CN108007599B - Biological non-toxic and degradable high-sensitivity temperature sensing chip and preparation method and application thereof - Google Patents
Biological non-toxic and degradable high-sensitivity temperature sensing chip and preparation method and application thereof Download PDFInfo
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- CN108007599B CN108007599B CN201711204582.5A CN201711204582A CN108007599B CN 108007599 B CN108007599 B CN 108007599B CN 201711204582 A CN201711204582 A CN 201711204582A CN 108007599 B CN108007599 B CN 108007599B
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Abstract
The invention discloses a biological non-toxic and degradable high-sensitivity temperature sensing chip and a preparation method and application thereof. The invention provides a temperature sensing chip, which comprises a chip body; the chip body is filled with conductive liquid; the chip body is made of degradable high polymer materials; the solvent of the conductive liquid is any one of water and alcohol, and the solute is saccharide, high molecular polymer, inorganic salt, acid or inorganic base. Compared with the traditional temperature sensing chip, the temperature sensing chip has the advantages of biological non-toxicity and degradability, no pollution to the environment, no harm to the human body, reduced size and cost, simple structure, convenient operation, high response sensitivity, convenient carrying, low price and batch production.
Description
Technical Field
The invention relates to a biological non-toxic and degradable high-sensitivity temperature sensing chip and a preparation method and application thereof, belonging to the field of temperature sensors.
Background
With the progress of industrial modernization in China and the continuous high-speed growth of electronic information industry, the temperature sensor as a sensor for judging the cold and hot degree of an object accounts for more than 40% of the total demand of the whole sensor. The conventional temperature sensors mainly include a glass sensor using liquid mercury as a sensing element, a thermocouple type temperature sensor using copper as a sensing element, and a thermosensitive type temperature sensor using a semiconductor as a sensing element. The sensors are suitable for various fields due to different temperature measuring ranges, accuracies and sensitivities, for example, the mercury sensor is suitable for measuring the temperature of a human body with higher accuracy and measurement convenience, but the measuring temperature range is too narrow; the thermocouple type temperature sensor is widely applied to atmospheric environment temperature measurement due to the advantages of wide temperature measurement range, firmness, no need of power supply and the like, but the measurement accuracy is low; the thermal sensor is used for various industrial temperature monitoring with high sensitivity, and has large natural error and poor linear relation of temperature and resistance. Meanwhile, the sensors have a series of problems of biotoxicity, poor environmental compatibility of materials, difficult degradation and the like. These problems are not beneficial to building an environment-friendly society in our country and seriously restrict the sustainable development of the society, so the toxicity and degradability of the sensing material are important technical problems to be solved urgently by the temperature sensor.
Disclosure of Invention
The invention aims to provide a biological nontoxic and degradable high-sensitivity temperature sensing chip and a preparation method and application thereof.
The invention provides a temperature sensing chip, which comprises a chip body; the chip body is filled with conductive liquid; the chip body is made of degradable high polymer materials; the solvent of the conductive liquid is any one of water and alcohol, and the solute is saccharide, high molecular polymer, inorganic salt, acid or inorganic base.
In the temperature sensing chip, the degradable polymer material may be a degradable polymer material capable of forming a film, and specifically may be a synthetic degradable polymer material, such as any one of polyvinyl alcohol, polylactic acid, polyethylene glycol, polycaprolactone, and the like.
In the above temperature sensor chip, the alcohol is a liquid alcohol such as polyol, monol, etc., and may have a chemical formula of CH3(CH2)nOH、HO(CH2)nOH、HO(CH2OH)nOH or HO (CH)2)n(CH2OH)nCH3(ii) a Wherein n is any natural number between 0 and 12; the alcohol may be any one of ethanol, propanol, butanol, ethylene glycol, glycerol, erythritol, 1, 2-propanediol, 1, 2-butanediol, and 2, 3-pentanediol.
In the above temperature sensor chip, the saccharide may be common saccharide such as starch, chitosan, glucose, maltose, etc.
