CN114136203B - Preparation method of flexible strain sensor with high sensitivity and good cycling stability - Google Patents

Preparation method of flexible strain sensor with high sensitivity and good cycling stability Download PDF

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CN114136203B
CN114136203B CN202111338988.9A CN202111338988A CN114136203B CN 114136203 B CN114136203 B CN 114136203B CN 202111338988 A CN202111338988 A CN 202111338988A CN 114136203 B CN114136203 B CN 114136203B
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flexible
strain
strain sensor
high sensitivity
film
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CN114136203A (en
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张广平
吴绪苹
罗雪梅
宋竹满
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Institute of Metal Research of CAS
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
    • G01B7/16—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
    • G01B7/18—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge using change in resistance
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/20—Metallic material, boron or silicon on organic substrates
    • C23C14/205—Metallic material, boron or silicon on organic substrates by cathodic sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Measurement Of Length, Angles, Or The Like Using Electric Or Magnetic Means (AREA)

Abstract

The invention discloses a preparation method of a flexible strain sensor with high sensitivity and good cycling stability, and belongs to the technical field of strain electric measurement and sensors. The method comprises three steps: sputtering a layer of metal film on a flexible substrate, carrying out fatigue loading on the film to generate fatigue cracks on the surface of the film, and connecting electric leads at two ends of the film. The flexible strain sensor with high sensitivity and high cycling stability can be prepared by the method. The strain sensor prepared by the invention has high sensitivity factors of more than ten powers, can accurately sense extremely tiny strain (less than 1.5 percent of strain), has excellent cycle stability, realizes the combination of two key performances of the flexible strain sensor, has the advantages of easy preparation, convenient performance regulation and control and the like, and provides a new idea for the development of a strain detection technology in a flexible electronic device.

