CN109402579B - (001) Oriented CdS flexible stretchable photosensitive film material and preparation method thereof - Google Patents

(001) Oriented CdS flexible stretchable photosensitive film material and preparation method thereof Download PDF

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CN109402579B
CN109402579B CN201710712152.8A CN201710712152A CN109402579B CN 109402579 B CN109402579 B CN 109402579B CN 201710712152 A CN201710712152 A CN 201710712152A CN 109402579 B CN109402579 B CN 109402579B
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magnetron sputtering
metal film
buffer layer
film
flexible substrate
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CN109402579A (en
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王充
于玫
杨灿灿
于喆
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Shenzhen Institute of Advanced Technology of CAS
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    • 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
    • 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
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
    • C23C14/025—Metallic sublayers
    • 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
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    • 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
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    • C23C14/0629—Sulfides, selenides or tellurides of zinc, cadmium or mercury
    • 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
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment

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Abstract

The invention discloses a flexible stretchable photosensitive material and a preparation method thereof. The method comprises the following steps: 1) preparing a buffer layer with the resistivity of 5K omega-M-5M omega-M on a flexible substrate; 2) preparing a (001) -oriented CdS film on the buffer layer by adopting a magnetron sputtering method, wherein parameters of magnetron sputtering are as follows: the power density of the target gun is 5W/m2～10W/m2The vacuum back pressure is less than 9 x 10‑4Pa, the working air pressure is 0.5Pa to 10 Pa; 3) and annealing to obtain the photosensitive material. The CdS film with (001) orientation is prepared, the flexible and stretchable photosensitive material is obtained, the good electrical property of the flexible and stretchable photosensitive material can be still kept in a large-scale stress stretching state, and the prospect of wearable application is greatly improved.

Description

(001) Oriented CdS flexible stretchable photosensitive film material and preparation method thereof
Technical Field
The invention belongs to the technical field of preparation of wearable application-oriented flexible photoelectric sensing materials, relates to a flexible stretchable photosensitive material and a preparation method thereof, and particularly relates to a flexible stretchable photosensitive film material with (001) -oriented CdS and a preparation method thereof.
Background
Along with the continuous progress of society, the living standard of people is continuously improved, and the rhythm of life is constantly accelerated, and people also are higher and higher to the requirement of quality of life, and the appearance of intelligent wearable equipment has brought new facility for people's life, and wearable equipment can realize the information interaction with the organism to realize the monitoring to physiological index, also can real-time supervision surrounding environment relevant index and data. To realize the above functions, sensors with various functions are required to acquire data, and the sensors inevitably need to be in direct contact with biological tissues and human bodies, so that the wearable application-oriented sensor needs to simultaneously take account of information interaction capability and biological safety, which puts new requirements on flexibility of the sensor.
The flexible sensor is a type of sensor opposite to the rigid sensor, and can still maintain good sensing performance under the condition of deformation such as bending, stretching and the like.
In the preparation of flexible photoelectric devices, many efforts have been made by technicians, such as CN101532178A and CN203820886U, which disclose flexible photosensitive materials and methods for preparing the same, wherein flexible silicone rubber and other materials are respectively used as substrates, and photosensitive materials are prepared on the substrates by different processes. These processes initially achieve flexibility, but the resulting products do not have stretch properties and do not conform to skin and body tissue.
For the photosensitive sensor, a photosensitive material is a key component, and a photosensitive thin film material is a sensor which is made by utilizing the photoelectric effect of a semiconductor and has a resistance value which is changed along with the intensity of incident light; the incident light intensity, resistance decrease, the incident light is weak, resistance increases. Photosensitive materials are generally used for measurement of light, control of light, and photoelectric conversion (converting a change in light into a change in electricity). The cadmium sulfide photoresistor of the commonly used photoresistor changes along with the intensity change of incident light (visible light), the resistance value (dark resistance) of the photoresistor can reach 1-10M ohm under the dark condition, and the resistance value (bright resistance) of the photoresistor is only hundreds to thousands of ohms under the strong light condition (100 LX). The sensitivity (i.e. spectral characteristic) of the photoresistor to light is very close to the response of human eyes to visible light (0.4-0.76) mum, and the resistance value of the photoresistor changes only when the light is sensed by human eyes.
The wearable sensor is limited by the problems of hard materials, low sensitivity of photosensitive film materials and the like, so that the wearable sensor cannot be widely applied, and therefore the preparation process of the stretchable sensor material solves the problems of organ attachment and human tissue protection for wearable application.
For the performance of photosensitive materials, the crystal plane orientation is one of the important parameters determining the performance. The crystal plane orientation means: in the powder state of the crystal material, the distribution of each crystal face direction is equal, and the exposed crystal face is the crystal face with the lowest energy, namely the most stable crystal face. However, in the thin film material, due to the difference of the growth conditions, the surface energy of the substrate material is different, so the exposed and preferentially oriented crystal plane is not necessarily the most stable crystal plane, such as hexagonal CdS, and the exposed crystal plane in nature or most of the thin film materials is (101).
