CN108333234A - A kind of use for electrochemical tests film sample and preparation method thereof - Google Patents
A kind of use for electrochemical tests film sample and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of use for electrochemical tests film samples and preparation method thereof, belong to metallic film material technical field.The use for electrochemical tests film sample of the present invention, including substrate layer and the metal film layer that is arranged on substrate layer, metal film layer includes work department and sealing；The sealing has been conductively connected conductive electrode on the side surface far from substrate layer, and the insulated enclosure layer covered for the connecting portion to conductive electrode and sealing is provided on the sealing.The use for electrochemical tests film sample of the present invention can be such that electrode is well contacted with sample to be tested, can ensure the insulated enclosure in non-test region and the validity test area of sample to be tested, and then ensure accuracy and the sensitivity of sample to be tested electrochemical property test.
Description
Technical field
The present invention relates to a kind of use for electrochemical tests film samples and preparation method thereof, belong to metallic film material technology neck
Domain.
Background technology
Thin-film material can realize multiple functions, be widely used to multiple fields, as in integrated circuit metal line,
The wear-resistant coating etc. of high-temperaure coating and some workpiece surfaces on electrode, engine blade.
In application process, corrosion is to influence one of an important factor for its performance plays to thin-film material.Particularly, for gold
Belong to thin-film material, electrochemical corrosion influences to be particularly acute on it.In order to ensure that thin-film material can be under the conditions of corresponding normally
It is on active service, needs to test its chemical property.
In the aspect of performance of the electrochemical corrosion resistant of testing film material, compared with corrosion weight loss method, electrochemical method tool
There is the advantages of quicklook.For example, by polarization curve, the parameters such as corrosion potential, the corrosion electric current density of material can be obtained,
By electrochemical impedance spectroscopy, abundant dynamic information and electrode interface structural information can be obtained.
When carrying out electro-chemical test to metal film sample, need sample to be tested and electrode welding.For film material
Material, if taking the mode directly welded, thin-film material will appear warpage, remove the phenomenon that even falling off in the welding process, system
Sample success rate cannot be guaranteed.
Invention content
The use for electrochemical tests film sample that the purpose of the present invention is to provide a kind of connections reliably, sample preparation success rate is high.
The present invention also aims to provide a kind of preparation method of use for electrochemical tests film sample.
To achieve the above object, the technical solution of use for electrochemical tests film sample of the invention is：
A kind of use for electrochemical tests film sample, including substrate layer and the metal film layer that is arranged on substrate layer, gold
It includes work department and sealing to belong to film layer, and insulated enclosure layer is provided on the sealing.
The use for electrochemical tests film sample of the present invention, has been divided into work department and sealing, and sealing by metallic film
Insulated enclosure layer is set in portion, electrode can be arranged between sealing and insulated enclosure layer in this way, be made electrode and wait for test sample
Product well contact, and can ensure the insulated enclosure in non-test region and the validity test area of sample to be tested, and then ensure to wait for
The accuracy of sample electrochemical property test and sensitivity.Corrosion ring when insulated enclosure layer is to prevent sealing and test
Border contacts, and work department is only made to be contacted with corrosive environment when test.
In addition, electrode must keep drying with sample to be tested junction when test, if there is steam, test result can deviate really
Value, is unable to get ideal test result.On the sealing of the present invention insulated enclosure layer that is arranged can by conductive electrode with it is close
The position of envelope portion connection seals well.
The electro-chemical test is one kind in polarization curve test, cyclic voltammetry and electrochemical impedance test.
It is conductively connected conductive electrode on one side surface of the separate substrate layer of the sealing.Conductive electrode is arranged close
In envelope portion, the end of electrode can be made to be protected by the insulated enclosure layer on sealing, avoid electrode and metallic film junction by
To the influence of external force of environment, the stability of test is improved.
The substrate layer, metal film layer thickness ratio be 0.4~2：1.
The substrate layer is glass or polyimides.The thickness of the substrate layer is 0.125~1mm.
The metal film layer is metal or alloy, and the metal is one or more of in tungsten, molybdenum, copper, titanium, aluminium；It is described
Alloy is one kind in molybdenum tantalum alloy, molybdenum niobium alloy, Tin Silver Copper Alloy.In the molybdenum niobium alloy molybdenum and niobium mass ratio be 90~
95：5~10.
