CN114894353B - Carbon-based pressure resistance film sensor and preparation method and application thereof - Google Patents
Carbon-based pressure resistance film sensor and preparation method and application thereof Download PDFInfo
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- CN114894353B CN114894353B CN202210366465.3A CN202210366465A CN114894353B CN 114894353 B CN114894353 B CN 114894353B CN 202210366465 A CN202210366465 A CN 202210366465A CN 114894353 B CN114894353 B CN 114894353B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 114
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000010408 film Substances 0.000 claims description 122
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 24
- 238000000151 deposition Methods 0.000 claims description 16
- 229910003481 amorphous carbon Inorganic materials 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 239000010409 thin film Substances 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
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- 230000000873 masking effect Effects 0.000 claims description 4
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- 238000005477 sputtering target Methods 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
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- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/18—Measuring force or stress, in general using properties of piezo-resistive materials, i.e. materials of which the ohmic resistance varies according to changes in magnitude or direction of force applied to the material
-
- 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
- C23C14/04—Coating on selected surface areas, e.g. using masks
- C23C14/042—Coating on selected surface areas, e.g. using masks using masks
-
- 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
- C23C14/0605—Carbon
-
- 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
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
-
- 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
Abstract
The invention discloses a carbon-based pressure resistance film sensor and a preparation method and application thereof. The carbon-based pressure resistance film sensor consists of a wear-resistant layer, a sensing layer, an insulating layer and an electrode layer, wherein the wear-resistant layer, the sensing layer and the insulating layer are all made of carbon-based film materials, the sensing layer is a diamond-like carbon film, and sp is contained in the diamond-like carbon film 3 The content of the-C bond is 30-50%. The invention provides a carbon-based pressure resistance film sensor, wherein each functional layer (a wear-resistant layer, a sensing layer and an insulating layer) of the sensor is made of a carbon-based film material, and the sensor has good structural continuity, and physical and chemical performance parameters such as affinity, elastic modulus, thermal expansion coefficient and the like of each functional layer are matched, so that each functional layer has excellent interface bonding strength, and meanwhile, the high sensitivity of the sensor is ensured.
Description
Technical Field
The invention relates to the technical field of intelligent sensing, in particular to a carbon-based pressure resistance film sensor and a preparation method and application thereof.
Background
Along with the rapid development of technologies such as the internet of things, digital manufacturing, intelligent manufacturing and the like, the requirements on the front-end sensor are higher and higher. At present, most of the sensors are discrete devices, have no protection function, and cannot be installed in harsh working environments such as friction, oxidation, corrosion and the like. In addition, the sensor is far away from the surface of the device, real-time data such as the temperature and the pressure of the device are difficult to accurately reflect, and the working state of the device cannot be accurately judged.
To solve the above problems, the prior art replaces the discrete sensor with a thin film sensor, and provides a protective layer on the sensor surface to protect the sensor device. For example, in the prior art, a wear-resistant protection integrated multifunctional film sensor and a preparation method thereof are provided, and a layer of wear-resistant protection layer made of ceramic material is covered on the surface of the film sensor, so that the surface of an integrated element is protected, the film and an electrode of the sensor are effectively protected, and the service life of the film sensor is effectively prolonged; however, the insulating layer, the sensing layer and the wear-resistant protective layer of the film sensor are all made of different materials, and the physical properties such as elastic modulus, thermal expansion coefficient and the like of the different materials are not matched, so that the interface bonding strength of each functional layer of the film sensor is low, and the sensitivity of the sensor is reduced.
Therefore, how to enhance the wear resistance of the sensor and improve the interface bonding strength and the sensitivity of the sensor between the functional layers is a difficult problem to be solved by the current thin film sensor.
Disclosure of Invention
The invention aims to overcome the defects and the defects of low interface bonding strength and low sensor sensitivity of the prior wear-resistant film sensor, and provides a carbon-based pressure resistance film sensor, wherein each functional layer is made of a carbon-based film material and sp in a sensing layer 3 The content of the C bond is 30-50%, so that the interface bonding strength between functional layers of the wear-resistant film sensor and the sensitivity of the sensor are obviously improved.
The invention further aims to provide a preparation method of the carbon-based pressure resistance thin film sensor.
It is still another object of the present invention to provide the use of the carbon-based piezoresistive film sensor in sensing wear resistant workpieces.