The research on preparing a film material with a specific orientation in the preparation process of the CdS material is relatively less, how to regulate the crystal plane orientation of the photosensitive material so as to improve the flexibility, the stretchability and the sensitivity of the photosensitive material and obtain the photosensitive material which can still keep excellent performance under a large-scale strain condition has important significance, so that the problem that the flexible photosensitive sensing material which can still be stably used under the flexible stretchable use condition cannot be realized in the prior art is solved.
Disclosure of Invention
In view of the above problems in the prior art, an object of the present invention is to provide a flexible and stretchable photosensitive material and a method for preparing the same, and more particularly, to a flexible and stretchable photosensitive film material having (001) _ oriented CdS and a method for preparing the same. According to the invention, the CdS film with (001) orientation is prepared by controlling the resistance of the specific metal buffer layer and adjusting the process parameters during magnetron sputtering of the CdS film, so that the flexible and stretchable photosensitive material is obtained, the good electrical property of the photosensitive material can be still maintained in a large-scale stress stretching state, and the prospect of wearable application is greatly improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a photosensitive material that is flexible and has tensile properties, the photosensitive material comprising a flexible substrate, a buffer layer on the flexible substrate, and a (001) -oriented CdS thin film on the buffer layer.
In the present invention, the "photosensitive material that is flexible and has tensile properties" refers to: a flexible stretchable photosensitive material.
The buffer layer in the present invention is a metal-containing buffer layer.
The invention provides a photosensitive material which is provided with a (001) -oriented CdS film, wherein the CdS crystals have the characteristic of anisotropy, and the CdS films with different orientations have different properties, so that the obtained CdS film with a specific orientation (001) has flexible stretchability, the stretching rate of the CdS film is more than 10%, and the CdS film can still keep good electrical performance under large-scale deformation.
The photosensitive material is a flexible stretchable photosensitive sensing material with a CdS film and metal composite structure with specific orientation, has innovation, and is a metal and semiconductor composite structure photosensitive material with large-scale stretching discovered for the first time at home and abroad.
As a preferable technical scheme of the photosensitive material, the buffer layer is composed of a noble metal film and a low-melting-point metal film with the melting point of below 200 ℃, one side of the noble metal film of the buffer layer is in contact with the flexible substrate, and one side of the low-melting-point metal film of the buffer layer is in contact with the CdS film.
In this preferred embodiment, the melting point is 200 ℃ or lower, for example, 200 ℃, 180 ℃, 170 ℃, 160 ℃, 150 ℃, 135 ℃, 120 ℃, 100 ℃ or 80 ℃, preferably below 190 ℃.
Preferably, the noble metal thin film has a thickness of 2nm to 30nm, for example, 2nm, 4nm, 5nm, 8nm, 10nm, 12nm, 15nm, 18nm, 20nm, 22nm, 25nm, 26nm, 28nm, 30nm, or the like.
Preferably, the thickness of the low melting point metal thin film is 5nm to 20nm, for example, 5nm, 6nm, 8nm, 10nm, 13nm, 15nm, 16nm, 17nm, 18nm, or 20 nm.
Preferably, the CdS thin film has a thickness of 20nm to 1000nm, such as 20nm, 40nm, 100nm, 150nm, 200nm, 225nm, 300nm, 350nm, 400nm, 450nm, 500nm, 550nm, 600nm, 700nm, 750nm, 800nm, 850nm, 900nm, 1000nm, or the like.
Preferably, the noble metal thin film in the buffer layer includes any one of a gold thin film, a silver thin film, or a platinum thin film, or a combination of at least two of them, but is not limited to the above-listed noble metal thin films, and other noble metal thin films commonly used in the art to achieve the same effect may be used in the present invention.
Preferably, the low-melting-point metal film in the buffer layer is a metal film with a work function matched with that of the CdS film.
More preferably, the buffer layer is composed of a noble metal thin film and a low melting point metal thin film having a melting point of 200 ℃ or lower and a work function matching with the CdS thin film, and the low melting point thin film satisfying the above-described conditions for matching the melting point and the work function is not limited to an In thin film, but other low melting point thin films satisfying the above-described conditions for matching the melting point and the work function may be used In the present invention.
In the preferred technical scheme, the work function of the low-melting-point metal film with the melting point below 200 ℃ is matched with the micro-crack structure metal electrode and the photosensitive semiconductor material so as to form ohmic contact.
Preferably, the flexible substrate is a high molecular polymer flexible substrate, preferably a silicone rubber material, and more preferably a silicone rubber material with a stretch ratio of more than 200%.
Preferably, the flexible substrate has a thickness of no more than 0.5cm, such as 0.45cm, 0.4cm, 0.35cm, 0.32cm, 0.3cm, 0.25cm, 0.2cm, or 0.1cm, and the like.
