A kind of measuring method of metal double polar plates temperature difference resistance energy
Technical field
The present invention relates to a kind of field of fuel cell technology, more particularly to a kind of survey of metal double polar plates temperature difference resistance energy
Determine method.
Background technique
Metal material have conductivity height, good heat conductivity, ductility be good, easy to process, barrier gas mix alter, cost
The advantages that cheap, it is considered to be ideal bipolar plate material.But metal plate strong acid (pH=3), high humidity, high temperature (80 DEG C),
Easily corrode under the harsh working environment of fluorine ion (2-5ppm).Metal plate as bipolar plates in use, need to be in metal
Depositing coating on plate, to improve the corrosion-resistant and electric conductivity of metal double polar plates.After depositing coating, metal double polar plates performance is had greatly
The improvement of amplitude meets the requirement of operation of fuel cells.
But the material of metal substrate and coating (especially multicoat) is not usually identical, causes between different coating, applies
There are apparent difference for thermal expansion coefficient between layer and metal substrate.And fuel cell is in practical applications, is interval mostly
Work, such as the various vehicles, emergency power supply, unmanned aerial vehicle.Metal double polar plates frequently undergo difference variation, will lead to painting
The coefficient of expansion frequently changes between layer, between coating and metal substrate, causes the knot of coating layering and then coating and metal substrate
Resultant force decline, even coating shedding the phenomenon that occur.
The prior art mainly uses scratching instrument to be measured the coating binding force in metal double polar plates, and combines microscope
Use, obtain the combination force data of coating material in the original state (that is, initial number when metal double polar plates have not been used
According to).But the measuring method can not evaluate the difference variation of metal double polar plates in the long-term use to coating failure and
The influence of service life cannot determine the temperature difference resistance energy of metal double polar plates.
Summary of the invention
In view of this, the present invention provides a kind of measuring method of metal double polar plates temperature difference resistance energy, main purpose is energy
Enough long-term temperature difference resistance energy for rapidly evaluating metal double polar plates.
In order to achieve the above objectives, present invention generally provides following technical solutions:
On the one hand, the embodiment of the present invention provides a kind of measuring method of metal double polar plates temperature difference resistance energy, and feature exists
In including the following steps:
Measure initial binding force FA: determine the initial binding force F of the coating and metal substrate in metal double polar platesA;
Measure binding force FB: it simulates in the working environment of metal double polar plates in a fuel cell and simulates metal pair
Pole plate undergoes difference variation with fuel cell discontinuous operation;Simulate discontinuous operation N1After secondary, determine in metal double polar plates
The binding force F of coating and metal substrateB;
Temperature difference resistance can be assessed: according to FA、FB、N1Assess the temperature difference resistance energy of metal double polar plates.
The object of the invention to solve the technical problems also can be used following technical measures and further realize.
Preferably, the initial binding force F of measurementAThe step of, comprising:
Selecting the first metal double polar plates is the sample of metal double polar plates;
The repeatedly binding force of the coating in the first metal double polar plates of measurement and metal substrate, is averaged, it is double to obtain metal
The initial binding force F of coating and metal substrate in pole plateA。
Preferably, the measurement binding force FBThe step of, comprising:
1) selecting the second metal double polar plates is the sample of metal double polar plates, wherein second metal double polar plates are
The initial binding force F of measurementAThe Duplicate Samples of sample used in step;
2) the second metal double polar plates are put into the container for being loaded with simulated solution;Wherein, the simulated solution is simulation
The solution of the working environment of metal double polar plates in a fuel cell;
3) after so that the second metal double polar plates is impregnated the first setting time in the simulated solution of the first set temperature, then make institute
State simulated solution cooled to room temperature;Wherein, first set temperature is the metal double polar plates in actual work
Temperature;
4) step 3) N is repeated1After secondary, the second metal double polar plates are taken out, measure coating and gold in the second metal double polar plates
The binding force for belonging to substrate, obtains binding force FB。
Preferably, the simulated solution is that pH is 2~3, containing 2~5ppm fluorine ion and is passed through the sulphur of hydrogen or oxygen
Acid solution;And/or first setting time is 30s~10min, preferably 1~5min;And/or first set temperature
It is 60~90 DEG C, preferably 75~85 DEG C.