The above object of the present invention is achieved by the following technical scheme:
the carbon-based pressure resistance film sensor consists of a wear-resistant layer, a sensing layer, an insulating layer and an electrode layer;
the wear-resistant layer, the sensing layer and the insulating layer are all made of carbon-based film materials;
the sensing layer is a diamond-like carbon (DLC) film with the thickness of 200-600 nm;
sp in the diamond-like carbon film 3 The content of the-C bond is 30-50%.
According to the carbon-based pressure resistance film sensor, the wear-resistant layer, the sensing layer and the insulating layer are made of carbon-based film materials, so that physical and chemical performance parameters such as affinity, elastic modulus, thermal expansion coefficient and the like of the materials of each layer are matched, the interface bonding strength of each functional layer of the film sensor, especially the interface bonding strength between the insulating layer and the wear-resistant layer, is remarkably improved, the wear-resistant layer is not easy to peel off in the friction process, and the service life of the carbon-based pressure resistance film sensor is effectively prolonged.
In addition, the sensing layer of the carbon-based pressure resistance film sensor is a diamond-like carbon (DLC) film, and the pressure resistance performance of the DLC film and sp in the structure thereof 3 -C bond and sp 2 The content and distribution of the-C bonds, sp 3 The band gap of the C framework structure is large, thus playing an insulating and blocking role, and sp 2 The band gap of the-C is small, the conduction effect is achieved, and under the action of pressure, sp in the diamond-like carbon film 2 The C-bond rotates, the interconnection causes resistance change, and piezoresistance occurs. When sp is 3 When the content of the C bond is increased, sp 2 The size of the C bond cluster is reduced, the resistance change is large under the stress action, and the sensitivity coefficient is increased; but with sp 3 At the same time as the content of C bonds increases, the modulus of elasticity of the sensing layer increases, the resistance to deformation under stress increases, and the sensitivity coefficient decreases.
The sensing layer of the carbon-based pressure resistance film sensor is sp 3 -a diamond-like carbon film having a C bond content of 30% to 50%, exhibiting excellent piezoresistive properties; when sp is included in diamond-like carbon film 3 -C bond content < 30% or sp in diamond-like carbon film 3 The piezoresistive sensitivity coefficient is lower when the C bond content is more than 50 percent. Meanwhile, the inventor finds that when the thickness of the sensing layer is 200-600 nm, the sensing layer has good breakdown resistance and good deformability, and further the carbon-based pressure resistance thin film sensor has high sensitivity. In addition, sp in the sensing layer 3 The content of C bonds is calculated from Raman spectroscopy.
Preferably, sp in the sensing layer 3 The content of the-C bond is 35-45%.
In a specific embodiment, the insulating layer of the invention is silicon, oxygen co-doped diamond-like carbon (SiO 2 DLC: H) film with a thickness of 200 to 600nm, siO 2 -DLThe H film has good insulativity, and can reduce the thickness of the insulating layer, thereby improving the sensitivity of the carbon-based pressure resistance film sensor.
Preferably, the Si content in the insulating layer is 10-15% and the O content is 20-30%, wherein the Si content in the insulating layer is regulated and controlled by changing the power of a magnetron sputtering Si target, and the O content is controlled by introducing O 2 Is provided; in addition, when the content of Si in the insulating layer is 10-15% and the content of O is 20-30%, the insulating layer can be ensured to have excellent insulating property and better hardness, so that the interface bonding strength between the insulating layer and the sensing layer and between the insulating layer and the wear-resistant layer can be improved. The Si and O contents in the insulating layer are calculated by Raman spectroscopy.
In specific embodiments, the wear-resistant layer is a tetrahedral amorphous carbon (ta-C) film with a thickness of 400-600 nm.
The invention adopts the tetrahedral amorphous carbon film as the wear-resistant layer of the carbon-based pressure resistance film sensor, and compared with other wear-resistant materials, the tetrahedral amorphous carbon (ta-C) film simultaneously contains sp with high hardness (high wear resistance) 3 -C bond and graphite sp with lubricating action 2 And C bonds enable the wear-resistant layer to have wear resistance and lubricating performance, show low friction coefficient and low wear rate, fully exert the protection function of the wear-resistant layer, and effectively prolong the service life of the carbon-based pressure resistance film sensor.
Preferably, sp in the wear-resistant layer 3 The content of the-C bond is more than or equal to 60 percent.