Description

Preparation method of flexible strain sensor with high sensitivity and good cycling stability
Technical Field
The invention relates to the technical field of strain electric measurement and sensors, in particular to a preparation method of a flexible strain sensor with high sensitivity and good cycling stability.
Background
In recent years, flexible electronic technology is rapidly developed, and flexible electronic devices have wide application prospects in the fields of medical health monitoring, electronic simulation skin, human-computer interaction interfaces and the like. The flexible strain sensor is a flexible device for strain sensing, and is very important for the development of flexible electronic technology, and related scientific researches are endlessly developed in recent years. Sensitivity and cyclic stability are two very important performance indexes of the flexible strain sensor. For resistive strain sensors, sensitivity is usually expressed in terms of the relative change in resistance per unit strain, also known as the GF value, and cyclic stability is measured in terms of the number of cycles it takes to maintain a stable response during dynamic cyclic strain sensing. The traditional strain sensor has low sensitivity, mostly belongs to rigid devices, and cannot be applied to flexible devices. Most of the high-sensitivity flexible strain sensors developed in recent years are difficult to achieve good comprehensive performance, irreversible damage can occur after low cycle sensing, and the cycle stability is poor. Therefore, there is a need to develop new techniques for preparing flexible strain sensors with both high sensitivity and high cycling stability.
Disclosure of Invention
Aiming at the characteristic that the high sensitivity and the high cycling stability of the flexible strain sensor are difficult to combine, the invention aims to provide the preparation method of the flexible strain sensor with high sensitivity and good cycling stability.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a flexible strain sensor with high sensitivity and good cycling stability comprises the following steps:
(1) Cutting the flexible substrate into a rectangle with a proper size, and depositing one or more layers of metal films on the flexible substrate;
(2) Adopting a mechanical testing machine to carry out pulling-pulling fatigue loading on the flexible substrate deposited with the metal film in the step (1) in the length direction (also the strain sensing direction of a final device) at a certain strain amplitude and frequency, and unloading after a certain period of time to form transverse fatigue cracks with a certain density on the surface of the film;
(3) And (3) connecting electric leads at two ends of the flexible substrate metal film with the fatigue cracks obtained in the step (2) by using a conductive adhesive, so as to obtain the flexible strain sensor with high sensitivity and good cycle stability.
In the step (1), the metal film is deposited by a magnetron sputtering method, and the metal film can be a continuous compact state, a loose porous state, a plastic film with strong deformability, or a brittle film with poor deformability.
In the process of carrying out the pulling-pulling fatigue loading in the step (2), a sine loading mode is adopted, the maximum value and the minimum value of the load are respectively 10-25N and 1.0-3.0N, the loading frequency is 25-35Hz, and the loading frequency is more than 1000 weeks.
The flexible strain sensor has high sensitivity in the strain range of less than 1.5 percent, and the sensitivity factor can reach 10 3 The above.
The flexible strain sensor is performing cyclic strain sensing 10 4 After more than one week, the resistance strain response can still maintain a stable level.
The sensing performance of the flexible strain sensor can be adjusted by adjusting the strain amplitude and the loading frequency during fatigue loading in the preparation process or adjusting the mechanical property and the micro-morphology of the metal film.
The invention has the following advantages:
1. the flexible strain sensor prepared by the invention has high sensitivity in a small strain range, and the sensitivity factor can reach 10 3 In the above, the strain sensor can be used for accurately sensing micro strain (strain less than 1.5%) in a flexible electronic device, and the strain sensor preparation technology widely used at present cannot achieve such high sensitivity.
2. The flexible strain sensor prepared by the invention has excellent cycling stability, and can perform cycling strain sensing 10 4 After more than a week, the resistance strain response can still maintain a stable level, a good dynamic resistance response effect is shown, and the characteristics of high sensitivity and high cycle stability enable the strain sensor to have a good application prospect.
3. The flexible strain sensor prepared by the invention can adjust the sensing performance by adjusting the strain amplitude and the loading frequency during fatigue loading or adjusting the mechanical property and the micro-morphology of the metal film, and can be customized to the performance of a device according to the use requirement in practical application.
4. The flexible substrate used in the process of preparing the flexible strain sensor with high sensitivity and good cycling stability has a wider selection range, and can be selected in a targeted manner according to the difference of application scenes of devices.
Drawings
FIG. 1 is a schematic diagram of a process for manufacturing a flexible strain sensor with high sensitivity and good cycling stability according to the present invention.
FIG. 2 is a surface topography map of the fatigue cracked gold film obtained in step 2 of example 1.
Fig. 3 is a strain sensing test curve of the flexible strain sensor prepared in example 1, which has high sensitivity and good cyclic stability.
Fig. 4 is a test curve and a partial enlarged view of the cycling stability of the flexible strain sensor with high sensitivity and good cycling stability prepared in example 1.
Fig. 5 is a strain sensing test curve of the flexible strain sensor with high sensitivity and good cycling stability prepared in example 2.
Fig. 6 is a cycle stability test curve and a partial enlarged view of the flexible strain sensor with high sensitivity and good cycle stability prepared in example 2.
Fig. 7 is a strain sensing test curve of the flexible strain sensor with high sensitivity and good cycling stability prepared in example 3.
Fig. 8 is a cycle stability test curve and a partial enlarged view of the flexible strain sensor with high sensitivity and good cycle stability prepared in example 3.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
Example 1:
in this embodiment, a flexible strain sensor with high sensitivity and good cycling stability is prepared by sputtering and depositing a 90nm gold film on a polyimide (125 μm) substrate, and the preparation process is as shown in fig. 1, and the specific steps are as follows:
step 1: cutting the flexible polyimide substrate into a rectangle with the thickness of 2mm multiplied by 16mm, and depositing a layer of gold film with the thickness of 90nm on the flexible polyimide substrate by adopting a magnetron sputtering method.
Step 2: applying a tensile-tensile fatigue load to the polyimide substrate gold film prepared in the step (1), wherein a sine loading mode is adopted, the maximum value and the minimum value of the load are respectively 20N and 2N, the loading frequency is 30Hz, and the loading is 2.4 multiplied by 10 6 Unloading after week to prepare certain amount on the surfaceDensity of fatigue cracks, as shown in fig. 2;
and 3, step 3: and (3) connecting copper leads at two ends of the flexible substrate metal film with the fatigue cracks obtained in the step (2) by using conductive silver adhesive.
The strain sensing test curve of the flexible strain sensor prepared in the embodiment is shown in fig. 3, and the curve shows that the sensitivity factor of the sensor in a micro strain range of 0.5% -1.2% is as high as 3100.
Fig. 4 is a test curve and a partial enlarged view of the cycle stability of the flexible strain sensor prepared in this embodiment. In-cycle strain sensing 10 4 After more than one week, the resistance strain response can still maintain a stable level, and a good dynamic resistance response effect is shown.
Example 2
The embodiment is a flexible strain sensor which is prepared by sputtering and depositing a 170nm gold film on a polyimide (125 mu m) substrate and has high sensitivity and good cycling stability, and the method comprises the following specific steps:
step 1: cutting the flexible polyimide substrate into a rectangle with the thickness of 2mm multiplied by 16mm, and depositing a layer of gold film with the thickness of 170nm on the flexible polyimide substrate by adopting a magnetron sputtering method.
And 2, step: applying a tensile-tensile fatigue load to the polyimide substrate gold film prepared in the step (1), wherein a sine loading mode is adopted, the maximum value and the minimum value of the load are respectively 16N and 1.6N, the loading frequency is 30Hz, and the loading is 2.0 multiplied by 10 6 Unloading after a week to prepare fatigue cracks with a certain density on the surface of the steel plate;
and 3, step 3: and (3) connecting copper leads at two ends of the flexible substrate metal film with the fatigue cracks obtained in the step (2) by using conductive silver adhesive.
The strain sensing test curve of the flexible strain sensor prepared in the embodiment is shown in fig. 5, and the curve shows that the sensitivity factor of the sensor in the micro strain range of 0.4% -0.8% is as high as 3337.
Fig. 6 is a test curve and a partial enlarged view of the cycle stability of the flexible strain sensor prepared in this embodiment. In-cycle strain sensing 10 4 After more than one week, the resistance strain response can still be maintainedThe stable level is maintained, and the good dynamic resistance response effect is shown.
Example 3:
the embodiment is a flexible strain sensor which is prepared by sputtering and depositing a 10nm titanium/200 nm gold film on a polyimide (125 mu m) -based substrate and has high sensitivity and good cycling stability, and the method comprises the following specific steps:
step 1: cutting the flexible polyimide substrate into a rectangle with the thickness of 2mm multiplied by 16mm, depositing a Ti film with the thickness of 10nm on the flexible polyimide substrate by adopting a magnetron sputtering method, and then depositing a gold film with the thickness of 200 nm.
And 2, step: applying a tensile-tensile fatigue load to the polyimide-based bottom gold/titanium film prepared in the step (1), wherein a sine loading mode is adopted, the maximum value and the minimum value of the load are respectively 20N and 2N, the loading frequency is 30Hz, and the loading is 2.0 multiplied by 10 6 Unloading after a week to prepare fatigue cracks with a certain density on the surface of the steel plate;
and step 3: and (3) connecting copper leads at two ends of the flexible substrate metal film with the fatigue cracks obtained in the step (2) by using conductive silver adhesive.
The strain sensing test curve of the flexible strain sensor prepared by the embodiment is shown in fig. 7, and the curve shows that the sensitivity factor of the sensor in the micro-strain range of 0.6% -1.0% is as high as 3000.
Fig. 8 is a test curve and a partial enlarged view of the cycle stability of the flexible strain sensor prepared in this embodiment. In-cycle strain sensing 10 4 After more than one week, the resistance strain response can still maintain a stable level, and a good dynamic resistance response effect is shown.