In a second aspect, the present invention provides a method for preparing a photosensitive material according to the first aspect, the method comprising the steps of:
(1) preparing a buffer layer with the resistivity of 5K omega-M-5M omega-M on a flexible substrate;
(2) preparing a (001) -oriented CdS film on the buffer layer by adopting a magnetron sputtering method, wherein the magnetron sputtering method comprises the following process parameters: the power of the target gun is 5W/m2～10W/m2E.g. 5W/m2、5.5W/m2、6W/m2、7W/m2、7.5W/m2、8W/m2、9W/m2Or 10W/m2Etc.; the pressure of the vacuum back is less than 9 x 10-4Pa, e.g. 8X 10-4Pa、7×10-4Pa、6×10-4Pa、5×10- 4Pa、4×10-4Pa、3×10-4Pa or 2X 10-4Pa, etc.; the working pressure is 0.5-10 Pa, such as 0.5Pa, 1Pa, 2Pa, 3.5Pa, 4.5Pa, 5Pa, 6Pa, 8Pa or 10 Pa;
(3) and annealing to obtain the photosensitive material with flexibility and tensile property.
In the step (1) of the present invention, the resistivity of the buffer layer is, for example, 5K Ω · M to 5M Ω · M: 5K Ω · M, 10K Ω · M, 75K Ω · M, 125K Ω · M, 150K Ω · M, 200K Ω · M, 245K Ω · M, 300K Ω · M, 360K Ω · M, 400K Ω · M, 450K Ω · M, 500K Ω · M, 550K Ω · M, 600K Ω · M, 650K Ω · M, 700K Ω · M, 750K Ω · M, 800K Ω · M, 1M Ω · M, 1.2M Ω · M, 1.5M Ω · M, 2M Ω · M, 2.2M Ω · M, 3M Ω · M, 3.5M Ω · M, 4M Ω · M, 4.5M Ω · M, or 5M Ω · M, and the like.
The invention provides a preparation process of a novel flexible photosensitive sensing film material, which comprises the steps of utilizing proper process conditions to control and form a buffer layer with specific resistivity within the range of 5K omega-M-5M omega-M, then carrying out magnetron sputtering on the buffer layer with specific resistivity, controlling the conditions of target gun power, vacuum background air pressure and working air pressure, and finally carrying out low-temperature annealing to obtain a CdS film with (001) orientation, thereby realizing the preparation of the flexible and stretchable photosensitive sensing film.
The CdS photosensitive film with the photo-sensing function and the specific orientation is prepared by the method, the sensing material can be used under large-scale strain, and the use tensile rate range is larger than 10%.
As a preferable technical scheme of the method, the buffer layer in the step (1) is composed of a noble metal film and a low-melting-point metal film with the melting point of below 200 ℃, one side of the noble metal film of the buffer layer is contacted with the flexible substrate, and one side of the low-melting-point metal film of the buffer layer is contacted with the CdS film.
In the preferred technical scheme, the noble metal/low-melting-point metal buffer layer is prepared on the flexible substrate, and the CdS film with a specific orientation (001) is prepared on one side of the low-melting-point metal of the buffer layer, so that the flexible stretchable photosensitive function can be realized, and the photosensitive sensing film material for measuring the light intensity under large-scale strain can be realized.
In the invention, the specific resistivity range of 5K omega-M to 5M omega-M is controlled and formed by different growth conditions, a buffer layer consisting of a noble metal film and a low-melting metal film is prepared by magnetron sputtering, and the resistivity is adjusted to the required range by adjusting the process parameters such as the power, the air pressure and the like of the magnetron sputtering.
As a preferred technical scheme of the method, the process for preparing the buffer layer on the flexible substrate comprises the following steps:
(A) preparing a noble metal film on a flexible substrate by magnetron sputtering;
(B) then preparing a low-melting-point metal film with the melting point below 200 ℃ on the noble metal film, thereby forming a buffer layer consisting of the noble metal film and the low-melting-point metal film on the flexible substrate.
Preferably, the magnetron sputtering in the step (A) is direct current or radio frequency magnetron sputtering.
Preferably, during the magnetron sputtering of the step (A), the power density of the target gun is 1W/m2～10W/m2E.g. 1W/m2、2W/m2、3W/m2、3.5W/m2、4W/m2、5W/m2、5.5W/m2、6W/m2、7W/m2、8.5W/m2Or 10W/m2Etc.; the working air pressure is 0.5Pa to 10Pa, for example, 0.5Pa, 1Pa, 2Pa, 3.5Pa, 4.5Pa, 5Pa, 6Pa, 8Pa, or 10 Pa.
Preferably, during the magnetron sputtering in the step (A), the vacuum back pressure is less than 9X 10-3Pa, e.g. 8X 10-3Pa、、7×10-4Pa、6×10-4Pa、5×10-4Pa、4×10-4Pa、3×10-4Pa、2×10-4Pa or 1X 10-4Pa, and the like.