When sp in the wear-resistant layer 3 When the content of the C bond is more than or equal to 60%, the wear-resistant layer has higher hardness, so that the wear-resistant lubrication performance of the wear-resistant layer can be enhanced, and the critical load value of the sensor can be better improved.
Preferably, sp in the wear-resistant layer 3 The content of the C bond is less than or equal to 80 percent.
The invention also provides a preparation method of the carbon-based pressure resistance film sensor, which adopts an arc evaporation composite magnetron sputtering coating machine for preparation; the electric arc evaporation composite magnetron sputtering coating machine consists of a vacuum chamber, three magnetron sputtering sources, an electric arc evaporation source and a workpiece support capable of rotating simultaneously, wherein the workpiece support is arranged in the vacuum chamber.
The preparation method comprises the following steps:
s1, depositing a lower insulating layer on the surface of a substrate by magnetron sputtering;
s2, depositing an electrode layer by adopting a masking method and magnetron sputtering on the basis of the lower insulating layer in the S1;
s3, depositing a diamond-like carbon (DLC) film sensing layer by adopting a masking method and magnetron sputtering on the basis of the electrode layer in the S2;
s4, on the basis of the diamond-like carbon (DLC) film sensing layer in the S3, an insulating layer is deposited by magnetron sputtering;
s5, depositing a wear-resistant layer by adopting a cathodic arc on the basis of the upper insulating layer in the S4, and obtaining the carbon-based pressure resistance film sensor.
The application of the carbon-based pressure resistance film sensor in the sensing of the wear-resistant workpiece is also within the protection scope of the invention.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides a carbon-based pressure resistance film sensor, wherein each functional layer (a wear-resistant layer, a sensing layer and an insulating layer) of the sensor is made of a carbon-based film material, and the sensor has good structural continuity, and physical parameters such as elastic modulus, thermal expansion coefficient and the like of each functional layer are matched, so that the sensor has excellent interface bonding strength between each functional layer, the critical load value reaches 36-62N, and the high sensitivity of the sensor reaches 4.2-7.4. In addition, the carbon-based pressure resistance film sensor also has excellent wear resistance, and the wear rate reaches 6.4x10 -8 mm 3 The friction coefficient is as low as 0.1, and the device can be suitable for various working conditions and can monitor the working state of the surface of a workpiece in real time.
2. The invention also provides a preparation method of the carbon-based pressure resistance film sensor, which has short period and low cost, can be used for large-scale industrial production, and is suitable for all coating manufacturing industries.
Drawings
FIG. 1 is a schematic diagram of the manufacturing process of a carbon-based pressure resistance thin film sensor in example 1;
FIG. 2 is a schematic diagram of a carbon-based pressure resistance thin film sensor in example 1;
FIG. 3 is a schematic diagram of a mask plate used in the preparation process of the carbon-based pressure resistance thin film sensor in example 1;
FIG. 4 is a scratch diagram of a carbon-based pressure-resistant thin film sensor in embodiment 1;
FIG. 5 is a graph showing friction curves of the carbon-based pressure resistance thin film sensor in example 1;
FIG. 6 shows the wear scar morphology of the carbon-based resistive film sensor of example 1.
Detailed Description
The invention will be further described with reference to the following specific embodiments, but the examples are not intended to limit the invention in any way. Raw materials reagents used in the examples of the present invention are conventionally purchased raw materials reagents unless otherwise specified.
Example 1
A carbon-based pressure resistance film sensor is composed of a wear-resistant layer, a sensing layer, an insulating layer and an electrode layer (shown in figure 2);
wherein the sensing layer is a diamond-like carbon (DLC) film with the thickness of 200nm; sp in the sensing layer 3 -a C bond content of 30%;
the insulating layer is silicon-oxygen co-doped diamond-like carbon (SiO) 2 DLC: H) film having a thickness of 1 μm, si content of 15% and O content of 30%;
the wear-resistant layer is a tetrahedral amorphous carbon (ta-C) film with the thickness of 400nm; sp in the wear-resistant layer 3 -a C bond content of 60%; wherein sp in the sensing layer and the wear-resistant layer 3 The C bond content and the Si and O contents in the insulating layer are calculated by Raman spectrometry.