Preferably, in the step of temperature difference resistance can be assessed, including it is calculated using the following equation out the metal pair
The step of start-stop time of resistance to temperature difference N of pole plate:
N=(FA-F0)/(FA-FB)×N1;
Wherein, F0For preset critical;When the binding force of coating and metal substrate is less than or equal to F0When, it is believed that coating loses
Effect;Preferably, F0For 25~27N.
Preferably, in the measurement binding force FBThe step of after, before temperature difference resistance the step of capable of assessing, also wrap
Include accelerated test determination step;Wherein, the accelerated test determination step includes:
Heating and cooling step: after metal double polar plates are heated to the second set temperature, after keeping the second setting time, then by institute
It states metal double polar plates to be put into the simulated solution of third set temperature, impregnates third setting time;Wherein, the simulated solution is
Simulate the solution of the working environment of metal double polar plates in a fuel cell;Second set temperature is greater than the reality of metal double polar plates
Border operating temperature;
Measure binding force FC: repeat the heating and cooling step N2It is secondary, determine coating and metal substrate in metal double polar plates
Binding force FC;
Terminate test: metal double polar plates pass through N3After secondary Circularly liftable temperature step, coating failure stops test.
Preferably, in the accelerated test determination step, selecting third metal double polar plates is the tested of metal double polar plates
Sample;Wherein, the third metal double polar plates are the initial binding force F of measurementAThe Duplicate Samples of sample used in step;
The third metal double polar plates are the measurement binding force FBThe Duplicate Samples of sample used in step.
Preferably, second set temperature is 40~260 DEG C, preferably 120~200 DEG C;And/or
Second setting time is 30s~10min, preferably 1~5min;And/or
The third set temperature is -10~20 DEG C, preferably -5~5 DEG C, further preferably 0 DEG C.
Preferably, in the step of temperature difference resistance can be assessed, including the metal double polar plates are calculated using the following equation out
The start-stop time of resistance to temperature difference N the step of:
N=N3×S;
Wherein, S is the accelerated ratio in the accelerated test determination step, and calculation formula is as follows:
S=(Δ2/Δ1)×(N1/N2);
Wherein, Δ2=FA-FC, Δ1=FA-FB。
Preferably, using the binding force of coating and metal substrate in scratching instrument measurement metal double polar plates.
Compared with prior art, the measuring method of metal double polar plates temperature difference resistance energy of the invention at least has following beneficial
Effect:
The measuring method of metal double polar plates temperature difference resistance energy provided in an embodiment of the present invention, according to metal double polar plates floating coat
Initial combination power, simulation metal double polar plates with fuel cell discontinuous operation undergo difference variation N1Coating after secondary combines
Power, to assess the long-term temperature difference resistance energy of metal double polar plates;The measuring method shortens commenting for metal double polar plates temperature difference resistance energy
Estimate the period and be measured it is not necessary that metal double polar plates are fitted into fuel cell, sensing equipment simply, be greatly lowered cost,
Improve determination efficiency.
Further, the measuring method of metal double polar plates temperature difference resistance energy provided in an embodiment of the present invention, it is double according to metal
The initial combination power of pole plate floating coat simulates metal double polar plates as fuel cell discontinuous operation undergoes difference variation N1Painting afterwards
Layer binding force, estimates the start-stop time of resistance to temperature difference N of metal double polar plates;The evaluation method further shortens the metal double polar plates longevity
The assessment cycle of life.
Further, the measuring method of metal double polar plates temperature difference resistance energy provided in an embodiment of the present invention is with specific reference to metal
The initial combination power of bipolar plates floating coat simulates metal double polar plates as fuel cell discontinuous operation undergoes difference variation N1Afterwards
Coating binding force, accelerated test determination step, evaluation method go out the start-stop time of resistance to temperature difference N of metal double polar plates;The evaluation method
Further shorten the assessment cycle in metal double polar plates service life.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, with presently preferred embodiments of the present invention, detailed description is as follows below.