Preferably, in the magnetron sputtering process in the step (A), the temperature of the sample stage is 25 ℃ to 200 ℃, such as 25 ℃, 35 ℃, 50 ℃, 65 ℃, 80 ℃, 90 ℃, 100 ℃, 120 ℃, 135 ℃, 150 ℃, 170 ℃, 180 ℃, 190 ℃ or 200 ℃ and the like.
Preferably, in the magnetron sputtering process in step (a), the growth time is 1s to 30s, such as 1s, 3s, 4s, 5s, 6s, 8s, 10s, 12s, 14s, 16s, 18s, 20s, 23s, 25s, or 30 s.
Preferably, the low melting point metal film of step (B) is a metal film having a work function matching that of the CdS film.
Preferably, the low-melting-point metal film is prepared in the step (B) by adopting a magnetron sputtering method, and the magnetron sputtering is preferably direct-current magnetron sputtering or radio-frequency magnetron sputtering.
Preferably, the step (B) adopts a magnetron sputtering method to prepare the low-melting-point metal film, and the following process parameters are controlled: the power of the target gun is 1W/m2～3W/m2E.g. 1W/m2、1.5W/m2、1.8W/m2、2W/m2、2.2W/m2、2.4W/m2、2.7W/m2Or W/m2Etc.; the working air pressure is 0.5Pa to 10Pa, for example, 0.5Pa, 1Pa, 3Pa, 4Pa, 5Pa, 7Pa, 8Pa, 10Pa, or the like.
Preferably, the step (B) adopts a magnetron sputtering method to prepare the low-melting-point metal film, and the vacuum back pressure is controlled to be less than 2 x 10-3Pa, e.g. 1.5X 10-3Pa、1×10-3Pa、0.5×10-3Pa or 0.2X 10-3Pa, and the like.
Preferably, the step (B) adopts a magnetron sputtering method to prepare the low-melting metal film, and the temperature of the sample stage is controlled to be 25-200 ℃, such as 25 ℃, 30 ℃, 45 ℃, 60 ℃, 80 ℃, 100 ℃, 125 ℃, 145 ℃, 170 ℃, 180 ℃ or 200 ℃ and the like.
Preferably, the step (B) uses a magnetron sputtering method to prepare the low melting point metal thin film, and the growth time is controlled to be 10s to 60s, for example, 10s, 20s, 25s, 35s, 40s, 50s, 55s or 60s, etc.
In the process of preparing the buffer layer on the flexible substrate, the target gun power and the working air pressure of the magnetron sputtering in the steps (A) and (B) are the most critical parameters for adjusting the resistivity of the buffer layer, and the method is favorable for accurately controlling the resistivity of the buffer layer to be 5K omega-M-5M omega-M.
In the step (2), the magnetron sputtering adopted for preparing the (001) -oriented CdS film is the radio frequency magnetron sputtering.
Preferably, in the step (2) of preparing the (001) oriented CdS thin film by magnetron sputtering, the temperature of the sample stage is 25 ℃ to 200 ℃, for example, 25 ℃, 30 ℃, 35 ℃, 40 ℃, 60 ℃, 80 ℃, 100 ℃, 125 ℃, 130 ℃, 140 ℃, 150 ℃, 165 ℃, 180 ℃ or 200 ℃.
As a preferable technical scheme of the method, in the step (2) of preparing the (001) oriented CdS film by adopting a magnetron sputtering method, the growth time is preferably 80 s-500 s, such as 80s, 100s, 125s, 140s, 160s, 185s, 200s, 220s, 245s, 280s, 320s, 350s, 375s, 400s, 450s or 500 s.
As a preferable technical scheme of the method, the annealing in the step (3) is performed in Ar gas and/or N2Under protection.
The "Ar gas and/or N" according to the invention2"means: may be Ar gas or N gas2Ar gas and N may also be used2The mixed gas of (1).
Preferably, the annealing temperature in step (3) is 150 ℃ to 200 ℃, such as 150 ℃, 160 ℃, 165 ℃, 175 ℃, 180 ℃, 190 ℃ or 200 ℃, etc.
Preferably, the annealing time in the step (3) is 10min, 15min, 18min, 20min, 22min, 24min, 25min, 27min, 28min or 30min, etc.