Claims (2)

1. A preparation method of a flexible strain sensor with high sensitivity and good cycling stability is characterized by comprising the following steps: the method comprises the following steps:
(1) Cutting the flexible substrate into a rectangle with a proper size, and depositing one or more layers of metal films on the flexible substrate; the metal film is deposited by adopting a magnetron sputtering method, the surface appearance of the metal film is in a continuous compact state or a loose porous state, and the metal film selects a plastic film with strong deformability or a brittle film with poor deformability according to the plastic deformability;
(2) Adopting a mechanical testing machine to carry out pulling-pulling fatigue loading on the flexible substrate deposited with the metal film in the step (1) in the length direction of the flexible substrate with a certain strain amplitude and frequency, and unloading after a certain number of cycles so as to form transverse fatigue cracks with a certain density on the surface of the film; wherein, in the process of carrying out the pulling-pulling fatigue loading, a sine loading mode is adopted, the maximum value and the minimum value of the load are respectively 10-25N and 1.0-3.0N, the loading frequency is 25-35Hz, and the loading frequency is more than 1000 weeks;
(3) Connecting electric leads at two ends of the flexible substrate metal film with the fatigue cracks obtained in the step (2) by using conductive adhesive to obtain the flexible strain sensor with high sensitivity and good cycling stability; the flexible strain sensor has high sensitivity in the strain range of less than 1.5 percent, and the sensitivity factor can reach 10 3 The above;
the flexible strain sensor is performing cyclic strain sensing 10 4 After more than one week, the resistance strain response can still maintain a stable level.
2. The method of claim 1 for making a flexible strain sensor with high sensitivity and good cycling stability, wherein the method comprises the steps of: the sensing performance of the flexible strain sensor is adjusted by adjusting the strain amplitude and the loading frequency during fatigue loading in the preparation process or adjusting the mechanical property and the micro-morphology of the metal film.
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CN111766001A (en) * 2019-04-01 2020-10-13 天津大学 Micro-wrinkle gold thin film flexible crack sensor with controllable scale

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101226163A (en) * 2008-01-22 2008-07-23 西安交通大学 Method for measuring metallic film fatigue life on a flexible substrate
CN104949609A (en) * 2015-05-20 2015-09-30 清华大学 Flexible graphene sensor and manufacture method thereof
CN109163654A (en) * 2018-09-10 2019-01-08 中国工程物理研究院电子工程研究所 A kind of flexible strain transducer of super fast response and preparation method thereof
CN111174685A (en) * 2018-11-09 2020-05-19 北京纳米能源与***研究所 Flexible strain sensor and manufacturing method thereof
CN111766001A (en) * 2019-04-01 2020-10-13 天津大学 Micro-wrinkle gold thin film flexible crack sensor with controllable scale

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