CN110095200B - Thermosensitive sensor based on spin cross complex and preparation method thereof - Google Patents
Thermosensitive sensor based on spin cross complex and preparation method thereof Download PDFInfo
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Abstract
The invention provides a thermosensitive sensor based on a spin cross complex and a preparation method thereof, belonging to the technical field of semiconductors. The invention relates to a thermosensitive sensor based on a spin cross complex, which comprises [ Fe (Htrz) ]3](CF3SO3)2Film, for carrying or sandwiching [ Fe (Htrz) ]3](CF3SO3)2Conducting means for the film, the conducting means being for carrying [ Fe (Htrz) ]3](CF3SO3)2Plastic flexible substrate of film or for sandwiching said [ Fe (Htrz) ]3](CF3SO3)2Two metal electrode layers of the film. The present invention utilizes spin-cross complexes [ Fe (Htrz) ]3](CF3SO3)2The resistance of the sensor is changed under the condition of temperature change, and a sensor with high heat sensitivity is prepared. The spin cross complex has unique reversible responsiveness to an external temperature field, and the response is not interfered by other external factors, so that the prepared sensor has the advantages of high sensitivity, high precision, quick thermal response and good repeatability.
Description
Technical Field
The invention belongs to the technical field of semiconductors, and particularly relates to a thermal sensor based on a spin cross complex and a preparation method thereof.
Background
With the trend of miniaturization of conventional silicon-based semiconductor devices approaching the limits of process fabrication and physical properties and the rapid development of nanotechnology in recent years, the moore's law in the chip industry will be at the end. Due to the unique molecular bistable property, the organic electroluminescent material has a very wide application prospect in the field of molecular electronic devices such as novel molecular level information storage, optical switches, thermal switches and the like, and the switching type molecules are greatly concerned by people as soon as the molecular bistable material appears, so that the organic electroluminescent material is expected to replace the traditional inorganic semiconductor material to a certain extent, and a practical and feasible solution is expected to be provided for overcoming the limitation of the moore's law in the future.
As a more typical and widely studied switch-type molecule, spin-cross complexes refer to certain molecules having dn(n = 4-7) the first transition metal ion complex with electronic configuration generates a high spin state under the excitation of a specific external field such as temperature, pressure, illumination, magnetic field and the like5T2g(S =2) and low spin state1A1g(S =0), a phenomenon of mutual transition, i.e. spin transition, also called spin transition. This spin transfer is accompanied by other synergistic effects such as color change, change in dielectric constant, change in conductivity, and large thermal hysteresis, which are the basis of single molecules or molecular aggregates as materials for thermal switches, optical switches, and information storage elements. Therefore, spin-crossbar molecules are an ideal molecular system for developing new types of thermosensitive sensors, photothermal switches, and information storage devices. However, since the phenomenon of spin crossing is discovered, the application of the device has not been a great breakthrough all the time, and the overall research on spin crossing is greatly limited, and the fundamental reason is that it is difficult to prepare a stable, reliable, thickness-controllable molecular thin film with spin transition.
The thermosensitive sensor has the characteristics of good stability, good linearity, short response time, good applicability and the like, has important influence and wide application background in the field of sensors, not only directly influences the basic living conditions of human beings, but also has great influence on the aspects of industry and agriculture, biological products, medical treatment and health, environmental protection industry, power system monitoring, national defense construction, aerospace and the like. The traditional heat-sensitive sensor usually adopts rigid inorganic materials, has poor flexibility, more additional circuit elements, inconvenient later maintenance and higher cost, and is particularly suitable for winding type and film type sensors. In addition, since the conventional thermal sensor generally has a thermal hysteresis effect, sensitivity is limited and accuracy is difficult to be ensured. These disadvantages make it difficult for conventional heat-sensitive sensors to be used in increasingly miniaturized electronic devices, such as wearable electronics, where the sensor and product often need to be integrated to form an integrated system, in addition to the basic performance requirements. In addition, the charging equipment used by people at present often has an overheating condition, and no prompt is given on a mobile phone, so that explosion is caused, and potential safety hazards exist.
Disclosure of Invention
In view of the above, the invention provides a spin cross complex-based thermal sensor and a preparation method thereof, and the spin cross complex sensor has the advantages of high sensitivity, high precision, fast thermal response, good repeatability, good flexibility, simple structure and low cost.
The invention relates to a thermosensitive sensor based on a spin cross complex, which comprises [ Fe (Htrz) ]3](CF3SO3)2Film for supporting or sandwiching said [ Fe (Htrz) ]3](CF3SO3)2Conducting means for the film, said conducting means being for carrying said [ Fe (Htrz) ]3](CF3SO3)2Plastic flexible substrate of film or for sandwiching said [ Fe (Htrz) ]3](CF3SO3)2Two metal electrode layers of the film.