As a further preferred embodiment of the method of the present invention, the method comprises the following steps (see fig. 1 for a schematic process flow diagram for preparing the flexible stretchable photosensitive material):
(1) preparing a buffer layer with the resistivity of 5K omega-M-5M omega-M on a flexible substrate, wherein the buffer layer is composed of a noble metal film and a low-melting-point metal film with the melting point below 200 ℃, one side of the noble metal film of the buffer layer is in contact with the flexible substrate, and the specific process comprises the following steps:
(A) preparing a noble metal thin film layer on a high molecular polymer flexible substrate by magnetron sputtering, wherein the magnetron sputtering has the following technological parameters: the power density of the target gun is 1W/m2～10W/m2The vacuum back pressure is less than 9 x 10-3Pa, the working pressure is 0.5Pa to 10Pa, the temperature of the sample stage is 25 ℃ to 200 ℃, and the growth time is 1s to 30 s;
(B) then preparing a low-melting-point metal film layer with the melting point below 200 ℃ on the noble metal film by magnetron sputtering, wherein the parameters of the magnetron sputtering are as follows: the power of the target gun is 1W/m2～3W/m2The pressure of the vacuum back is less than 2 x 10-3Pa, working pressure of 0.5-10 Pa, sample stage temperature of 25-200 deg.C, and growth time of 10-60 s, so as to obtain the invented productA buffer layer composed of a noble metal thin film and a low-melting metal thin film is formed on the substrate, and the resistivity of the buffer layer is 5K omega M-5M omega M.
(2) Preparing a (001) -oriented CdS film on the buffer layer by adopting a radio frequency magnetron sputtering method, wherein the process parameters of the radio frequency magnetron sputtering method are as follows: the power density of the target gun is 5W/m2～10W/m2The vacuum back pressure is less than 9 x 10-4Pa, the working pressure is 0.5 Pa-10 Pa.
(3) Annealing at 150-200 deg.C (i.e. low temperature annealing) under Ar protection to obtain the photosensitive material with flexibility and tensile property, i.e. flexible and stretchable photosensitive material (see FIG. 2 for its structural schematic diagram).
According to the preferred technical scheme, a precious metal film is prepared on a flexible substrate through magnetron sputtering, then a precious metal/low-melting metal buffer layer is formed by preparing a metal with matched work function and low melting point on the precious metal film, the technological parameters of magnetron sputtering are adjusted to enable the resistivity of the buffer layer to be 5K omega-M-5M omega-M, under the condition of the specific resistivity, a CdS film material with specific (001) orientation is prepared by utilizing magnetron sputtering and adjusting parameters such as proper target gun power, vacuum background air pressure, working air pressure and the like, and finally the photosensitive film material with stretchability is realized through low-temperature annealing.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the CdS film with (001) orientation is prepared by controlling the resistance of the specific metal buffer layer and adjusting the process parameters during magnetron sputtering of the CdS film, so that the flexible and stretchable photosensitive material is obtained, the good electrical property of the photosensitive material can be still maintained in a large-scale stress stretching state, and the prospect of wearable application is greatly improved.
2. According to the invention, the low-melting-point metal and the noble metal which are matched in work function are compounded to be used as the buffer layer, the low-melting-point metal which is matched in work function plays a role in optimizing an interface between the noble metal and CdS, ohmic contact, namely low-resistance contact, is formed between the metal and the CdS, the electrical property of the sensor can be greatly improved, and a foundation is laid for realizing better photosensitive property of the sensing material.
3. The invention provides a process for obtaining a flexible sensing material by compounding metal and CdS under a low-temperature condition, which provides an important technical reference for the field of flexible sensor preparation.
4. The invention prepares the CdS film with (001) orientation by controlling the growth conditions, which provides important technical reference for the process of preparing the CdS film with specific orientation.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention for preparing a flexible stretchable photosensitive material.
Fig. 2 is a schematic structural diagram of a flexible stretchable photosensitive material prepared by the present invention, wherein 1 represents a high molecular polymer flexible substrate, 2 represents a noble metal layer, 3 represents a low melting point metal layer, and 4 represents a (001) -oriented CdS thin film.
Fig. 3 is an XRD pattern of the sample prepared in example 1.
Fig. 4 is an SEM image of the sample prepared in example 1.
Fig. 5 is an XRD pattern of the sample prepared in example 2.
Fig. 6 is an SEM image of the sample prepared in example 2.
Fig. 7 is an XRD spectrum of the sample prepared in comparative example 1.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
Example 1
Firstly, preparing a gold film on a PDMS substrate by magnetron sputtering, wherein the process for preparing the gold film is direct current magnetron sputtering, and the power of a target gun is 5W/m2The vacuum back pressure is 5 × 10-3Pa, the working pressure is 3Pa, the temperature of the sample stage is 25 ℃, the growth time is 5s, and the thickness of the obtained Au film is 10 nm.
Then preparing low-melting-point metal In with work function matched with CdS on the gold film to form an Au/In buffer layer, wherein the process for preparing the In film is direct-current magnetron sputtering, and the power of a target gun is 2W/m2The vacuum back pressure is 2 x 10-3Pa, workThe air pressure is 1Pa, the temperature of the sample stage is 35 ℃, the growth time is 20s, and the thickness of the obtained In film is 15 nm. The Au/In buffer layer finally obtained had a resistivity of 8 K.OMEGA.m.
And preparing a CdS film on the Au/In buffer layer by magnetron sputtering, wherein the obtained film is a CdS film material with (001) orientation. The preparation process is radio frequency magnetron sputtering, and the power of a target gun is 5W/m2The vacuum back pressure is 5 × 10-4Pa, working pressure of 0.5Pa, sample stage temperature of 100 ℃, and growth time of 300 s.
