CN111896595B - Method for system integration high-flux preparation and high-flux electrochemical test - Google Patents
Method for system integration high-flux preparation and high-flux electrochemical test Download PDFInfo
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- CN111896595B CN111896595B CN202010642504.9A CN202010642504A CN111896595B CN 111896595 B CN111896595 B CN 111896595B CN 202010642504 A CN202010642504 A CN 202010642504A CN 111896595 B CN111896595 B CN 111896595B
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The application discloses a method for system integration high-flux preparation and high-flux electrochemical test, and relates to the technical field of material genetic engineering; the method comprises a sample generation step and a sample electrochemical test step; the sample generation step comprises an N-level high-flux preparation step to obtain X groups of samples with different preparation conditions, wherein each level of high-flux preparation step comprises a plurality of parallel high-flux preparation operations; the high throughput preparation operation specifically includes: passing the plurality of reactants through a plurality of condition generators to generate a plurality of groups of samples; the sample electrochemical testing step comprises the step of carrying out high-flux electrochemical testing on the sample; the method for integrating high-flux preparation and high-flux electrochemical test by the system disclosed by the application can be used for carrying out rapid iteration on the preparation and test of materials and efficiently completing the preparation and characterization of a large number of materials.
Description
Technical Field
The application relates to the technical field of material genetic engineering, in particular to a method for preparing a system integrated high-flux and testing a high-flux electrochemical test, and especially relates to a method for preparing a system integrated high-flux and testing a high-flux electrochemical test, which can rapidly generate various conditions and shorten the research and development period of a material.
Background
In material genetic engineering, in order to shorten the material research and development period, high-throughput preparation and characterization of samples are indispensable research links. The high-throughput preparation and characterization are supported by big data, and the high-throughput design, preparation and characterization technology is adopted, so that the material research is promoted to be changed from a traditional error testing mode to a new mode with low cost and quick response, the research and development speed of the new material is accelerated, and the aim of 'double halving' of the research and development cost and period is fulfilled.
The chinese patent publication No. CN107153025a discloses a method for preparing a material with high flux, which comprises heating a material sample, preserving heat, then keeping the material sample in place after heat preservation, and cooling one end of the material sample after heat preservation, wherein the sample mainly dissipates heat in a heat conduction manner along a longitudinal direction, and the cooling rate is slow, so that the cooling rate of the sample from bottom to top is gradually reduced, thereby realizing a series of continuous different cooling rates on one sample; thus, a material aggregate having different microstructures and properties is obtained.
However, a series of continuous different cooling rate conditions obtained by the genetic engineering of the material are not accurate enough and cannot be controlled, and the practical value is not high.
Disclosure of Invention
In view of the shortcomings of the prior art, it is an object of the present application to provide a method for system integration of high-throughput preparation and high-throughput electrochemical testing.
The application aims at realizing the following technical scheme: a method for integrating high-flux preparation and high-flux electrochemical test by a system comprises a sample generation step and a sample electrochemical test step;
the sample generation step comprises an N-level high-flux preparation step to obtain X groups of samples with different preparation conditions, wherein N is greater than or equal to 1, and each high-flux preparation step comprises a plurality of parallel high-flux preparation operations; the high throughput preparation operation specifically comprises: passing the plurality of reactants through a plurality of condition generators to generate a plurality of groups of samples; the condition generator is used for generating a certain condition gradient distribution instrument;
the sample electrochemical testing step includes performing a high-throughput electrochemical testing step on the sample.
Preferably, the high-throughput electrochemical testing step comprises: and carrying out electrochemical tests on a plurality of groups of samples with different preparation conditions obtained in the N-level high-flux preparation step to obtain the electrochemical performance of the samples.
Preferably, when N is greater than 1, the sample obtained from the high-throughput preparation operation in the N-1 stage high-throughput preparation step is a reactant of the high-throughput preparation operation in the N-stage high-throughput preparation step.
Preferably, the condition generator comprises one or more of a concentration gradient generator, a temperature gradient generator, a pressure gradient generator, a voltage gradient generator, and an illumination gradient generator.
Preferably, the number of condition generators is greater than or equal to 3.
Preferably, X is greater than or equal to 100.
Preferably, the N-level high throughput preparation step results in X sets of samples of different preparation conditions having a period of less than or equal to X/5 times the period of a single sample preparation.
Preferably, the high-throughput electrochemical testing step is used for simultaneously performing electrochemical tests on 8 or more samples to obtain electrochemical performance data. The class N high throughput electrochemical test procedure results in an electrochemical test data cycle of X sets of samples with a temporal cost advantage over repeating the electrochemical test of X individual samples.
In summary, compared with the prior art, the application has the following beneficial effects:
(1) The preparation of a large number of samples under different conditions and the performance test are completed rapidly, so that the material research and development period is shortened greatly;
(2) Multiple conditions can be generated simultaneously, and material research and development under complex condition change is supported;
(3) The data is visual and easy to quantify by adopting a performance verification method of electrochemical test, and the comparison is convenient;
(4) The prepared sample is subjected to subsequent testing almost without loss, and the obtained data is more accurate.
Drawings
Other features, objects and advantages of the present application will become more apparent upon reading of the detailed description of non-limiting embodiments, given with reference to the accompanying drawings in which:
FIG. 1 is a flow chart of a method for integrating high-throughput preparation and high-throughput electrochemical testing for a system in example 2 of the present application.