The carbon-based pressure resistance film sensor is prepared by adopting an arc evaporation composite magnetron sputtering coating machine, wherein the arc evaporation composite magnetron sputtering coating machine consists of a vacuum chamber, three magnetron sputtering sources respectively provided with graphite, copper and silicon targets, a graphite target and a workpiece support capable of rotating simultaneously are arranged on an arc evaporation source, and the workpiece support is arranged in the vacuum chamber.
The specific preparation method comprises the following steps (shown in figure 1):
s1, preparing a lower insulating layer:placing the pretreated substrate into a vacuum chamber of an arc evaporation composite magnetron sputtering coating machine, then starting a graphite sputtering target and a silicon sputtering target, and controlling the introduction of O 2 The flow rate is 2-6 sccm, the flow rate of Ar is 150-250 sccm, C 2 H 2 The flow is 20-30 sccm, the cavity pressure is controlled to be 0.5Pa, the bias voltage is-100V, the power of the C target magnetron sputtering power supply is 2.5kw, the power of the Si target magnetron sputtering power supply is 0.5 kw-0.75 kw, and the deposition time is 1.5-2.5 h;
s2, preparing a Cu electrode: taking out the sample in the step S1, covering a No. 1 mask plate (shown in fig. 3), and then loading back into the vacuum cavity; vacuumizing to a vacuum degree of 5.0X10 -3 Starting a copper sputtering target below Pa, controlling the flow of Ar to be 200-300 sccm, controlling the cavity pressure to be 0.4Pa, the bias voltage to be-100V, the power of a magnetron sputtering power supply to be 2kw, and the deposition time to be 15-30 min;
s3, preparing a sensing layer: taking out the sample in the step S2, replacing the mask plate with the No. 2 mask plate, and then loading the sample back into the vacuum cavity; vacuumizing to a vacuum degree of 5.0X10 -3 Starting a graphite sputtering target below Pa, controlling the flow rate of Ar to be 200sccm, controlling the cavity pressure to be 0.5Pa, the bias voltage to be-100V, the power of a magnetron sputtering power supply to be 2.5kw, and the deposition time to be 40min;
s4, preparing an upper insulating layer: taking out the sample in the step S3, removing the mask plate, and then loading the sample back into the vacuum cavity; vacuumizing to a vacuum degree of 5.0X10 -3 Under Pa, opening the graphite sputtering target and the silicon sputtering target, and controlling the introduction of O 2 The flow rate is 2-6 sccm, the flow rate of Ar is 150-250 sccm, C 2 H 2 The flow is 20-30 sccm, the cavity pressure is controlled to be 0.5Pa, the bias voltage is-100V, the power of a graphite target magnetron sputtering power supply is 2.5kw, the power of a silicon target magnetron sputtering power supply is 0.5 kw-0.75 kw, and the deposition time is 1.5-2.5 h;
s5, preparing a wear-resistant layer: and (3) placing the sample in the step (S4) into a vacuum chamber of a composite magnetron sputtering coating machine, starting an arc graphite target, controlling the flow of Ar to be 200-300 sccm, controlling the cavity pressure to be 0.8-1 Pa, the bias voltage to be-60V, the arc flow of the arc target to be 60-80A, and the deposition time to be 20min, thus obtaining the carbon-based pressure resistance film sensor.
Wherein, the preprocessing in the step S1 is as follows:
(1) Cleaning a substrate: delivering the polished substrate into an ultrasonic cleaner, sequentially carrying out ultrasonic cleaning by using acetone and absolute ethyl alcohol respectively, rinsing by using deionized water, and drying by using common nitrogen;
(2) Vacuumizing and glow cleaning: cleaning the coating chamber by a high-power dust collector; placing the ultrasonically cleaned substrate on a workpiece support of a vacuum chamber, and vacuumizing the vacuum chamber to vacuum of 5.0X10 -3 Under Pa, 100-300 sccm argon is introduced, the bias voltage is set to be minus 600V to minus 900V, and the etching cleaning process lasts for 5-30 min;
(3) Ion beam etching the substrate: 200-300 sccm argon is introduced into the ion source, the partial pressure is set to-800 to-1000V, the power of the ion source is 0.8-1.2 kW, and the working time is 10-30 min.