In the temperature sensing chip, the high molecular polymer may be a high molecular polymer capable of ionizing ions in the solvent, such as polyacrylic acid, polybutylene acid, polylactic acid, and the like. The molecular weight of the high molecular polymer is 300-100000, such as 4000.
In the above temperature sensor chip, the chemical formula of the inorganic salt, acid or inorganic base may be XnYmWherein X is H, Li, Na, Ka, Mg, Ca, Fe, Cu, Al or NH4(ii) a Y is F, Cl, Br, I, SO4、NO3、CH3COO and OH; n and m are any natural number between 1 and 4. The solute may be sodium chloride, acetic acid, sodium fluoride, calcium chloride, magnesium sulfate, aluminum nitrate, ammonium acetate, sodium hydroxide, etc.
In the temperature sensing chip, the mass concentration of the conductive liquid may be 0.001% to 20%, specifically 11%.
In the temperature sensing chip, a micro-channel can be arranged in the chip body; two ends of the micro flow channel can be respectively communicated with the outside through an opening formed on the chip body to form an electrode interface; the electrode interface can be connected with an electrode matched with the electrode interface; the micro flow channel may be filled with the conductive liquid.
The depth of the micro-channel is 1-1000 microns, the width is 1-1000 microns, and the length is 0.01-10 cm; the thickness of the chip body is 2-2000 microns.
The invention further provides a preparation method of the temperature sensing chip, which comprises the following steps: and packaging the conductive liquid in a shell made of the degradable high polymer material to obtain the temperature sensing chip.
In the above method, the specific steps of encapsulating the conductive liquid in the shell made of the degradable polymer material are as follows:
(1) making the degradable high polymer material into an upper-layer cover plate and a lower-layer gasket by using a mould; one surface of the upper cover plate is provided with a groove, and two ends of the upper cover plate, which are positioned in the groove, are respectively provided with the openings;
(2) and injecting the conductive liquid into the groove, then attaching the lower gasket to one surface, provided with the groove, of the upper cover plate, wherein the groove forms a micro-channel, the opening forms an electrode interface, and an electrode is connected to the electrode interface to obtain the temperature sensing chip.
In the step (1), the mold of the upper cover plate can be a glass sheet provided with a convex groove and can be prepared by adopting a photoetching method. The mold of the lower gasket layer can be a glass sheet with a smooth surface. The preparation steps of the upper cover plate or the lower gasket are as follows: and pressing the melted high polymer material on the die to obtain the upper cover plate or the lower gasket.
In the step (2), the attaching step is as follows: and (3) tightly attaching the lower gasket to the surface, provided with the micro-channel, of the upper cover plate, and performing hot pressing. The hot pressing temperature can be 60-100 ℃, such as 70 ℃; the time may be 1 to 3 minutes, such as 1 minute.
The invention also provides application of the temperature sensing chip in preparation of a temperature sensor, biological body temperature measurement or industrial temperature monitoring.
The invention has the following beneficial effects:
the temperature sensing chip of the invention has the advantages that the conductivity of the conductive liquid is greatly influenced by the temperature, the obvious response signal can be generated only by the temperature difference of one degree centigrade, the shell is very thin, and the heat conduction is completed in a very short time, so when the external temperature is changed and transmitted to the chip body, the conductivity of the conductive liquid stored in the chip body is changed along with the temperature, and the change can be rapidly detected by electrochemical equipment.
The solvent in the conductive liquid used by the invention is water, alcohol, ester and other liquids, and the solution formed by doping the liquids and different types of salts has good conductive capability, and the conductive performance changes along with the change of temperature. The sensitivity of resistance values of solutions consisting of different solvents and solutes to temperature response is different, and the magnitude of the sensitivity is related to the viscosity change rate of the solute; meanwhile, different types of solvents have different melting points, so that the solvents can be selected according to the requirements of the measurement environment. Therefore, the liquid such as water, alcohol, ester and the like is used as a novel temperature sensing element to prepare the temperature sensor, and the sensing chip has the advantages of being non-toxic and degradable, and has the characteristics of wide temperature measurement range, high sensitivity, batch preparation and the like. Therefore, the sensing element has wide application prospect in the fields of biological body temperature measurement, industrial temperature monitoring and the like.