The thickness of the metal film layer is 50nm~3mm.Preferably, the thickness of the metal film layer be 50nm~
3000nm.Or the thickness of the metal film layer is 0.01mm~3mm.
The insulated enclosure layer is silicon rubber.Preferably, insulated enclosure layer is single-component room-temperature-vulsilicone silicone rubber.It insulate close
The thickness of sealing is 1mm~3mm.
The area for being used for contacting with metallic film on substrate is 2cm2~10cm2.It is used for connecing with environment to be measured on metallic film
Tactile sample to be tested work area is 1cm2.The area of the exposed surface of the work area namely work department.
Conductive electrode is copper or silver.The total length of conductive electrode is 5cm~20cm.It is set on the middle part peripheral surface of conductive electrode
It is equipped with insulating layer.Conductive electrode is 0.5cm~1cm not by the length in the exposed portion of insulating layer covering per one end.
Silver paste covering part is provided between the sealing and insulated enclosure layer, one end of the conductive electrode is embedded in silver
It starches in covering part.The area of silver paste covering part is 0.5~0.6cm2.The thickness of silver paste covering part is 1~3mm.
The technical solution of preparation method of the use for electrochemical tests film sample of the present invention is：
A kind of preparation method of use for electrochemical tests film sample, includes the following steps：Take sample layer, the sample layer packet
The metal film layer for including old bottom and being arranged on substrate layer coats insulated enclosure material on the sealing of metal film layer
Material, and formed insulated enclosure layer to get.
Before coating insulating sealing materials on the sealing of metal film layer, it is fixedly connected and leads on the sealing of metallic film
Electrode is fixedly connected with conductive electrode and includes the following steps：Silver paste is coated on the sealing of metallic film and forms the first silver medal
One end of conductive electrode is placed on the first silver slurry layer by pulp layer, is then coated silver paste on the first silver slurry layer again and is formed second
Silver slurry layer, solidification silver paste to get.The solidification silver paste is 0.5~2h of vacuum drying at 80~200 DEG C.First silver slurry layer and
Two silver slurry layers form silver paste covering part.
The area of silver paste covering part is 0.5~0.6cm2.The thickness of silver paste covering part is 1~3mm.
The sample layer is dried in vacuo 8~12h before coating insulating sealing materials at 80~200 DEG C.
Cured after coating insulating sealing materials on the sealing of metal film layer and forms the insulated enclosure layer.
Insulating sealing materials are cured as room temperature curing.
The substrate layer is glass or polyimides.The thickness of the substrate layer is 0.125~1mm.
The metal film layer is metal or alloy, and the metal is one or more of in tungsten, molybdenum, copper, titanium, aluminium；It is described
Alloy is one kind in molybdenum tantalum alloy, molybdenum niobium alloy, Tin Silver Copper Alloy.In the molybdenum niobium alloy molybdenum and niobium mass ratio be 90~
95：5~10.
Sample layer is deposited metal on substrate and is obtained by physical vapour deposition (PVD), chemical vapor deposition or thermal spraying
's.The thickness for the metal layer being deposited on substrate is 50nm~3mm.Preferably, the thickness of the metal film layer be 50nm~
3000nm.Or the thickness of the metal film layer is 0.01mm~3mm.
Specifically, when using physical vapour deposition (PVD) or chemical vapor deposition method, the thickness of the metal film layer is
50nm~3000nm.When using heat spraying method, the thickness of the metal film layer is 0.01mm~3mm.
The insulated enclosure layer is silicon rubber.Preferably, insulated enclosure layer is single-component room-temperature-vulsilicone silicone rubber.It insulate close
The thickness of sealing is 1mm~3mm.
Conductive electrode is copper or silver.The total length of conductive electrode is 5cm~20cm.It is set on the middle part peripheral surface of conductive electrode
It is equipped with insulating layer.Conductive electrode is 0.5cm~1cm not by the length in the exposed portion of insulating layer covering per one end.