Example 2
A carbon-based pressure resistance film sensor consists of a wear-resistant layer, a sensing layer, an insulating layer and an electrode layer;
wherein the sensing layer is a diamond-like carbon (DLC) film with the thickness of 200nm; sp in the sensing layer 3 -C bond content 50%;
the insulating layer is silicon-oxygen co-doped diamond-like carbon (SiO) 2 DLC: H) film with a thickness of 1 μm;
the wear-resistant layer is a tetrahedral amorphous carbon (ta-C) film with the thickness of 400nm; sp in the wear-resistant layer 3 -C bond content of 60%.
The method for manufacturing the carbon-based piezoresistive film sensor is basically the same as that of example 1, except that the bias voltage is set to-300V in step S3.
Example 3
A carbon-based pressure resistance film sensor consists of a wear-resistant layer, a sensing layer, an insulating layer and an electrode layer;
wherein the sensing layer is a diamond-like carbon (DLC) film with the thickness of 200nm; sp in the sensing layer 3 -C bond content of 35%;
the insulating layer is silicon-oxygen co-doped diamond-like carbon (SiO) 2 DLC: H) film with a thickness of 1 μm;
the wear-resistant layer is a tetrahedral amorphous carbon (ta-C) film with the thickness of 400nm; sp in the wear-resistant layer 3 -C bond content of 60%.
The method for manufacturing the carbon-based piezoresistive film sensor is basically the same as that of example 1, except that the bias voltage is set to-150V in step S3.
Example 4
A carbon-based pressure resistance film sensor consists of a wear-resistant layer, a sensing layer, an insulating layer and an electrode layer;
wherein the sensing layer is a diamond-like carbon (DLC) film with the thickness of 200nm; sp in the sensing layer 3 -C bond content 45%;
the insulating layer is silicon-oxygen co-doped diamond-like carbon (SiO) 2 DLC: H) film with a thickness of 1 μm;
the wear-resistant layer is a tetrahedral amorphous carbon (ta-C) film with the thickness of 400nm; sp in the wear-resistant layer 3 -C bond content of 60%.
The method for manufacturing the carbon-based piezoresistive film sensor is basically the same as that of example 1, except that the bias voltage is set to-200V in step S3.
Example 5
A carbon-based pressure resistance film sensor consists of a wear-resistant layer, a sensing layer, an insulating layer and an electrode layer;
wherein the sensing layer is a diamond-like carbon (DLC) film with the thickness of 600nm; sp in the sensing layer 3 -a C bond content of 30%;
the insulating layer is silicon-oxygen co-doped diamond-like carbon (SiO) 2 DLC: H) film with a thickness of 1 μm;
the wear-resistant layer is a tetrahedral amorphous carbon (ta-C) film with the thickness of 400nm; sp in the wear-resistant layer 3 -C bond content of 60%.
The preparation method of the carbon-based pressure resistance film sensor is basically the same as that of the embodiment 1, except that the magnetron sputtering deposition time in the step S3 is 120min.
Example 6
A carbon-based pressure resistance film sensor consists of a wear-resistant layer, a sensing layer, an insulating layer and an electrode layer;
wherein the sensing layer is a diamond-like carbon (DLC) film with the thickness of 200nm; sp in the sensing layer 3 -a C bond content of 30%;
the insulating layer is silicon-oxygen co-doped diamond-like carbon (SiO) 2 DLC: H) film with a thickness of 1 μm;
the wear-resistant layer is a tetrahedral amorphous carbon (ta-C) film with the thickness of 400nm; sp in the wear-resistant layer 3 -C bond content 80%.
The method for manufacturing the carbon-based piezoresistive film sensor is basically the same as that of example 1, except that the bias voltage is set to-80V in step S5.
Example 7
A carbon-based pressure resistance film sensor consists of a wear-resistant layer, a sensing layer, an insulating layer and an electrode layer;
wherein the sensing layer is a diamond-like carbon (DLC) film with the thickness of 200nm; sp in the sensing layer 3 -a C bond content of 30%;
the insulating layer is silicon-oxygen co-doped diamond-like carbon (SiO) 2 DLC: H) film with a thickness of 1 μm;
the wear-resistant layer is a tetrahedral amorphous carbon (ta-C) film with the thickness of 400nm; sp in the wear-resistant layer 3 -C bond content 50%.
The method for manufacturing the carbon-based piezoresistive film sensor is basically the same as that of example 1, except that the bias voltage is set to-40V in step S5.