Compared with the traditional temperature sensing chip, the temperature sensing chip has the advantages of biological non-toxicity and degradability, no pollution to the environment, no harm to the human body, reduced size and cost, simple structure, convenient operation, high response sensitivity, convenient carrying, low price and batch production.
Drawings
Fig. 1 is a schematic structural diagram of a temperature sensing chip according to the present invention.
FIG. 2 is a flow chart of the present invention for preparing a temperature sensing chip.
Fig. 3 is a graph showing the response of a temperature sensing chip to temperature using a glycol solution of calcium chloride as a conductive liquid.
Fig. 4 is a response diagram of temperature sensing chips with different concentrations of sodium chloride aqueous solution as conductive liquid to different test temperatures.
FIG. 5 is a graph showing the response of temperature sensing chips with different concentrations of starch aqueous solution as conductive liquid to different test temperatures.
Fig. 6 is a graph showing the response of the temperature sensing chip with different concentrations of acid (acetic acid, polyacrylic acid) aqueous solution as the conductive liquid to different test temperatures.
Fig. 7 is a graph showing the response of the temperature sensing chip with different concentrations of calcium chloride in glycol solution as the conductive liquid to different test temperatures.
FIG. 8 is a graph of the response of a temperature sensing chip with magnesium chloride solutions in different solvents as a conductive liquid to different test temperatures.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
EXAMPLE 1 preparation of conductive liquid temperature sensing chip and response to temperature
Structure of conductive liquid temperature sensing chip
As shown in FIG. 1, the temperature sensing chip of the invention comprises a chip body made of degradable high molecular materials such as polyvinyl alcohol, polylactic acid, polyethylene glycol or polycaprolactone, wherein the thickness of the chip body is 2-200 microns; a micro channel with the depth of 1-1000 microns, the width of 1-1000 microns and the length of 0.01-10 cm is arranged in the chip body; two ends of the micro-channel are communicated with the outside through an opening formed on the chip body to form an electrode interface; the electrode interface is connected with an electrode matched with the electrode interface; the micro flow channel is filled with conductive liquid, and the solvent of the conductive liquid is any one of water and alcohol; the alcohol has the formula CH3(CH2)nOH、HO(CH2)nOH、HO(CH2OH)nOH or HO (CH)2)n(CH2OH)nCH3(ii) a Wherein n is any natural number between 0 and 12; the chemical formula of the solute is XnYmWherein X is H, Li, Na, Ka, Mg, Ca, Fe, Cu, Al or NH4(ii) a Y is F, Cl, Br, I, SO4、NO3、CH3COO and OH; n and m are any natural number between 1 and 4; the mass concentration of solute in the conductive liquid is 0.001-10%.
Preparation of conductive liquid temperature sensing chip
The temperature sensing chip is prepared according to the flow chart shown in fig. 2, and the specific steps are as follows:
(1) preparation of a degradable high polymer material film (upper cover sheet) with micro-channels:
A. preparing a mould: a convex groove with a pattern is carved on a glass sheet with the thickness of 3cm multiplied by 3cm by an ultraviolet photoetching machine to obtain a mould;
B. preparing an upper cover sheet: the glass sheet is placed on a 160-DEG C hot table to be heated, 0.3g of degradable high polymer material polylactic acid (molecular weight is 4000) is placed in the glass sheet to be melted, and another flat glass sheet is used as a high polymer material to form a thin film with one flat surface and one groove pattern, namely an upper cover plate with the thickness of 400 microns and one micro-channel.
C. Opening: openings are respectively arranged at the two ends of the upper layer cover plate, which are positioned on the micro-channel.
