vacuum tightness of vacuum chamber is 5 * 10
-4Pa, partial pressure of ar gas are 0.5Pa, and sputtering voltage is radio frequency 720V (frequency is 13.56MHz), and sputtering current is 0.21A, and sputtering power is 102W, and self-bias is 440V, and sputtering time is 43 minutes; The thickness that plates out magnesium fluoride film 3 is 650nm; Then at the electroplate film 4 of magnesium fluoride film 3, the vacuum tightness of vacuum chamber is 5 * 10
-4Pa, partial pressure of ar gas are 0.6Pa, and sputtering voltage is direct current 310V, and electric current is 0.06A, and the time is 2 minutes and 15 seconds; The thickness of silverskin 4 is 35nm; At the surface gold-plating film 5 of silver-colored film 4, the vacuum tightness of vacuum chamber is 5 * 10 at last
-4Pa, partial pressure of ar gas are 0.6Pa, and sputtering voltage is direct current 310V, and electric current is 0.06A, and the time is 65 seconds; The thickness of gold film 5 is 15nm.
Cedar oil with refractive index and prismatic refraction rate coupling will be bonded together with BK7 prism 1 through the microslide 2 of plated film.
Embodiment 3
Sensor construction is with embodiment 1.
Preparation process:
Three-layer thin-film on the microslide all adopts the method for magnetron sputtering to be coated with, to guarantee coating quality and accurately to control thickness.At first plate magnesium fluoride film 3 on microslide, the vacuum tightness of vacuum chamber is 5 * 10
-4Pa, partial pressure of ar gas are 0.5Pa, and sputtering voltage is radio frequency 750V (frequency is 13.56MHz), and sputtering current is 0.23A, and sputtering power is 117W, and self-bias is 460V, and sputtering time is 38 minutes; The thickness that plates out magnesium fluoride film 3 is 650nm; Follow electroplate film 4 at magnesium fluoride film 3; The vacuum tightness of vacuum chamber is 5 * 10
-4Pa, partial pressure of ar gas are 0.6Pa, and sputtering voltage is direct current 300V, and electric current is 0.05A, and the time is 2 minutes and 45 seconds; The thickness of silverskin 4 is 35nm; At the surface gold-plating film 5 of silver-colored film 4, the vacuum tightness of vacuum chamber is 5 * 10 at last
-4Pa, partial pressure of ar gas are 0.6Pa, and sputtering voltage is direct current 300V, and electric current is 0.05A, and the time is 1 minute and 20 seconds; The thickness of gold film 5 is 15nm.
Cedar oil with refractive index and prismatic refraction rate coupling will be bonded together with BK7 prism 1 through the microslide 2 of plated film.
Consult Fig. 2, this figure is an incident P polarized light when being He-Ne laser (wavelength is 632.8nm), the reflected light spectrogram of sensor of the present invention when testing sample is water.
Claims (2)
1. a long-range surface plasma resonance sensor is characterized in that this sensor is to be matrix and to constitute by cedar oil stickup microslide that with the BK7 prism outside surface of described microslide is coated with magnesium fluoride film, silverskin and golden film successively on matrix.
2. the preparation method of the described sensor of claim 1 is characterized in that this method comprises following concrete steps:
A, to select the BK7 prism for use be described sensor base;
B, selection and the identical microslide of BK7 prism material, the size of microslide is slightly less than the bottom surface of BK7 prism;
C, to the microslide plated film
I) ground floor magnesium fluoride film
Adopt magnetron sputtering method that microslide is plated magnesium fluoride film, the vacuum tightness of vacuum chamber is 5 * 10
-4Pa, partial pressure of ar gas are 0.5Pa, and sputtering voltage is radio frequency 700～750V, and frequency is 13.56MHz, and sputtering current is 0.18～0.23A, and sputtering power is 85～117W, and self-bias is 400～440V, and sputtering time is 38～52 minutes; The thickness of magnesium fluoride film is 650nm;
Ii) second layer silver film
Adopt magnetron sputtering method to the microslide silver plating film, the vacuum tightness of vacuum chamber is 5 * 10
-4Pa, partial pressure of ar gas are 0.6Pa, and sputtering voltage is direct current 297～310V, and electric current is 0.04～0.06A, and the time is 2 minutes 15 seconds～3 minutes and 30 seconds; The thickness of silverskin is 35nm;
Iii) the 3rd layer of gold thin film
Adopt magnetron sputtering method to the microslide gold coated films, the vacuum tightness of vacuum chamber is 5 * 10
-4Pa, partial pressure of ar gas are 0.6Pa, and sputtering voltage is direct current 297～310V, and electric current is 0.04～0.06A, and the time is 1 minute 5 seconds～1 minute and 40 seconds; The gold film thickness is 15nm;