The beneficial effects of the invention are as follows：
The preparation method of the use for electrochemical tests film sample of the present invention is simple to operation, and cost is relatively low, and can make
Electrode is well contacted with sample to be tested, can ensure the insulated enclosure in non-test region and the validity test face of sample to be tested
Product, and then ensure accuracy and the sensitivity of sample to be tested electrochemical property test.
Description of the drawings
Fig. 1 is the structural schematic diagram of the use for electrochemical tests film sample in embodiment 1；
Fig. 2 is the electrochemical impedance spectroscopy test result of the sample in embodiment 1-4；
Fig. 3 is that the dynamic potential polarization curve of the sample in embodiment 1-4 tests test result.
Specific implementation mode
Technical scheme of the present invention is described further with reference to specific embodiment.
Silver paste used in following example is provided by Guangzhou Kai Xiang Electronic Products Inc., single-component room-temperature vulcanized silicon rubber
Glue is provided by Wuxi day Si Da electronic seals material factory.
Embodiment 1
The use for electrochemical tests film sample of the present embodiment includes sample layer, and sample layer includes that substrate layer 1 and setting exist
Metal film layer 2 on substrate layer, metal film layer include work department and sealing, sealing and lining corresponding with sealing
Insulated enclosure layer 3 is provided on the peripheral surface of floor portions and end face.
Substrate layer is glass.Substrate layer is the rectangle of long 2cm, width 1cm.The thickness of substrate layer is 0.5mm.Metal film layer
For molybdenum.Metallic film is also the rectangle of long 2cm, width 1cm.The thickness of metal film layer is 500nm.Insulated enclosure layer is one pack system
Room temperature vulcanized silicone rubber.The thickness of insulated enclosure layer is 3mm.
Film sample further includes conductive electrode 5, one end of conductive electrode 5 be fixed at sealing and insulated enclosure layer it
Between.Specifically, being provided with silver paste covering part 4 between sealing and insulated enclosure layer, the corresponding end of conductive electrode, which is wrapped, to be set
It sets in silver paste covering part.Silver paste covering part is circle, and area is about 0.5cm2, thickness 2mm.
Metal film layer is divided into above-mentioned work department and sealing using the center line of rectangle along its length as line of demarcation.Work
Surface of the portion far from substrate layer side constitutes region to be measured, and the work area in region to be measured is 1cm2。
Conductive electrode is copper, length 10cm, the length in the conductive electrode portion between sealing and insulated enclosure layer
Degree is 0.5cm.It is about wherein 0.318cm by the length for the part that silver paste covering part is wrapped up.The other end has the length of 0.5cm naked
Dew, the portion of external of intermediate 0.5cm long are enclosed with insulating layer.
The preparation method of the use for electrochemical tests film sample of the present embodiment includes the following steps：
1) deposition forms molybdenum film and obtains sample layer on the upper surface of glass substrate.Specifically use magnetron sputtering
Method deposits molybdenum film on a glass substrate.Glass substrate is used to acetone and absolute ethyl alcohol ultrasonic cleaning respectively successively first
15min is fixed on coating chamber substrate bottom plate after drying.Then 4.8 × 10 are evacuated to-4Pa, being filled with argon gas makes sputtering pressure protect
0.5Pa is held, adjusting electric current makes sputtering power keep 100W.Next reverse sputtering cleaning is carried out to target, removes surface impurity layer,
Baffle is removed after 10min, starts to deposit molybdenum film on a glass substrate.Baffle is closed after about 30min, stops sputtering, it is final to obtain
To certain thickness molybdenum film.