Preferably, the plastic flexible substrate is one or two of polyethylene terephthalate and polyimide.
Preferably, the material of the metal electrode layer is one or more of aluminum, gold, silver, iron, cobalt, nickel and lanthanum strontium manganese oxygen.
Preferably, [ Fe (Htrz) ]3](CF3SO3)2The thickness of the film is 10-1000 nm.
Preferably, [ Fe (Htrz) ]3](CF3SO3)2The film has spin conversion characteristics, and simultaneously has remarkable resistance change, low spin state at low temperature and low resistance state as electric conduction, and high spin state at high temperature and high resistance state as electric conduction.
A method for preparing a spin-cross complex-based thermosensitive sensor as described above, comprising the steps of:
(1) rapidly mixing a trifluoromethanesulfonic acid solution of ferrous trifluoromethanesulfonate with the mass fraction of 1.8-2.2% and a trifluoromethanesulfonic acid solution of 1,2, 4-triazole, and then placing the reacted solution for about 1 half and a half under a steady-state condition to complete crystallization, wherein the concentration of the trifluoromethanesulfonic acid solution is 0.4-1.5 mol/L;
(2) centrifuging, washing and drying the precipitate in the solution to obtain [ Fe (Htrz) ]3](CF3SO3)2Single crystal;
(3) a reaction product of [ Fe (Htrz) ]3](CF3SO3)2The single crystal is prepared into [ Fe (Htrz) ] with mass concentration of 18-22 mg/ml3](CF3SO3)2A solution;
(4) reacting [ Fe (Htrz) ] described in step (2)3](CF3SO3)2The single crystal is made into a thin film on a conducting device by vacuum evaporation so that [ Fe (Htrz) ]3](CF3SO3)2The film is adhered to a plastic flexible substrate or sandwiched between two metal electrode layers.
(5) Reacting [ Fe (Htrz) ] described in step (3)3](CF3SO3)2The solution was made into a thin film on a conducting device by solution spin coating method such that [ Fe (Htrz) ]3](CF3SO3)2The film is adhered to a plastic flexible substrate or sandwiched between two metal electrode layers.
Wherein when [ Fe (Htrz) ]3](CF3SO3)2In the case of single crystal, the specific method of evaporation is: at 4X 10-4 Carrying out thermal evaporation in a Pa vacuum atmosphere, wherein the evaporation rate is 0.1-0.5 nm/s. When using [ Fe (Htrz)3](CF3SO3)2In the case of a solution, the solvent used in the solution spin coating method is propionitrile.
The present invention utilizes spin-cross complexes [ Fe (Htrz) ]3](CF3SO3)2The resistance of the sensor is changed under the condition of temperature change, and a sensor with high heat sensitivity is prepared. The spin cross complex has unique reversible responsiveness to an external temperature field, and the response is not interfered by other external factors, so that the prepared sensor has the advantages of high sensitivity, high precision, quick thermal response, good repeatability, good flexibility, simple structure, low cost, long service life and the like, can be suitable for various miniaturized devices, particularly wearable electronic products, and can also be applied to temperature overheating protection of some small industrial instruments.
Drawings
FIG. 1 shows a thermal sensor based on spin-cross complexes and a method for preparing the same, according to an embodiment of the present invention, [ Fe (Htrz) ]3](CF3SO3)2A graph of the susceptibility of the film as a function of temperature;
FIG. 2 is a schematic structural diagram of a thermal sensor based on a spin-cross complex and a thermal sensor prepared by a preparation method thereof according to an embodiment of the present invention;
FIG. 3 is a schematic structural diagram of another thermosensitive sensor prepared by the method for preparing the thermosensitive sensor based on the spin cross coordination compound;
fig. 4 is a schematic structural diagram of another thermosensitive sensor prepared by the method and based on the spin cross complex.
Detailed Description
Example one
Referring to fig. 1 and 2, a novel flexible self-adhesive thermal sensor may be applied to portable consumer electronics products such as smart phones.
The invention relates to a thermosensitive sensor based on a spin cross complex, which comprises [ Fe (Htrz) ]3](CF3SO3)2Film for supporting the [ Fe (Htrz) ]3](CF3SO3)2A plastic flexible substrate of film, which may be polyethylene terephthalate or polyimideImine, preferably [ Fe (Htrz) ]3](CF3SO3)2The thickness of the film was 10 nm.