Specific embodiment
It is of the invention to reach the technical means and efficacy that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Preferred embodiment, to specific embodiment, structure, feature and its effect applied according to the present invention, detailed description is as follows.Under
It states in bright, what different " embodiment " or " embodiment " referred to is not necessarily the same embodiment.In addition, one or more embodiments
In special characteristic, structure or feature can be combined by any suitable form.
Embodiment 1
The present embodiment provides a kind of measuring methods of metal double polar plates temperature difference resistance energy specifically to include the following steps:
Measure initial binding force FA: determine the initial binding force F of the coating and metal substrate in metal double polar platesA。
Measure binding force FB: it simulates in the working environment of metal double polar plates in a fuel cell and simulates metal pair
Pole plate undergoes difference variation with fuel cell discontinuous operation;Simulate discontinuous operation N1After secondary, determine in metal double polar plates
The binding force F of coating and metal substrateB。
Temperature difference resistance can be assessed: according to FA、FB、N1Predict the start-stop time of resistance to temperature difference of metal double polar plates.
Preferably, measuring initial binding force FAStep, measurement binding force FBIt is parallel tested with two respectively in step
Sample (so-called Duplicate Samples refer to the identical sample of structure, material), i.e. the first metal double polar plates are (as the initial knot of measurement
Resultant force FAThe sample of step) and the second metal double polar plates (measure initial binding force FBStep).
Preferably, measuring initial binding force FAThe step of, specifically: selecting the first metal double polar plates is metal double polar plates
Sample;Oil removing is carried out to the first metal double polar plates with alcohol to clean, then is cleaned by ultrasonic completely with pure water, is dried with nitrogen.It is more
The binding force of coating and metal substrate in the first metal double polar plates of secondary measurement, is averaged, obtains the painting in metal double polar plates
The initial binding force F of layer and metal substrateA。
Preferably, the measurement binding force FBThe step of, include the following steps:
1) selecting the second metal double polar plates is the sample of metal double polar plates, is carried out with alcohol to the second metal double polar plates
Oil removing cleaning, then be cleaned by ultrasonic completely with pure water, it is dried with nitrogen.
2) the second metal double polar plates are put into the container for being loaded with simulated solution;Wherein, the simulated solution is simulation
The solution of the working environment of metal double polar plates in a fuel cell.
Preferably, in this step, the simulated solution is that pH is 2~3, containing 2~5ppm fluorine ion and is passed through hydrogen
Or the sulfuric acid solution of oxygen.
3) after so that the second metal double polar plates is impregnated the first setting time in the simulated solution of the first set temperature, then make institute
State simulated solution cooled to room temperature;Wherein, first set temperature is the metal double polar plates in actual work
Temperature.
Preferably, in this step, the first setting time is 30s~10min, preferably 1~5min, further preferably
5min.First set temperature is 60~90 DEG C, preferably 75~85 DEG C, further preferably 80 DEG C.
4) step 3) N is repeated1After secondary, the second metal double polar plates are taken out, measure coating and gold in the second metal double polar plates
The binding force for belonging to substrate, obtains binding force FB。
Here, N1Number without clearly requiring, but must guarantee the F measuredBBe worth it is genuine and believable, avoid measurement error from causing
Final assessed value deviates actual result.Preferably, by N1F is measured after secondaryBValue needs so that Δ1/FA>=1%, it is preferred that Δ1/
FA>=2%, it is further preferred that Δ1/FA≤ 5%;Wherein, Δ1=FA-FB。
The measuring method of metal double polar plates temperature difference resistance energy provided in this embodiment, with specific reference to metal double polar plates floating coat
Initial combination power, simulation metal double polar plates with fuel cell discontinuous operation undergo difference variation N1Coating after secondary combines
Power, to assess the long-term temperature difference resistance energy of metal double polar plates;The measuring method shortens commenting for metal double polar plates temperature difference resistance energy
Estimate the period and be measured it is not necessary that metal double polar plates are fitted into fuel cell, sensing equipment simply, be greatly lowered cost,
Improve determination efficiency.
Embodiment 2
Preferably, the present embodiment provides a kind of measuring methods of metal double polar plates temperature difference resistance energy, with upper embodiment phase
Than, in the temperature difference resistance energy appraisal procedure of the present embodiment, the resistance to temperature difference start and stop including calculating metal double polar plates by formula (1)
Times N:
N=(FA-F0)/(FA-FB)×N1Formula (1);
In formula (1), F0For preset critical;When the binding force of coating and metal substrate is less than or equal to F0When, it is believed that
Coating failure;Preferably, F0For 25~27N, further preferably 25N.