And finally, annealing for 20min at 180 ℃ under the protection of Ar gas to form good ohmic contact between the CdS film and the buffer layer, thereby obtaining the flexible stretchable (001) oriented photosensitive CdS film material with the stretching rate of more than 10%.
FIG. 3 is an XRD pattern of a sample prepared in this example 1, from which it can be seen that the sample has (002) orientation and (002) and (001) are equivalent parallel crystal planes.
Fig. 4 is an SEM image of the sample prepared in example 1, and it can be seen from the figure that the prepared cadmium sulfide thin film has the characteristics of SK growth mode, i.e., island-like growth is mainly used, growth is performed in a layered mode when a certain thickness is reached, and then growth is performed in an island-like mode in such a reciprocating cycle. The figure shows that the prepared film material has good compactness and good uniformity.
Example 2
Firstly, preparing a platinum film on a rubber substrate by magnetron sputtering, wherein the process for preparing the platinum film is direct current magnetron sputtering, and the power of a target gun is 4W/m2The vacuum back pressure is 5 × 10-3Pa, working pressure of 2Pa, sample stage temperature of 25 ℃, growth time of 3s, and obtained Pt film thickness of 12 nm.
Then preparing low-melting-point metal In with work function matched with CdS on the Pt film to form a Pt/In buffer layer, wherein the process for preparing the In film is direct-current magnetron sputtering, and the power of a target gun is 3W/m2The vacuum back pressure is 1 × 10-3Pa, working pressure of 0.8Pa, sample stage temperature of 30 ℃, growth time of 22s, and thickness of the obtained In film of 20 nm. The resistivity of the finally obtained Pt/In buffer layer is 1M omega M.
And preparing the CdS film on the Pt/In buffer layer by magnetron sputtering, wherein the obtained film is a CdS film material with (001) orientation. The preparation process is radio frequency magnetron sputtering, and the power of a target gun is 6W/m2The vacuum back pressure is 2 x 10-4Pa, working pressure of 0.7Pa, sample stage temperature of 80 ℃ and growth time of 240 s.
And finally, annealing for 10min at 190 ℃ under the protection of Ar gas to form good ohmic contact between the CdS film and the buffer layer, thereby obtaining the flexible stretchable (001) oriented photosensitive CdS film material with the stretching rate of more than 10%.
FIG. 5 is an XRD pattern of a sample prepared in this example 2, from which it can be seen that the sample has (002) orientation and (002) and (001) are equivalent parallel crystal planes.
Fig. 6 is an SEM image of the sample prepared in example 2, and it can be seen that the prepared cadmium sulfide thin film has the characteristics of SK growth mode, i.e., island-like growth is mainly used, growth is performed in a layered mode when a certain thickness is reached, and then growth is performed in an island-like mode in such a reciprocating cycle. The figure shows that the prepared film material has good compactness and good uniformity.
Example 3
Firstly, preparing a silver film on a PDMS substrate by magnetron sputtering, wherein the process for preparing the gold film is radio frequency magnetron sputtering, and the power of a target gun is 8W/m2Vacuum back pressure of 4X 10-3Pa, working pressure of 5Pa, sample stage temperature of 30 ℃, growth time of 20s, and thickness of the obtained Ag film of 10 nm.
Then preparing low-melting-point metal In with work function matched with CdS on the silver film to form an Ag/In buffer layer, wherein the process for preparing the In film is direct-current magnetron sputtering, and the power of a target gun is 1W/m2The vacuum back pressure is 1.5 multiplied by 10-3Pa, working pressure of 3Pa, temperature of the sample stage of 40 ℃, growth time of 30s, and thickness of the obtained In film of 20 nm. The resistivity of the finally obtained Ag/In buffer layer was 0.8 M.OMEGA.m.
Preparing a CdS film on the Ag/In buffer layer by magnetron sputtering, wherein the obtained film is a CdS film material with (001) orientationAnd (5) feeding. The preparation process is radio frequency magnetron sputtering, and the power of a target gun is 7.5W/m2The vacuum back pressure is 6.5 multiplied by 10-4Pa, working pressure of 7Pa, sample stage temperature of 50 deg.C, and growth time of 150 s.
And finally, annealing for 25min at 155 ℃ under the protection of Ar gas to form good ohmic contact between the CdS film and the buffer layer, thereby obtaining the flexible stretchable (001) oriented photosensitive CdS film material with the stretching rate of more than 10%.
Example 4
Firstly, preparing a platinum film on a rubber substrate by magnetron sputtering, wherein the process for preparing the platinum film is direct current magnetron sputtering, and the power of a target gun is 10W/m2Vacuum back pressure of 8 x 10-3Pa, working pressure of 10Pa, sample stage temperature of 60 ℃, growth time of 30s, and obtained Pt film thickness of 20 nm.