Said [ Fe (Htrz)3](CF3SO3)2The film has spin conversion characteristics, and simultaneously has remarkable resistance change, low spin state at low temperature and low resistance state as electric conduction, and high spin state at high temperature and high resistance state as electric conduction.
A method for preparing a spin-cross complex-based thermosensitive sensor as described above, comprising the steps of:
(1) rapidly mixing a trifluoromethanesulfonic acid solution of ferrous trifluoromethanesulfonate with the mass fraction of 1.8% and a trifluoromethanesulfonic acid solution of 1,2, 4-triazole, and then placing the reacted solution for about 1 half and a half under a steady-state condition to complete crystallization, wherein the concentration of the trifluoromethanesulfonic acid solution is 0.4 mol/L;
(2) centrifuging, washing and drying the precipitate in the solution to obtain [ Fe (Htrz) ]3](CF3SO3)2Single crystal;
(3) a reaction product of [ Fe (Htrz) ]3](CF3SO3)2The single crystal is prepared into [ Fe (Htrz) ] with mass concentration of 18-22 mg/ml3](CF3SO3)2A solution;
(4) reacting [ Fe (Htrz) ] described in step (2)3](CF3SO3)2The single crystal is formed into a thin film on a conducting device by vacuum evaporation, or [ Fe (Htrz) ] described in step (3)3](CF3SO3)2The solution was made into a thin film on a conducting device by solution spin coating method such that [ Fe (Htrz) ]3](CF3SO3)2The film is adhered to a plastic flexible substrate.
The specific method of vapor deposition is as follows: at 4X 10-4 Thermal deposition was carried out in a vacuum atmosphere of Pa at a deposition rate of 0.4 nm/s. The solvent used in the solution spin coating method is propionitrile. (the performance of the products prepared within the range of 0.1-0.5 nm/s of the evaporation rate is similar).
[Fe(Htrz)3](CF3SO3)2The film has a temperature-dependent spin transition characteristic, wherein the spin transition temperature is 62 ℃ in the temperature rising direction and 10 ℃ in the temperature lowering direction. Simultaneously, with obvious color and resistance changes, the film is purple at low temperature and light blue at high temperature.
The flexible substrate in this embodiment is a flexible substrate capable of being pasted and can be adhered to an electronic product.
In the charging process, when the product is overshot or heated seriously, the color change is used for reminding a user, and accidents such as battery explosion caused by overheating of the device are avoided. The core component of the thermosensitive sensor is a spin cross complex film with the thickness of hundreds of nanometers, and the spin cross complex film grows on a flexible substrate with good thermal conductivity by a vacuum evaporation or solution processing method, as shown in figure 2, the whole flexible sensor has small volume and good flexibility, is made into a simple self-adhesive product according to needs, and is directly combined with a shell of portable equipment for use.
When a user uses a portable device such as a mobile phone for a long time or the device is in an overcharged state, the spin cross complex film can generate spin cross transition along with the gradual rise of the temperature of the mobile phone, the spin cross complex film is changed from a low spin state to a high spin state, and the color of the sensor is changed from purple to light blue, so that the aim of reminding the user of paying attention is fulfilled.
Example two
The invention relates to a thermosensitive sensor based on a spin cross complex, which comprises [ Fe (Htrz) ]3](CF3SO3)2Film for sandwiching [ Fe (Htrz) ]3](CF3SO3)2Two metal electrode layers of thin film forming a sandwich structure [ Fe (Htrz) ]3](CF3SO3)2The film is sandwiched by the electrodes, the metal electrode layer is made of aluminum, and the products made of the metal electrode layer gold and silver are similar to those in the embodiment.
Said [ Fe (Htrz)3](CF3SO3)2The thickness of the film was 1000 nm. Said [ Fe (Htrz)3](CF3SO3)2The film has spin conversion characteristics, and simultaneously has remarkable resistance change, low spin state at low temperature and low resistance state as electric conduction, and high spin state at high temperature and high resistance state as electric conduction.
A method for preparing a spin-cross complex-based thermosensitive sensor as described above, comprising the steps of:
(1) mixing a trifluoromethanesulfonic acid solution of ferrous trifluoromethanesulfonate with the mass fraction of 2.2% and a trifluoromethanesulfonic acid solution of 1,2, 4-triazole, and then placing the reacted solution for 1 half month to complete crystallization, wherein the concentration of the trifluoromethanesulfonic acid solution is 1.5 mol/L;
(2) centrifuging, washing and drying the precipitate in the solution to obtain [ Fe (Htrz) ]3](CF3SO3)2Single crystal;
(3) reacting [ Fe (Htrz) ] described in step (2)3](CF3SO3)2The single crystal is made into a thin film on a conducting device by vacuum evaporation so that [ Fe (Htrz) ]3](CF3SO3)2The film is sandwiched between two metal electrode layers.