D, will be bonded together through the microslide and the BK7 prism of plated film with cedar oil; Wherein: the refractive index of cedar oil and prismatic refraction rate coupling.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102183507A (en) * | 2011-03-01 | 2011-09-14 | 吉林大学 | Method for exciting surface-enhanced Raman spectroscopy (SERS) through long range surface plasmon |
| CN102279175A (en) * | 2011-06-28 | 2011-12-14 | 吉林大学 | Device for directionally emitting enhanced Raman spectrums by utilizing surface plasmas |
| CN103460021A (en) * | 2011-03-28 | 2013-12-18 | 日东电工株式会社 | SPR sensor cell, and SPR sensor |
| CN104020140A (en) * | 2014-06-05 | 2014-09-03 | 大连理工大学 | Dual-channel self-compensation optical fiber surface plasma resonance biochemical sensor |
| CN104089931A (en) * | 2014-06-13 | 2014-10-08 | 电子科技大学 | High sensitivity refractive index sensor based on medium magneto-optic surface plasma resonance |
| CN104502279A (en) * | 2014-12-19 | 2015-04-08 | 中国计量学院 | Long-range surface plasma resonance device based on tilted fiber bragg grating |
| CN104697961A (en) * | 2014-12-15 | 2015-06-10 | 天津科技大学 | Long-range surface plasma resonance sensor and preparation method thereof |
| CN105074431A (en) * | 2013-03-22 | 2015-11-18 | 日东电工株式会社 | Surface plasmon resonance sensor cell and surface plasmon resonance sensor |
| CN107356996A (en) * | 2017-07-31 | 2017-11-17 | 杭州晶百检测技术有限公司 | A kind of prism for SPR detectors and preparation method thereof |
| CN108279454A (en) * | 2018-02-12 | 2018-07-13 | 林式 | The gold-plated prism assemblies of disposable SPR detections |
| CN109164068A (en) * | 2018-09-13 | 2019-01-08 | 东北大学 | A kind of symmetrical expression long-distance surface plasmon resonance sensor |
| CN109709068A (en) * | 2018-03-07 | 2019-05-03 | 长沙学院 | Tune long-range SPR device and the method using the units test refractive index |
| CN109709047A (en) * | 2018-03-07 | 2019-05-03 | 长沙学院 | A kind of bimetallic long-range surface plasmon resonance sensor and preparation method thereof |
| CN110057782A (en) * | 2019-04-24 | 2019-07-26 | 电子科技大学 | The adjustable penetration depth biosensor of near-infrared and method of memristor reconstruct |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102183507B (en) * | 2011-03-01 | 2012-11-21 | 吉林大学 | Method for exciting surface-enhanced Raman spectroscopy (SERS) through long range surface plasmon |
| CN102183507A (en) * | 2011-03-01 | 2011-09-14 | 吉林大学 | Method for exciting surface-enhanced Raman spectroscopy (SERS) through long range surface plasmon |
| CN103460021A (en) * | 2011-03-28 | 2013-12-18 | 日东电工株式会社 | SPR sensor cell, and SPR sensor |
| CN102279175A (en) * | 2011-06-28 | 2011-12-14 | 吉林大学 | Device for directionally emitting enhanced Raman spectrums by utilizing surface plasmas |
| CN105074431A (en) * | 2013-03-22 | 2015-11-18 | 日东电工株式会社 | Surface plasmon resonance sensor cell and surface plasmon resonance sensor |
| US9632027B2 (en) | 2013-03-22 | 2017-04-25 | Nitto Denko Corporation | Surface plasmon resonance sensor cell and surface plasmon resonance sensor |
| CN104020140A (en) * | 2014-06-05 | 2014-09-03 | 大连理工大学 | Dual-channel self-compensation optical fiber surface plasma resonance biochemical sensor |
| CN104089931A (en) * | 2014-06-13 | 2014-10-08 | 电子科技大学 | High sensitivity refractive index sensor based on medium magneto-optic surface plasma resonance |
| CN104697961A (en) * | 2014-12-15 | 2015-06-10 | 天津科技大学 | Long-range surface plasma resonance sensor and preparation method thereof |
| CN104502279A (en) * | 2014-12-19 | 2015-04-08 | 中国计量学院 | Long-range surface plasma resonance device based on tilted fiber bragg grating |
| CN107356996A (en) * | 2017-07-31 | 2017-11-17 | 杭州晶百检测技术有限公司 | A kind of prism for SPR detectors and preparation method thereof |
| CN108279454A (en) * | 2018-02-12 | 2018-07-13 | 林式 | The gold-plated prism assemblies of disposable SPR detections |
| CN109709068A (en) * | 2018-03-07 | 2019-05-03 | 长沙学院 | Tune long-range SPR device and the method using the units test refractive index |
| CN109709047A (en) * | 2018-03-07 | 2019-05-03 | 长沙学院 | A kind of bimetallic long-range surface plasmon resonance sensor and preparation method thereof |
| CN109164068A (en) * | 2018-09-13 | 2019-01-08 | 东北大学 | A kind of symmetrical expression long-distance surface plasmon resonance sensor |
| CN110057782A (en) * | 2019-04-24 | 2019-07-26 | 电子科技大学 | The adjustable penetration depth biosensor of near-infrared and method of memristor reconstruct |
| CN110057782B (en) * | 2019-04-24 | 2021-09-21 | 电子科技大学 | Near-infrared adjustable penetration depth biosensor and method based on memristor reconstruction |
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