Glass substrate is the rectangle of long 2cm, width 1cm, substrate thickness 0.5mm, the shapes and sizes and lining of metallic film
The shapes and sizes at bottom are identical, form and are completely covered to substrate top surface, and the thickness of metallic film is 500nm；
2) sample obtained in step 1) is placed in vacuum drying chamber, is dried in vacuo 10h at 150 DEG C, is cooled to
It is taken out after room temperature；Using the center line of the length direction of the rectangle of sample layer as line of demarcation, by the metal film layer of line of demarcation both sides point
Working region and sealing area are not set as it；
3) silver paste is coated at the center of the sealing area of metal film layer and forms the first silver slurry layer, and the first silver slurry layer is circle
Shape, area 0.5cm2, thickness 1mm；Then copper conductive electrode is taken, one end of conductive electrode is placed on the first silver slurry layer
Center；Silver paste is coated on the first silver slurry layer upper surface again and forms the second silver slurry layer, and conductive electrode is contacted with the first silver slurry layer
One end formed covering；Second silver slurry layer is also circle, area 0.5cm2, thickness 1mm；Then by above-mentioned coated silver paste
Layer is simultaneously arranged the sample layer of conductive electrode and is placed in vacuum drying chamber, is dried in vacuo 1h at 150 DEG C, silver paste is made to cure, obtain
To the sample layer of setting electrode；
4) sealing material will be coated on the outer surface of the sealing of the sample layer for the setting electrode that step 3) obtains, sealing material
Material is single-component room-temperature vulcanized silicone rubber, and sealing material is applied only to one end of sealing and substrate corresponding with sealing
In end outer surface, the corresponding end of conductive electrode is also covered, capped region forms non-test area, metal
The working region of film layer exposes, and the surface area of working region is 1cm2, this part working region forms test section；
After the sample layer for coating sealing material is cured at room temperature to get.
Embodiment 2
The use for electrochemical tests film sample of the present embodiment includes sample layer, and sample layer includes that substrate layer and setting are serving as a contrast
Metal film layer on bottom, metal film layer include work department and sealing, sealing and substrate corresponding with sealing
Insulated enclosure layer is provided on the peripheral surface of layer segment and end face.
Substrate layer is polyimides.Substrate layer is the rectangle of long 2cm, width 1cm.The thickness of substrate layer is 125 μm.Metal foil
Film layer is molybdenum.Metallic film is also the rectangle of long 2cm, width 1cm.The thickness of metal film layer is 500nm.Insulated enclosure layer is single
Component room temperature vulcanized silicone rubber.The thickness of insulated enclosure layer is 3mm.
Film sample further includes conductive electrode, one end of conductive electrode be fixed at sealing and insulated enclosure layer it
Between.Specifically, being provided with silver paste covering part between sealing and insulated enclosure layer, the corresponding end of conductive electrode is wrapped setting
In silver paste covering part.Silver paste covering part is circle, area 0.5cm2, thickness 2mm.
Metal film layer is divided into above-mentioned work department and sealing using the center line of rectangle along its length as line of demarcation.Work
The surface of side of the portion far from old bottom constitutes region to be measured, and the work area in region to be measured is 1cm2。
Conductive electrode is copper, length 8cm, the length in the conductive electrode portion between sealing and insulated enclosure layer
For 0.5cm.It is about wherein 0.318cm by the length for the part that silver paste covering part is wrapped up.The other end has the exposed of 0.5cm length,
The portion of external of intermediate 1cm long is enclosed with insulating layer.
The preparation method of the use for electrochemical tests film sample of the present embodiment includes the following steps：
1) deposition forms molybdenum film and obtains sample layer on the upper surface of polyimide substrate.Specifically use magnetic control
Sputtering method deposits molybdenum film on a glass substrate.Polyimide substrate is used to acetone and absolute ethyl alcohol ultrasound respectively successively first
Wave cleans 15min, and coating chamber substrate bottom plate is fixed on after drying.Then 4.8 × 10 are evacuated to-4Pa, being filled with argon gas makes sputtering
Air pressure keeps 0.5Pa, and adjusting electric current makes sputtering power keep 100W.Next reverse sputtering cleaning is carried out to target, removes surface
Impurity layer removes baffle after 10min, starts to deposit molybdenum film on substrate.Baffle is closed after about 30min, stops sputtering, finally
Obtain certain thickness molybdenum film.