Example 8
A carbon-based pressure resistance film sensor consists of a wear-resistant layer, a sensing layer, an insulating layer and an electrode layer;
wherein the sensing layer is a diamond-like carbon (DLC) film with the thickness of 200nm; sp in the sensing layer 3 -a C bond content of 30%;
the insulating layer is silicon-oxygen co-doped diamond-like carbon (SiO) 2 DLC: H) film having a thickness of 1.5 μm, si content of 10% and O content of 20%;
the wear-resistant layer is a tetrahedral amorphous carbon (ta-C) film with the thickness of 600nm; sp in the wear-resistant layer 3 -C bond content of 60%.
The preparation method of the carbon-based pressure resistance thin film sensor is basically the same as that of example 1, except that the deposition time in step S5 is 30min.
Comparative example 1
A carbon-based pressure resistance film sensor consists of a wear-resistant layer, a sensing layer, an insulating layer and an electrode layer;
wherein the sensing layer is a diamond-like carbon (DLC) film with the thickness of 200nm; sp in the sensing layer 3 -a C bond content of 20%;
the insulating layer is silicon-oxygen co-doped diamond-like carbon (SiO) 2 DLC: H) film with a thickness of 1 μm;
the wear-resistant layer is a tetrahedral amorphous carbon (ta-C) film with the thickness of 400nm; sp in the wear-resistant layer 3 -C bond content of 60%.
The method for manufacturing the carbon-based piezoresistive film sensor is basically the same as that of example 1, except that the bias voltage is set to-50V in step S3.
Comparative example 2
A carbon-based pressure resistance film sensor consists of a wear-resistant layer, a sensing layer, an insulating layer and an electrode layer;
wherein the sensing layer is a diamond-like carbon (DLC) film with the thickness of 200nm; sp in the sensing layer 3 -a C bond content of 60%;
the insulating layer is silicon-oxygen co-doped diamond-like carbon (SiO) 2 DLC: H) film with a thickness of 1 μm;
the wear-resistant layer is a tetrahedral amorphous carbon (ta-C) film with the thickness of 400nm; sp in the wear-resistant layer 3 -C bond content of 60%.
The method for manufacturing the carbon-based piezoresistive film sensor is basically the same as that of example 1, except that the bias voltage is set to-250V in step S3.
Performance testing
The carbon-based pressure resistance thin film sensors prepared in the above examples and comparative examples were subjected to performance test, and the specific test method is as follows:
(1) Scratch test: the sensor is subjected to scratch test by using a diamond needle through a scratch tester, the sensor damage condition after scratch is observed by using an optical microscope, the first occurrence of fracture (namely the occurrence of interlayer peeling) of the piezoresistive film sensor (wear-resistant layer) is taken as a critical load, the higher the load is, the higher the interface bonding force between the layers is, the more scratch resistance of the sensor is realized, and the specific test result is shown in table 1. In embodiment 1, the scratch graph of the carbon-based piezoresistive film sensor is shown in fig. 4, and fig. 4 shows that the critical load of the carbon-based piezoresistive film sensor reaches 48N, which indicates that the sensor has good interfacial bonding force between the layers.
(2) Piezoresistance effect test: the piezoresistive film sensor is loaded with pressure through a press, the resistor instrument is connected with the sensing layer through an electrode and a wire, the change of resistance is observed after the pressure is loaded, and the sensitivity coefficient GF is calculated through the following formula:
where Ro is the initial resistance, R is the resistance after loading the stress, F is the loaded stress, E is the elastic modulus of the material, epsilon is the corresponding tensile strain, and the specific test results are shown in table 1.
(3) The friction coefficient is measured by a ball-disc friction wear instrument, the pressure is 8N, the friction radius is 8mm, and the friction partner ball is Al 2 O 3 The friction circle number is 20000. As shown in the friction graph 5 of the carbon-based piezoresistive film sensor in embodiment 1, as can be seen from fig. 5, the abrasion-resistant layer of the carbon-based piezoresistive film sensor has excellent lubricity, the friction coefficient is as low as 0.1, and the friction coefficients of other embodiments are also at the same level.
(4) Wear rate, V (mm) was calculated by using a laser copolymerization Jiao Cechu friction post-wear trace cross-sectional view and combining the formula V=A×2pi r 3 ) The abrasion loss is calculated by the formulaThe wear rate was calculated. In embodiment 1, the wear mark morphology of the carbon-based piezoresistive film sensor is shown in fig. 6, and as can be seen from fig. 6, the wear-resistant layer of the carbon-based piezoresistive film sensor has good wear resistance, and the wear rate reaches 6.4x10 -8 mm 3 Nm; the wear rates of other embodiments are substantially at the same level.