Then preparing low-melting-point metal In with work function matched with CdS on the Pt film to form a Pt/In buffer layer, wherein the process for preparing the In film is direct-current magnetron sputtering, and the power of a target gun is 1.5W/m2The vacuum back pressure is 0.5 × 10-3Pa, working pressure of 9Pa, temperature of the sample stage of 120 ℃, growth time of 10s, and thickness of the obtained In film of 10 nm. The resistivity of the finally obtained Pt/In buffer layer was 1.5 M.OMEGA.m.
And preparing the CdS film on the Pt/In buffer layer by magnetron sputtering, wherein the obtained film is a CdS film material with (001) orientation. The preparation process is radio frequency magnetron sputtering, and the power of a target gun is 10W/m2Vacuum back pressure of 8 x 10-4Pa, working pressure of 8.5Pa, sample stage temperature of 150 ℃ and growth time of 400 s.
Finally in N2And under protection, annealing at 200 ℃ for 10min to form good ohmic contact between the CdS film and the buffer layer, thereby obtaining the flexible stretchable (001) -oriented photosensitive CdS film material with the stretching rate of more than 10%.
Example 5
Firstly, preparing a gold film on a high molecular polymer flexible substrate by magnetron sputtering, wherein the process for preparing the gold film is direct current magnetron sputtering, and the power of a target gun is 1.5W/m2True of trueAir pressure of the empty back is 1.5 multiplied by 10-3Pa, working pressure of 1Pa, sample stage temperature of 135 ℃, growth time of 2s, and thickness of the obtained Au film of 4 nm.
Then preparing low-melting-point metal In with work function matched with CdS on the Au film to form an Au/In buffer layer, wherein the process for preparing the In film is direct-current magnetron sputtering, and the power of a target gun is 2.5W/m2The vacuum back pressure is 1.2 × 10-3Pa, working pressure of 5Pa, temperature of the sample stage of 160 ℃, growth time of 45s, and thickness of the obtained In film of 19 nm. The Au/In buffer layer finally obtained had a resistivity of 1.8 M.OMEGA.m.
And preparing a CdS film on the Au/In buffer layer by magnetron sputtering, wherein the obtained film is a CdS film material with (001) orientation. The preparation process is radio frequency magnetron sputtering, and the power of a target gun is 8.5W/m2Vacuum back pressure of 4X 10-4Pa, working pressure of 10Pa, sample stage temperature of 185 ℃, and growth time of 200 s.
And finally, annealing for 15min at 175 ℃ under the protection of Ar gas to form good ohmic contact between the CdS film and the buffer layer, thereby obtaining the flexible stretchable (001) oriented photosensitive CdS film material with the stretching rate of more than 10%.
Comparative example 1
The preparation method and conditions were the same as those of example 1 except that the resistivity of the Au/In buffer layer was controlled to 1K Ω · m.
Fig. 7 is an XRD pattern of the sample prepared in comparative example 1, and it can be seen from the XRD pattern that the prepared sample has (100) orientation when the resistance value of the buffer layer is too small.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.

Claims (28)

1. A flexible photosensitive material with tensile properties, wherein the photosensitive material comprises a flexible substrate, a buffer layer on the flexible substrate, and a (001) oriented CdS thin film on the buffer layer; the buffer layer is composed of a noble metal film and a low-melting-point metal film with the melting point below 200 ℃, one side of the noble metal film of the buffer layer is in contact with the flexible substrate, and one side of the low-melting-point metal film of the buffer layer is in contact with the CdS film.
2. The photosensitive material of claim 1, wherein the noble metal thin film has a thickness of 2nm to 30 nm.
3. The photosensitive material of claim 1, wherein the low melting point metal thin film has a thickness of 5nm to 20 nm.
4. The photosensitive material of claim 1, wherein the CdS thin film has a thickness of 20nm to 1000 nm.
5. The photosensitive material according to claim 1, wherein the low melting point metal film in the buffer layer is a metal film having a work function matching that of the CdS film.
6. The photosensitive material of claim 1, wherein the low melting point metal film in the buffer layer is an indium film.
7. The photosensitive material of claim 1, wherein the flexible substrate is a high molecular polymer flexible substrate.
8. The photosensitive material of claim 1, wherein the flexible substrate is a silicone rubber material.
9. The photosensitive material of claim 1, wherein the flexible substrate is a silicone rubber material having an elongation of greater than 200%.
10. The photoactive material of claim 1 wherein the flexible substrate has a thickness of no more than 0.5 cm.
11. The photosensitive material of claim 1, wherein the CdS thin film has a stretch greater than 10%.
12. The method for preparing a photosensitive material according to claim 1, comprising the steps of:
(1) preparing a buffer layer with the resistivity of 5K omega-M-5M omega-M on a flexible substrate;
(2) preparing a (001) -oriented CdS film on the buffer layer by adopting a magnetron sputtering method, wherein the magnetron sputtering method comprises the following process parameters: the power density of the target gun is 5W/m2～10W/m2The vacuum back pressure is less than 9 x 10-4Pa, the working air pressure is 0.5Pa to 10 Pa;
(3) annealing to obtain a flexible photosensitive material with tensile property;
the buffer layer in the step (1) is composed of a noble metal film and a low-melting-point metal film with the melting point below 200 ℃, one side of the noble metal film of the buffer layer is in contact with the flexible substrate, and one side of the low-melting-point metal film of the buffer layer is in contact with CdS.