(2) Adding conductive liquid and packaging the chip:
A. adding a conductive liquid: sucking the conductive liquid by an injector, and injecting the conductive liquid into the micro-channel in the upper cover plate with the micro-channel to form a temperature measuring source;
B. preparing a lower-layer gasket: placing the high polymer material polylactic acid with the same weight in the step (1) into two flat glass sheets, and pressing the glass sheets into films with the same specification at 100 ℃ to obtain a lower-layer gasket;
C. packaging: the lower gasket is closely attached to one surface, provided with the micro-channel, of the upper gasket filled with the conductive liquid, and then the lower gasket is extruded at 70 ℃ for 1 minute to be closely attached, and the conductive liquid is arranged in a groove of one side film between the two films; the opening arranged on the upper surface forms an electrode interface; an iron electrode is inserted at the electrode interface and in contact with the conducting liquid at the same temperature.
The thickness of the chip body in the prepared temperature sensing chip is 800 microns; the depth of the microchannel was 200 microns, the width was 800 microns, and the length was 4 cm.
Response of conductive liquid temperature sensing chip to temperature
The electrode of the temperature sensing chip prepared in the above way is connected to an electrochemical workstation (model: CHI660E, Shanghai Chenghua instruments, Ltd.), the testing method adopts a current-time curve method, the output voltage is set to be constant at 1.0V, the temperature sensing chip is subjected to constant potential scanning, the obtained current-time curve is only related to the resistance change of the chip, and the specific experimental process and results are as follows:
a constant temperature heating table (model: BP-2B, Nannocechnology Co., Ltd., Chuang, Beijing) is selected as a constant temperature testing device, the temperature can be set to be any value between 30 ℃ and 65 ℃, and the room temperature is controlled to be constant at 25 ℃.
1) Adjusting the temperature of the constant temperature heating table to be 45 ℃, connecting the electrode wire of the temperature sensing chip to an electrochemical workstation, scanning the chip at constant potential, setting the voltage to be 1.0V, and recording the currentTime profile, observing the variation of the current with the temperature variation, setting a heating temperature for a time of 2min and a cooling time of 2min for 8 cycles, wherein the response value (Δ G/G)0) Depends on a set formula: delta G/G0＝[1-I/I0]X 100%, where I represents the real-time current, and I0Indicating the initial current at the time of initial testing.
The experimental results are shown in fig. 3, the conductive liquid used is a glycol solution of calcium chloride (11% by mass concentration), and it can be seen from fig. 3 that the response value of each cycle is substantially consistent in 14 cycles, that is, the response value of each cycle is about 80% at a temperature difference of 20K.
2) And connecting an electrode connecting wire of the temperature sensing chip to an electrochemical workstation, carrying out constant potential scanning on the chip, setting the voltage to be 1.0V, recording a current-time curve, observing the change of the current along with the temperature change, setting the heating temperature time to be 2min, and setting the cooling time to be 2 min. Wherein the heating temperature is sequentially increased from 30 ℃ to 60 ℃ so that the temperature difference values are 5 ℃, 10 ℃, 15 ℃, 20 ℃, 25 ℃, 30 ℃ and 35 ℃ in sequence.
FIG. 4 is a graph showing the response of temperature sensing chips with different concentrations of aqueous solutions of sodium chloride (0.01g/mL, 0.02g/mL, 0.05g/mL, 0.10g/mL) as conductive liquids to different test temperatures, and it can be seen from FIG. 4 that the response of temperature sensing chips with aqueous solutions of sodium chloride with mass concentrations ranging from 0.01 to 0.10g/mL as conductive liquids to temperature has higher sensitivity.
FIG. 5 is a corresponding graph of temperature sensor chips with starch aqueous solutions of different concentrations as conductive liquids (0.01g/mL, 0.02g/mL, 0.04g/mL, 0.08g/mL) at different test temperatures, and it can be seen from FIG. 5 that the temperature sensor chips with starch aqueous solutions of mass concentrations in the range of 0.01-0.0.08 g/mL as conductive liquids all have higher sensitivity to temperature responses.