The present embodiment with specific reference to metal double polar plates floating coat initial combination power, simulation metal double polar plates with fuel electricity
Pond discontinuous operation undergoes difference variation N1Coating binding force afterwards, evaluation method go out the start-stop time of resistance to temperature difference N of metal double polar plates;
The evaluation method further shortens the assessment cycle in metal double polar plates service life.
Embodiment 3
Preferably, the present embodiment provides a kind of measuring methods of metal double polar plates temperature difference resistance energy, with above-described embodiment phase
Than the measuring method of the present embodiment is further improved as follows:
In the measurement binding force FBThe step of after, further include accelerating before temperature difference resistance the step of capable of assessing
Test determination step.Wherein, the accelerated test determination step includes:
1) heating and cooling step: after metal double polar plates are heated to the second set temperature, after keeping the second setting time, then will
The metal double polar plates are put into the simulated solution of third set temperature, impregnate third setting time.
Wherein, second set temperature is greater than the actual work temperature of metal double polar plates;The simulated solution is simulation
The solution of the working environment of metal double polar plates in a fuel cell, specific ingredient is referring to embodiment 1.
Preferably, in this step, second set temperature is 40~260 DEG C, preferably 120~200 DEG C.Second sets
It fixes time as 30s~10min, preferably 1~5min.Third set temperature be -10~20 DEG C, preferably -5~5 DEG C, further
Preferably 0 DEG C.
2) binding force F is measuredC: repeat the heating and cooling step N2It is secondary, determine coating and Metal Substrate in metal double polar plates
The binding force F of plateC。
Here, N2Number without clearly requiring, but must guarantee the F measuredCBe worth it is genuine and believable, avoid measurement error from causing
Final assessed value deviates actual result.Preferably, by N2F is measured after secondaryCValue is so that Δ2/FA>=1%, preferably Δ2/FA≥
2%, preferred Δ2/FA≤ 5%;Wherein, Δ2=FA-FC。
3) terminate test: metal double polar plates pass through N3After secondary Circularly liftable temperature step, coating failure stops test.
Preferably, selecting third metal double polar plates is the sample of metal double polar plates in accelerated test determination step;
Wherein, third metal double polar plates are the Duplicate Samples of the first metal double polar plates, the second metal double polar plates.
Preferably, according to the accelerated test step that the present embodiment increases newly, correspondingly, the step of temperature difference resistance can be assessed
In, the calculation formula of the start-stop time of resistance to temperature difference N of metal double polar plates is as follows:
N=N3× S formula (2);
In formula (2), S is the accelerated ratio in the accelerated test determination step, and calculation formula is as follows:
S=(Δ2/Δ1)×(N1/N2) formula (3);
In formula (3), Δ2=FA-FC, Δ1=FA-FB。
The measuring method of metal double polar plates temperature difference resistance energy provided in this embodiment is with specific reference to metal double polar plates floating coat
Initial combination power, simulation metal double polar plates with fuel cell discontinuous operation undergo difference variation N1Rear coating binding force,
Accelerated test determination step, evaluation method go out the start-stop time of resistance to temperature difference N of metal double polar plates;The evaluation method further shortens
The assessment cycle in metal double polar plates service life.
Preferably, in above-described embodiment, main coating and metal substrate using in scratching instrument measurement metal double polar plates
Binding force.
It is further described below by specific EXPERIMENTAL EXAMPLE as follows:
EXPERIMENTAL EXAMPLE 1
1) take it is long × wide be 20mm × 20mm 3 pieces of identical metal double polar plates, be respectively defined as the first metal bipolar
Plate, the second metal bipolar, third metal double polar plates;And by after the cleaning of above 3 pieces of metal double polar plates, with being dried with nitrogen.