13. The method of claim 12, wherein the step (1) of preparing the buffer layer on the flexible substrate comprises:
(A) preparing a noble metal film on a flexible substrate by magnetron sputtering;
(B) then preparing a low-melting-point metal film with the melting point below 200 ℃ on the noble metal film, thereby forming a buffer layer consisting of the noble metal film and the low-melting-point metal film on the flexible substrate.
14. The method of claim 13, wherein the magnetron sputtering of step (a) is dc or rf magnetron sputtering.
15. The method of claim 13, wherein during the magnetron sputtering of step (A), the target gun power density is 1W/m2～10W/m2The working pressure is 0.5 Pa-10 Pa.
16. The method of claim 13, wherein during said magnetron sputtering of step (a), a vacuum backing pressure is less than 9 x 10-3Pa。
17. The method of claim 13, wherein during the magnetron sputtering in step (A), the temperature of the sample stage is 25 ℃ to 200 ℃, and the growth time is preferably 1s to 30 s.
18. The method of claim 13, wherein the low melting point metal film of step (B) is a metal film having a work function matched to that of CdS film.
19. The method according to claim 13, wherein step (B) is carried out by using magnetron sputtering, preferably DC or RF magnetron sputtering, to prepare the low melting point metal film.
20. The method according to claim 13, wherein the step (B) adopts a magnetron sputtering method to prepare the low-melting-point metal film, and the following process parameters are controlled: the power of the target gun is 1W/m2～3W/m2The working pressure is 0.5 Pa-10 Pa.
21. The method of claim 13, wherein the step (B) is to prepare the low melting point metal film by magnetron sputtering, and the vacuum back pressure is controlled to be less than 2 x 10-3Pa。
22. The method according to claim 13, wherein the step (B) adopts a magnetron sputtering method to prepare the low-melting-point metal film, and the following process parameters are controlled: the temperature of the sample stage is 25-200 ℃, and the growth time is 10-60 s.
23. The method according to claim 12, wherein the magnetron sputtering used in the step (2) of preparing the (001) -oriented CdS thin film is radio frequency magnetron sputtering.
24. The method as claimed in claim 12, wherein in the step (2) of preparing the (001) oriented CdS film by magnetron sputtering, the temperature of the sample stage is 25-200 ℃ and the growth time is 80-500 s.
25. The method of claim 12, wherein the annealing of step (3) is performed under Ar gas and/or N2Under protection.
26. The method of claim 12, wherein the annealing of step (3) is performed at a temperature of 150 ℃ to 200 ℃.
27. The method of claim 12, wherein the annealing of step (3) is performed for a time period of 10min to 30 min.
28. The method according to claim 12, characterized in that it comprises the steps of:
(1) preparing a buffer layer with the resistivity of 5K omega-M-5M omega-M on a flexible substrate, wherein the buffer layer is composed of a noble metal film and a low-melting-point metal film with the melting point below 200 ℃, one side of the noble metal film of the buffer layer is in contact with the flexible substrate, and the specific process comprises the following steps:
(A) preparing a noble metal film on a flexible substrate by magnetron sputtering, wherein the magnetron sputtering has the following technological parameters: the power density of the target gun is 1W/m2～10W/m2The vacuum back pressure is less than 9 x 10-3Pa, the working pressure is 0.5Pa to 10Pa, the temperature of the sample stage is 25 ℃ to 200 ℃, and the growth time is 1s to 30 s;
(B) then is atPreparing a low-melting-point metal film with a melting point below 200 ℃ on the noble metal film by magnetron sputtering, wherein the parameters of the magnetron sputtering are as follows: the power of the target gun is 1W/m2～3W/m2The pressure of the vacuum back is less than 2 x 10-3Pa, the working air pressure is 0.5Pa to 10Pa, the temperature of the sample stage is 25 ℃ to 200 ℃, and the growth time is 10s to 60s, so that a buffer layer consisting of a noble metal film and a low-melting metal film is formed on the flexible substrate, and the resistivity of the buffer layer is 5K omega M to 5M omega M;
(2) preparing a (001) -oriented CdS film on the buffer layer by adopting a radio frequency magnetron sputtering method, wherein the process parameters of the radio frequency magnetron sputtering method are as follows: the power density of the target gun is 5W/m2～10W/m2The vacuum back pressure is less than 9 x 10-4Pa, the working air pressure is 0.5Pa to 10 Pa;
(3) annealing at 150-200 ℃ under the protection of Ar to obtain the flexible photosensitive material with tensile property.
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