Fig. 6 is a corresponding graph of temperature sensing chips of acid (1.0%, 2.5%, 5.0% acetic acid, 1.2%, 3.0/6.0% polyacrylic acid) aqueous solutions with different concentrations for different test temperatures, and it can be seen from fig. 6 that the temperature sensing chips using the aqueous solution of acetic acid with a mass percentage in the range of 1.0-5.0% or polyacrylic acid with a mass percentage in the range of 1.2-6.0% as the conductive liquid have higher sensitivity to the temperature.
FIG. 7 is a corresponding graph of temperature sensing chips of ethylene glycol solutions (0.1mmol/L, 0.2mmol/L, 0.3mmol/L) of calcium chloride with different concentrations for different test temperatures, and it can be seen from FIG. 7 that the temperature sensing chips of the ethylene glycol solutions of calcium chloride with mass percentage content in the range of 0.1-0.3 mmol/L as conductive liquid all have higher sensitivity to temperature response.
FIG. 8 is a graph showing the response of magnesium chloride solutions (ethylene glycol, 1, 2-propylene glycol, 1, 2-butylene glycol, and 2, 3-pentanediol, respectively) with concentration of 0.01mmol/L in different solvents to different test temperatures, and it can be seen from FIG. 8 that the temperature sensing chips, in which the chloridase solutions (ethylene glycol, 1, 2-propylene glycol, 1, 2-butylene glycol, and 2, 3-pentanediol, respectively) with solvents are used as conductive liquids, all have high sensitivity to the temperature.
From the graph of FIG. 4 to FIG. 8, the response value Δ G/G is between 30 ℃ and 60 ℃0The temperature difference rises along with the rise of the temperature difference, and the temperature difference increases regularly. Wherein the response value Δ G/G0The relation equation with the temperature difference delta T is as shown in formula (1):
in the formula (1), A, B and C are constants.
Claims (7)
1. A temperature sensing chip, characterized by: it comprises a chip body; the chip body is filled with conductive liquid; the chip body is made of degradable high polymer materials; the solvent of the conductive liquid is alcohol;
the alcohol is any one of ethylene glycol, glycerol, erythritol, 1, 2-propanediol, 1, 2-butanediol and 2, 3-pentanediol;
the solute in the conductive liquid is calcium chloride and/or magnesium chloride;
the mass concentration of solute in the conductive liquid is 0.001% -10%;
a micro-channel is arranged in the chip body; two ends of the micro flow channel are communicated with the outside through openings formed in the chip body to form electrode interfaces; the electrode interface is connected with an electrode matched with the electrode interface; the micro flow channel is filled with the conductive liquid.
2. The temperature sensing chip of claim 1, wherein: the degradable high polymer material is a degradable high polymer material capable of forming a film.
3. The temperature sensing chip of claim 1, wherein: the degradable high polymer material is a synthetic degradable high polymer material.
4. The temperature sensing chip of claim 1, wherein: the degradable high polymer material is any one of polyvinyl alcohol, polylactic acid, polyethylene glycol and polycaprolactone.
5. The temperature sensing chip of claim 1, wherein: the depth of the micro-channel is 1-1000 microns, the width is 1-1000 microns, and the length is 0.01-10 cm; the thickness of the chip body is 2-2000 microns.
6. The method for manufacturing a temperature sensing chip according to any one of claims 1 to 5, comprising the steps of: encapsulating the conductive liquid in a shell made of the degradable high polymer material to obtain the temperature sensing chip;
the steps of encapsulating the conductive liquid in the shell made of the degradable high polymer material are as follows:
(1) making the degradable high polymer material into an upper-layer cover plate and a lower-layer gasket by using a mould; one surface of the upper cover plate is provided with a groove, and two ends of the upper cover plate, which are positioned in the groove, are respectively provided with the openings;
(2) and injecting the conductive liquid into the groove, then attaching the lower gasket to one surface, provided with the groove, of the upper cover plate, wherein the groove forms a micro-channel, the opening forms an electrode interface, and an electrode is connected to the electrode interface to obtain the temperature sensing chip.
7. Use of the temperature sensing chip of any one of claims 1-5 in the manufacture of a temperature sensor, in biological thermometry, or in industrial temperature monitoring.
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