The prepared product is a novel intelligent thermosensitive sensor and can be applied to portable consumer electronics products such as smart phones.
The thermosensitive sensor consists of a spin cross complex film and an upper layer of film electrode and a lower layer of film electrode, wherein the metal electrode is a non-magnetic electrode, such as aluminum, gold, silver and the like, to form a diode with a sandwich structure, as shown in figure 3, each functional layer film is realized by a vacuum evaporation or solution processing method, and the thickness is dozens to hundreds of nanometers.
When a user uses a portable device such as a mobile phone or the like for a long time or the device is in an overcharged state, on one hand, as the temperature of the mobile phone gradually rises, the device can overheat, the electronic structure of the spin cross complex film is changed from a low spin state to a high spin state, and simultaneously, the color of the film is changed from purple to light blue, so that the effect of warning the user is achieved. On the other hand, since the resistance of the spin-crossed thin film also changes with spin transition, the resistance is small in the low spin state, the device resistance is significantly large in the high spin state, and the thin film is in the high resistance state in the overheat state, thereby being capable of automatically stopping charging in time.
EXAMPLE III
The invention relates to a thermosensitive sensor based on a spin cross complex, which comprises [ Fe (Htrz) ]3](CF3SO3)2Film for sandwiching [ Fe (Htrz) ]3](CF3SO3)2Conducting means for the thin film for sandwiching said [ Fe (Htrz) ]3](CF3SO3)2The performance of the product prepared by two metal electrode layers of the film, wherein the metal electrode layer is made of iron, and the metal electrode layers are made of cobalt, nickel and lanthanum strontium manganese oxygen is similar to that of the product prepared by the embodiment.
Said [ Fe (Htrz)3](CF3SO3)2The thickness of the film was 500 nm.
Said [ Fe (Htrz)3](CF3SO3)2The film has spin conversion characteristics, and simultaneously has remarkable resistance change, low spin state at low temperature and low resistance state as electric conduction, and high spin state at high temperature and high resistance state as electric conduction.
A method for preparing a spin-cross complex-based thermosensitive sensor as described above, comprising the steps of:
(1) rapidly mixing 2.0 mass percent of a trifluoromethanesulfonic acid solution of ferrous trifluoromethanesulfonate and 1,2, 4-triazole, and then placing the reacted solution for about 1 half and a half under a steady-state condition to complete crystallization, wherein the concentration of the trifluoromethanesulfonic acid solution is 1.0 mol/L;
(2) centrifuging the precipitate in the solution, separating, washing, oven drying to obtain [ Fe (Htrz) ]3](CF3SO3)2Single crystal;
(3) reacting [ Fe (Htrz) ] described in step (2)3](CF3SO3)2Single crystal production by vacuum evaporation on a conducting deviceForming a film such that [ Fe (Htrz)3](CF3SO3)2The film is adhered to the plastic and sandwiched between two metal electrode layers.
The thermosensitive sensor prepared in the embodiment can be applied to portable consumer electronics products such as smart phones.
As shown in fig. 4, the thermal sensor is connected to an electronic product and a power supply, and the thermal sensor is composed of a spin cross complex film and upper and lower film electrodes, wherein the metal electrodes are ferromagnetic electrodes, such as fe, co, ni, etc., to form an organic spin valve device, and the spin valve functions as the minimum resistance when the spin cross film in the middle is in accordance with the spin orientations of the two ferromagnetic electrodes, and the maximum resistance when the spin orientations are opposite. The functional layer films are realized by a vacuum evaporation method or a solution processing method, and the thickness is dozens to hundreds of nanometers.
When a user uses a portable device such as a mobile phone or the like for a long time or the device is in an overcharged state, on one hand, as the temperature of the mobile phone gradually rises, the device can overheat, the electronic structure of the spin cross complex film is changed from a low spin state to a high spin state, and simultaneously, the color of the film is changed from purple to light blue, so that the effect of warning the user is achieved. On the other hand, when the spin-cross coordination compound is converted into a high spin state, the electron spin orientation of the spin-cross film is opposite to that of the film electrode, the spin valve is in a high resistance state, current is not easy to pass through, in addition, the resistance of the film is also obviously increased in the high spin state, the whole sensor is in the high resistance state at this moment, and the effect of automatically stopping charging can be timely achieved.