Polyimide substrate be long 2cm, width 1cm rectangle, substrate thickness be 125 μm of mm, the shape of metallic film and greatly
It is small identical with the shapes and sizes of substrate, substrate top surface is formd and is completely covered, the thickness of metallic film is
500nm；
2) sample obtained in step 1) is placed in vacuum drying chamber, is dried in vacuo 12h at 100 DEG C, is cooled to
It is taken out after room temperature；Using the center line of the length direction of the rectangle of sample layer as line of demarcation, by the metal film layer of line of demarcation both sides point
Working region and sealing area are not set as it；
3) silver paste is coated at the center of the sealing area of metal film layer and forms the first silver slurry layer, and the first silver slurry layer is circle
Shape, area 0.5cm2, thickness 1mm；Then copper conductive electrode is taken, one end of conductive electrode is placed on the first silver slurry layer
Center；Silver paste is coated on the first silver slurry layer upper surface again and forms the second silver slurry layer, and conductive electrode is contacted with the first silver slurry layer
One end formed covering；Second silver slurry layer is also circle, area 0.5cm2, thickness 1mm；Then by above-mentioned coated silver paste
Layer is simultaneously arranged the sample layer of conductive electrode and is placed in vacuum drying chamber, is dried in vacuo 2h at 100 DEG C, silver paste is made to cure, obtain
To the sample layer of setting electrode；
4) sealing material will be coated on the outer surface of the sealing of the sample layer for the setting electrode that step 3) obtains, sealing material
Material is single-component room-temperature vulcanized silicone rubber, and sealing material is applied only to one end of sealing and substrate corresponding with sealing
In end outer surface, the corresponding end of conductive electrode is also covered, capped region forms non-test area, metal
The working region of film layer exposes, and the surface area of working region is 1cm2, this part working region forms test section；
After the sample layer for coating sealing material is cured at room temperature to get.
Embodiment 3
The use for electrochemical tests film sample of the present embodiment includes sample layer, and sample layer includes that substrate layer and setting are serving as a contrast
Metal film layer on bottom, metal film layer include work department and sealing, sealing and substrate corresponding with sealing
Insulated enclosure layer is provided on the peripheral surface of layer segment and end face.
Substrate layer is glass.Substrate layer is the square that the length of side is 2cm.The thickness of substrate layer is 1mm.Metal film layer is
Molybdenum niobium alloy.The mass ratio of molybdenum and niobium is 95 in molybdenum niobium alloy：5.Metallic film is also the square that the length of side is 2cm.Metal foil
The thickness of film layer is 500nm.Insulated enclosure layer is single-component room-temperature vulcanized silicone rubber.The thickness of insulated enclosure layer is 2mm.
Film sample further includes conductive electrode, one end of conductive electrode be fixed at sealing and insulated enclosure layer it
Between.Specifically, being provided with silver paste covering part between sealing and insulated enclosure layer, the corresponding end of conductive electrode is wrapped setting
In silver paste covering part.Silver paste covering part is circle, area 0.6cm2, thickness 2mm.
Metal film layer is divided into above-mentioned work department and sealing.Surface of the work department far from substrate layer side constitutes to be measured
The work area in region, region to be measured is 1cm2。
Conductive electrode is silver, length 20cm, the length in the conductive electrode portion between sealing and insulated enclosure layer
Degree is 0.5cm.It is about wherein 0.318cm by the length for the part that silver paste covering part is wrapped up.The other end has the length of 0.5cm naked
Dew, the portion of external of intermediate 0.8cm long are enclosed with insulating layer.
The preparation method of the use for electrochemical tests film sample of the present embodiment includes the following steps：
1) molybdenum niobium alloy metallic film is formed by method similar to Example 1 on the upper surface of glass substrate to obtain
Sample layer, glass substrate are the square that the length of side is 2cm, substrate thickness 1mm, the shapes and sizes of metallic film and substrate
Shapes and sizes are identical, form and are completely covered to substrate top surface, and the thickness of metallic film is 500nm；
2) sample obtained in step 1) is placed in vacuum drying chamber, is dried in vacuo 10h at 150 DEG C, is cooled to
It is taken out after room temperature；Sample layer surface is divided into working region and sealing area, wherein work area is 1cm2；
3) silver paste is coated at the center of the sealing area of metal film layer and forms the first silver slurry layer, and the first silver slurry layer is circle
Shape, area 0.6cm2, thickness 1mm；Then silver-colored conductive electrode is taken, one end of conductive electrode is placed on the first silver slurry layer
Center；Silver paste is coated on the first silver slurry layer upper surface again and forms the second silver slurry layer, and conductive electrode is contacted with the first silver slurry layer
One end formed covering；Second silver slurry layer is also circle, area 0.6cm2, thickness 1mm；Then by above-mentioned coated silver paste
Layer is simultaneously arranged the sample layer of conductive electrode and is placed in vacuum drying chamber, is dried in vacuo 1h at 150 DEG C, silver paste is made to cure, obtain
To the sample layer of setting electrode；
4) sealing material will be coated on the outer surface of the sealing of the sample layer for the setting electrode that step 3) obtains, sealing material
Material is single-component room-temperature vulcanized silicone rubber, and sealing material is applied only to one end of sealing and substrate corresponding with sealing
In end outer surface, the corresponding end of conductive electrode is also covered, capped region forms non-test area, metal
The working region of film layer exposes, and the surface area of working region is 1cm2, this part working region forms test section；
After the sample layer for coating sealing material is cured at room temperature to get.