Test results
TABLE 1
In the present invention, the critical load values of the carbon-based piezoresistive film sensors in examples 1 to 4 and comparative examples 1 to 2 are different, but in the knowledge of those skilled in the art, 45N to 48N are substantially at the same level, i.e., other conditions are unchanged, sp in the sensing layer 3 The effect on the critical load value is small when the C bond content varies within a certain range; at the same time, sp in the sensing layer of the carbon-based pressure resistance film sensor can be found 3 When the content of the C bond is 30-50%, the excellent interface bonding strength between the layers is realized, and meanwhile, the higher sensitivity coefficient is kept.
As is clear from examples 1 and 5, when the thickness of the sensing layer is large, the stress between the sensing layer and the other layers increases, resulting in a decrease in interface bonding strength and a decrease in critical load; meanwhile, due to the increase of the thickness of the sensing layer, the strain of the sensing layer is smaller under the same stress effect, and the sensitivity coefficient is slightly reduced.
As can be seen from examples 1, 6 and 7, sp in the carbon-based pressure-resistant thin film sensor sensing layer 3 The content of the-C bonds is the same, sp in the wear-resistant layer 3 The higher the C bond content, the greater the hardness of the wear-resistant layer and the greater the critical load value; however, as the hardness of the wear-resistant layer increases, the overall deformability of the carbon-based piezoresistive film sensor decreases, and the sensitivity coefficient decreases.
The above examples of the present invention are merely illustrative of the present invention and are not intended to limit the embodiments of the present invention. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are desired to be protected by the following claims.
Claims (7)
1. The carbon-based pressure resistance film sensor is characterized by comprising a wear-resistant layer, a sensing layer, an insulating layer and an electrode layer;
the wear-resistant layer, the sensing layer and the insulating layer are all made of carbon-based film materials;
the sensing layer is a diamond-like carbon film, and the thickness of the sensing layer is 200-600 nm;
sp in the diamond-like carbon film 3 The content of the C bond is 30-50%;
the insulating layer is a diamond-like carbon film co-doped with silicon and oxygen, the content of silicon in the insulating layer is 10% -15%, and the content of oxygen is 20% -30%.
2. The carbon-based piezoresistive film sensor according to claim 1, wherein sp in the sensing layer 3 The content of the-C bond is 35-45%.
3. The carbon-based piezoresistive thin film sensor according to claim 1, wherein the wear-resistant layer is a tetrahedral amorphous carbon film.
4. The carbon-based piezoresistive film sensor according to claim 3, wherein sp in the wear-resistant layer 3 The content of the-C bond is more than or equal to 60 percent.
5. The carbon-based piezoresistive film sensor according to claim 3, wherein sp in the wear-resistant layer 3 The content of the C bond is 60-80%.
6. A method of manufacturing a carbon-based piezoresistive film sensor according to any one of claims 1 to 5, comprising the steps of:
s1, depositing a lower insulating layer on the surface of a substrate by magnetron sputtering;
s2, depositing an electrode layer by adopting a masking method and magnetron sputtering on the basis of the lower insulating layer in the S1;
s3, depositing a diamond-like carbon film sensing layer by adopting a masking method and magnetron sputtering on the basis of the electrode layer in the S2;
s4, depositing an insulating layer by magnetron sputtering on the basis of the diamond-like carbon film sensing layer in the S3;
s5, depositing a wear-resistant layer by adopting a cathodic arc on the basis of the upper insulating layer in the S4, and obtaining the carbon-based pressure resistance film sensor.
7. Use of a carbon-based piezoresistive film sensor according to any of claims 1-5 in sensing wear resistant workpieces.
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EP1354181A1 (en) * | 2001-01-08 | 2003-10-22 | Fraunhofer-Gesellschaft Zur Förderung Der Angewandten Forschung E.V. | Sensor for determining the state of parameters on mechanical components while using amorphous carbon layers having piezoresistive properties |
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CN102225640A (en) * | 2011-04-07 | 2011-10-26 | 宁波甬微集团有限公司 | Film for raising abrasion resistance of compressor slide plate and preparation method thereof |
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