2) binding force of the coating and metal substrate in the first metal double polar plates is repeatedly measured, and is averaged FA=
47.4N。
3) the second metal double polar plates are put into in the container being loaded in 80 DEG C of simulated solution (wherein, simulated solution is
PH=2, fluorinion concentration 2ppm, the sulfuric acid solution for being passed through 20ml/min hydrogen), after 5min, beaker is transferred to room temperature shape
Cooled to room temperature under state.
4) it repeats step 3) 1500 times, takes out the second metal double polar plates and measure the second metal double polar plates after cleaning, drying
In coating and metal substrate binding force FB=46.3N.
5) the metal double polar plates start-stop time of resistance to temperature difference N is calculated:
N=(47.4-25)/(47.4-46.3) × 1500=30545 times.
EXPERIMENTAL EXAMPLE 2
1) take it is long × wide be 20mm × 20mm 3 pieces of identical metal double polar plates, be respectively defined as the first metal bipolar
Plate, the second metal bipolar, third metal double polar plates;And by after the cleaning of above 3 pieces of metal double polar plates, with being dried with nitrogen.
2) binding force of the coating and metal substrate in the first metal double polar plates is repeatedly measured, and is averaged FA=
48.3N。
3) the second metal double polar plates are put into in the container being loaded in 80 DEG C of simulated solution (wherein, simulated solution is
PH=2, fluorinion concentration 2ppm, the sulfuric acid solution for being passed through 20ml/min hydrogen), after 5min, beaker is transferred to room temperature shape
Cooled to room temperature under state.
4) it repeats step 3) 2000 times, takes out the second metal double polar plates and measure the second metal double polar plates after cleaning, drying
In coating and metal substrate binding force FB=46.1N.
5) the metal double polar plates start-stop time of resistance to temperature difference N is calculated:
N=(48.3-25)/(48.3-46.1) × 2000=21182 times.
EXPERIMENTAL EXAMPLE 3
1) take it is long × wide be 20mm × 20mm 3 pieces of identical metal double polar plates, be respectively defined as the first metal bipolar
Plate, the second metal bipolar, third metal double polar plates;And by after the cleaning of above 3 pieces of metal double polar plates, with being dried with nitrogen.
2) binding force of the coating and metal substrate in the first metal double polar plates is repeatedly measured, and is averaged FA=44N.
3) the second metal double polar plates are put into the container being loaded in 80 DEG C of simulated solution (wherein, pH=2, fluorine from
Sub- concentration is 2ppm, temperature is 80 DEG C, is passed through the sulfuric acid solution of 20ml/min hydrogen), after 5min, beaker is transferred to room temperature shape
Cooled to room temperature under state.
4) it repeats step 3) 2400 times, takes out the second metal double polar plates and measure the second metal double polar plates after cleaning, drying
In coating and metal substrate binding force FB=42.8N.
5) third metal plate is put into baking oven and is heated to 180 DEG C and stablizes 10min, then take out third metal double polar plates
Be put into 0 DEG C of simulated solution (simulated solution pH=2, fluorinion concentration 2ppm, be passed through 20ml/min hydrogen sulfuric acid it is molten
Liquid) impregnate 5min.
6) it repeats step 5) 30 times, after third metal double polar plates are cleaned up, measures the painting in third metal double polar plates
The binding force of layer and metal substrate is Fc=43.0N.
7) there is coating shedding phenomenon after repeating step 660 time altogether, stop test.
8) the metal double polar plates start-stop time of resistance to temperature difference N is calculated:
N=N3× S=N3×(Δ2/Δ1)×(N1/N2)=660 × (1/1.2) × (2400/30)=44000 time.
To sum up, the measuring method of metal double polar plates temperature difference resistance energy provided in an embodiment of the present invention, according to metal double polar plates
The initial combination power of floating coat simulates metal double polar plates as fuel cell discontinuous operation undergoes difference variation N1Coating after secondary
Binding force, to assess the long-term temperature difference resistance energy of metal double polar plates;The measuring method shortens metal double polar plates temperature difference resistance energy
Assessment cycle and be measured it is not necessary that metal double polar plates are fitted into fuel cell, sensing equipment simply, be greatly lowered into
Originally, determination efficiency is improved.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, according to
According to technical spirit any simple modification, equivalent change and modification to the above embodiments of the invention, this hair is still fallen within
In the range of bright technical solution.