Embodiment 4
The use for electrochemical tests film sample of the present embodiment includes sample layer, and sample layer includes that substrate layer and setting are serving as a contrast
Metal film layer on bottom, metal film layer include work department and sealing, sealing and substrate corresponding with sealing
Insulated enclosure layer is provided on the peripheral surface of layer segment and end face.
Substrate layer is glass.Substrate layer is the square that the length of side is 2cm.The thickness of substrate layer is 0.7mm.Metal film layer
For molybdenum tantalum alloy.The mass ratio of molybdenum and niobium is 92 in molybdenum niobium alloy：8.
Metallic film is also the square that the length of side is 2cm.The thickness of metal film layer is 500nm.Insulated enclosure layer is single
Component room temperature vulcanized silicone rubber.The thickness of insulated enclosure layer is 1.5mm.
Film sample further includes conductive electrode, one end of conductive electrode be fixed at sealing and insulated enclosure layer it
Between.Specifically, being provided with silver paste covering part between sealing and insulated enclosure layer, the corresponding end of conductive electrode is wrapped setting
In silver paste covering part.Silver paste covering part is circle, area 0.6cm2, thickness 2mm.
Metal film layer is divided into above-mentioned work department and sealing.Surface of the work department far from substrate layer side, which constitutes, waits for
Region is surveyed, the work area in region to be measured is 1cm2。
Conductive electrode is copper, length 8cm, the length in the conductive electrode portion between sealing and insulated enclosure layer
For 0.5cm.It is about wherein 0.318cm by the length for the part that silver paste covering part is wrapped up.The other end has the length of 0.5cm exposed,
The portion of external of intermediate 0.6cm long is enclosed with insulating layer.
The preparation method of the use for electrochemical tests film sample of the present embodiment includes the following steps：
1) molybdenum tantalum alloy metallic film is formed by method similar to Example 1 on the upper surface of glass substrate to obtain
Sample layer, glass substrate are the square that the length of side is 2cm, substrate thickness 0.7mm, the shapes and sizes and substrate of metallic film
Shapes and sizes it is identical, substrate top surface is formd and is completely covered, the thickness of metallic film is 500nm；
2) sample obtained in step 1) is placed in vacuum drying chamber, is dried in vacuo 12h at 100 DEG C, is cooled to
It is taken out after room temperature；Sample layer surface is divided into working region and sealing area, wherein work area is 1cm2；
3) silver paste is coated at the center of the sealing area of metal film layer and forms the first silver slurry layer, and the first silver slurry layer is circle
Shape, area 0.6cm2, thickness 1mm；Then copper conductive electrode is taken, one end of conductive electrode is placed on the first silver slurry layer
Center；Silver paste is coated on the first silver slurry layer upper surface again and forms the second silver slurry layer, and conductive electrode is contacted with the first silver slurry layer
One end formed covering；Second silver slurry layer is also circle, area 0.6cm2, thickness 1mm；Then by above-mentioned coated silver paste
Layer is simultaneously arranged the sample layer of conductive electrode and is placed in vacuum drying chamber, is dried in vacuo 1h at 150 DEG C, silver paste is made to cure, obtain
To the sample layer of setting electrode；
4) sealing material will be coated on the outer surface of the sealing of the sample layer for the setting electrode that step 3) obtains, sealing material
Material is single-component room-temperature vulcanized silicone rubber, and sealing material is applied only to one end of sealing and substrate corresponding with sealing
In end outer surface, the corresponding end of conductive electrode is also covered, capped region forms non-test area, metal
The working region of film layer exposes, and the surface area of working region is 1cm2, this part working region forms test section；
After the sample layer for coating sealing material is cured at room temperature to get.