In addition, the general battery products have a short service life at a low temperature, and the battery life is also short. When the spin cross coordination compound is used in combination with an intelligent thermosensitive sensor, in a cold environment, the spin cross coordination compound is in a low spin state, so that on one hand, the resistance of the spin cross coordination compound is reduced, on the other hand, the electron spin orientation of the spin cross film is consistent with the electron spin orientation of the film electrode, the spin valve is in a low resistance state, the circuit is conducted, and the charge can be provided for portable equipment, so that the spin cross coordination compound can be used in emergency situations.
The present invention utilizes spin-cross complexes [ Fe (Htrz) ]3](CF3SO3)2The resistance of the sensor is changed under the condition of temperature change, and a sensor with high heat sensitivity is prepared. The spin cross complex has unique reversible responsiveness to an external temperature field, and the response is not interfered by other external factors, so that the prepared sensor has the advantages of high sensitivity, high precision, quick thermal response, good repeatability, good flexibility, simple structure, low cost, long service life and the like, can be suitable for various miniaturized devices, particularly wearable electronic products, and can also be applied to temperature overheating protection of some small industrial instruments.
The present invention is not limited to the above-described specific embodiments, and various modifications and variations are possible. Any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention should be included in the scope of the present invention.
Claims (9)
1. A thermal sensor based on spin cross complex is characterized by comprising [ Fe (Htrz) ]3](CF3SO3)2Film for supporting or sandwiching said [ Fe (Htrz) ]3](CF3SO3)2Conducting means for the film, said conducting means being for carrying said [ Fe (Htrz) ]3](CF3SO3)2Plastic flexible substrate of film or for sandwiching said [ Fe (Htrz) ]3](CF3SO3)2Two metal electrode layers of thin film, [ Fe (Htrz) ]3](CF3SO3)2The thickness of the film is 10-1000 nm; the thermosensitive sensor based on the spin cross complex is prepared by the following steps: (1) mixing a trifluoromethanesulfonic acid solution of ferrous trifluoromethanesulfonate and a trifluoromethanesulfonic acid solution of 1,2, 4-triazole, and then placing the reacted solution until crystallization is completed;
(2) the precipitate in the solution is centrifugally separated, washed and dried,to obtain [ Fe (Htrz) ]3](CF3SO3)2Single crystal;
(3) a reaction product of [ Fe (Htrz) ]3](CF3SO3)2The single crystal is prepared into [ Fe (Htrz) ] with mass concentration of 18-22 mg/ml3](CF3SO3)2A solution;
(4) reacting [ Fe (Htrz) ] described in step (2)3](CF3SO3)2The single crystal is formed into a thin film on a conducting device by vacuum evaporation, or [ Fe (Htrz) ] described in step (3)3](CF3SO3)2The solution was made into a thin film on a conducting device by solution spin coating method such that [ Fe (Htrz) ]3](CF3SO3)2The film is adhered to a plastic flexible substrate or is mounted between two metal electrode layers.
2. The spin-cross complex-based thermosensitive sensor according to claim 1, wherein the plastic flexible substrate is one or both of polyethylene terephthalate and polyimide.
3. The spin-cross complex-based thermal sensor according to claim 2, wherein the metal electrode layer is made of one or more of aluminum, gold, silver, iron, cobalt, nickel, and lanthanum strontium manganese oxide.
4. The spin-cross complex-based thermosensitive sensor according to claim 2, wherein [ Fe (Htrz) ]3](CF3SO3)2The film has spin conversion characteristics, and simultaneously has remarkable resistance change, low spin state at low temperature and low resistance state as electric conduction, and high spin state at high temperature and high resistance state as electric conduction.
5. The spin-cross complex-based thermosensitive sensor according to claim 1, wherein the mass fraction of the ferrous triflate is 1.8-2.2%.
6. The spin-cross complex-based thermosensitive sensor according to claim 1, wherein the concentration of the trifluoromethanesulfonic acid solution is 0.4-1.5 mol/L.
7. The spin-cross complex-based thermosensitive sensor according to claim 1, wherein the specific method of evaporation is: at 4X 10-4 Carrying out thermal evaporation in a Pa vacuum atmosphere, wherein the evaporation rate is 0.1-0.5 nm/s.
8. The spin-cross complex-based thermosensitive sensor according to claim 1, wherein the solvent used in the spin coating process is propionitrile.
9. The application of the heat-sensitive sensor according to any one of claims 1 to 4, wherein the flexible substrate is an adhesive flexible substrate, the heat-sensitive sensor is adhered in an electronic product, and in the charging process, when the product is overshot and generates heat seriously, the heat-sensitive sensor plays a role in reminding a user through color change, so that accidents such as battery explosion and the like caused by overheating of a device are avoided; the thermosensitive sensor is applied to portable charging equipment to protect electric appliances.
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