Test example
Use for electrochemical tests film sample in Example 1-4 is tested as follows：
1) electrochemical impedance spectroscopy is tested
The electrochemical impedance spectroscopy of the obtained samples to be tested of embodiment 1-4 is surveyed using CHI600E electrochemical analysers
Examination, test results are shown in figure 2.
Wherein, test temperature is 20 DEG C, the NaCl solution that solution system is 0.9%, and reference electrode selects calomel electrode, auxiliary
It is 5mV to help electrode to select graphite electrode, sinusoid potential amplitude, and scan frequency is 1 × 10-2Hz~1 × 105Hz。
2) dynamic potential polarization curve is tested
The dynamic potential polarization curve of the obtained samples to be tested of embodiment 1-4 is carried out using CHI600E electrochemical analysers
Test, test results are shown in figure 3.
Wherein, test temperature is 20 DEG C, the NaCl solution that solution system is 0.9%, and reference electrode selects calomel electrode, auxiliary
Electrode is helped to select graphite electrode, sweep speed 0.01mV/s, electric potential scanning ranging from -100mV~300mV is (relative to open circuit
Current potential).
From figures 2 and 3, it will be seen that method for making sample provided by the invention can measure the electrochemistry resistance of metal film sample
Anti- spectrum and dynamic potential polarization curve, to reflect the corrosion resistance of metallic film well.In addition, this method has sample preparation
Process is simple, success rate is high, electrode and the advantages that film contacts are good and test result is accurate.
Claims (10)
1. a kind of use for electrochemical tests film sample, which is characterized in that including substrate layer and the metal being arranged on substrate layer
Film layer, metal film layer include work department and sealing；The sealing is conductively connected on the side surface far from substrate layer
There is conductive electrode, it is close that the insulation covered for the connecting portion to conductive electrode and sealing is provided on the sealing
Sealing.
2. use for electrochemical tests film sample according to claim 1, it is characterised in that：The substrate layer is glass or gathers
Acid imide.
3. use for electrochemical tests film sample according to claim 1, it is characterised in that：The substrate layer, metallic film
The thickness ratio of layer is 0.4~2：1.
4. use for electrochemical tests film sample according to claim 1, it is characterised in that：The metal film layer is metal
Or alloy, the metal are one or more of in tungsten, molybdenum, copper, titanium, aluminium；The alloy is molybdenum tantalum alloy, molybdenum niobium alloy, Xi Yin
One kind in copper alloy.
5. use for electrochemical tests film sample according to claim 1, it is characterised in that：The insulated enclosure layer is silicon rubber
Glue.
6. use for electrochemical tests film sample according to claim 1, it is characterised in that：Conductive electrode is copper or silver.
7. according to the use for electrochemical tests film sample described in claim 1-6 any one, it is characterised in that：The sealing
Silver paste covering part is provided between insulated enclosure layer, one end of the conductive electrode is embedded in silver paste covering part.
8. a kind of preparation method of use for electrochemical tests film sample, which is characterized in that include the following steps：Sample layer is taken, institute
It includes old bottom and the metal film layer that is arranged on substrate layer to state sample layer, and metal film layer includes work department and sealing
Portion coats insulating sealing materials on the sealing of metal film layer, and formed insulated enclosure layer to get.
9. the preparation method of use for electrochemical tests film sample according to claim 8, it is characterised in that：Metal film layer
Sealing on coating insulating sealing materials before, be fixedly connected with conductive electrode on the sealing of metallic film, be fixedly connected and lead
Electrode includes the following steps：Silver paste is coated on the sealing of metallic film and forms the first silver slurry layer, by conductive electrode
One end is placed on the first silver slurry layer, is then coated silver paste on the first silver slurry layer again and is formed the second silver slurry layer, cures silver paste, i.e.,
.
10. the preparation method of use for electrochemical tests film sample according to claim 9, it is characterised in that：The solidification
Silver paste is 0.5~2h of vacuum drying at 80~200 DEG C.
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