Detailed Description
The following examples will assist those skilled in the art in further understanding the present application, but are not intended to limit the application in any way. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the spirit of the application. The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be obtained in combination with each other between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, and should be considered as specifically disclosed herein, the application is described in detail below in connection with the specific embodiments:
example 1
A method for integrating high-flux preparation and high-flux electrochemical test by a system specifically comprises the following steps: 50mL of 20% nickel chloride solution (reactant 1) and 50mL of 20% cobalt chloride solution (reactant 2) were added to the condition generator 1, and the condition generator 1 in this example was a concentration gradient generator which divides 33mL of 10% nickel chloride solution and 33mL of 10% cobalt chloride solution into 20 parts of 5mL of solutions with concentrations of 20% nickel chloride, 19% nickel chloride 1% cobalt chloride, 18% nickel chloride 2% cobalt chloride … …% nickel chloride 18% cobalt chloride, 1% nickel chloride 19% cobalt chloride, and 20% cobalt chloride by using the microfluidic principle.
The above 20 parts of the solution was added to the condition generator 3, and the condition generator 3 in this example was a temperature gradient generator capable of generating five temperature gradients of 20 ℃, 40 ℃, 60 ℃, 80 ℃ and 100 ℃. The condition generator 3 divides the above 20 parts of 5mL solution into 5 groups of 20 parts of 1mL solution each corresponding to one reaction temperature.
Through the treatment of the reactant 1 and the reactant 2 by the condition generator 1 and the condition generator 3, 100 groups of different reaction conditions of 20 concentration gradients multiplied by 5 temperature gradients are obtained, and the reactants with the different conditions are added into a reaction kettle to be reduced by using 5M sodium borohydride, so that 100 different products under 100 different reaction conditions can be obtained, namely 100 nickel-cobalt alloys with different component morphologies in the embodiment.
And (3) carrying out electrochemical test on the 100 nickel-cobalt alloys to obtain 100 parts of electrochemical test results, and then selecting the nickel-cobalt alloy meeting the performance requirement from the electrochemical test results to obtain the nickel-cobalt alloy optimal reaction condition meeting the performance requirement.
Example 2:
as shown in fig. 1, a method for integrating high-throughput preparation and high-throughput electrochemical testing by a system specifically comprises the following steps: a method for integrating high-flux preparation and high-flux electrochemical test by a system specifically comprises the following steps: 50mL of a 20% nickel chloride solution (reactant 1) and 50mL of a 4mM platinum tetrachloride solution (reactant 2) were added to the condition generator 1, and the condition generator 1 in this example was a concentration gradient generator which divides the 20% nickel chloride solution and the 4mM platinum tetrachloride solution into 5 parts of 20mL solutions of different concentrations of 20% nickel chloride, 15% nickel chloride 1mM platinum tetrachloride, 10% nickel chloride 2mM platinum tetrachloride, 5% nickel chloride 3mM platinum tetrachloride, and 4mM platinum tetrachloride, respectively, using the microfluidic principle.
2mL of a 5M sodium borohydride solution (reactant 3, sodium borohydride as the reducing agent) was added to the condition generator 2, and the condition generator 2 in this example was a concentration gradient generator capable of diluting the 5M platinum tetrachloride solution to 4 concentrations of 1M, 2M, 3M, and 4M, respectively. And sequentially mixing 4 sodium borohydride solutions with 5 nickel chloride and platinum tetrachloride mixed solutions to obtain 20 sodium borohydride, nickel chloride and platinum tetrachloride mixed solutions with different concentrations.
The above 20 parts of the solution was added to the condition generator 3, and the condition generator 3 in this example was a temperature gradient generator capable of generating five temperature gradients of 20 ℃, 40 ℃, 60 ℃, 80 ℃ and 100 ℃. The condition generator 3 divides the above 20 parts of solution into 5 groups, each group corresponding to one reaction temperature.
The reactant 1, the reactant 2 and the reactant 3 are treated by the condition generator 1, the condition generator 2 and the condition generator 3 to obtain 100 groups of different reaction conditions of 5 concentration gradients, 4 reducing agent concentrations and 5 temperature gradients, and 100 different products under 100 different reaction conditions can be obtained by adding the reactants under different conditions into a reaction kettle, namely 100 platinum cobalt nickel ternary alloys with different component morphologies in the embodiment.
And carrying out electrochemical test on the 100 platinum cobalt nickel ternary alloys to obtain 100 electrochemical test results, and then selecting the platinum cobalt nickel ternary alloys meeting the performance requirements from the electrochemical test results to obtain the nickel cobalt alloy ternary alloy optimal reaction conditions meeting the performance requirements.
The foregoing describes specific embodiments of the present application. It is to be understood that the application is not limited to the particular embodiments described above, and that various changes or modifications may be made by those skilled in the art within the scope of the appended claims without affecting the spirit of the application. The embodiments of the application and the features of the embodiments may be combined with each other arbitrarily without conflict.
Claims (1)
1. The method for integrating high-flux preparation and high-flux electrochemical testing by a system is characterized by comprising a sample generation step and a sample electrochemical testing step;
the sample generation step comprises an N-level high-flux preparation step to obtain X groups of samples with different preparation conditions, wherein N is greater than or equal to 1, and each high-flux preparation step comprises a plurality of parallel high-flux preparation operations; the high throughput preparation operation specifically comprises: passing the plurality of reactants through a plurality of condition generators to generate a plurality of groups of samples; the condition generator is used for generating a certain condition gradient distribution instrument;
the sample electrochemical testing step comprises the step of carrying out high-flux electrochemical testing on a sample;
the condition generator comprises one or more of a concentration gradient generator, a temperature gradient generator, a pressure gradient generator, a voltage gradient generator and an illumination gradient generator;
the number of the condition generators is more than or equal to 3;
the high-throughput electrochemical testing step comprises: carrying out electrochemical tests on a plurality of groups of samples with different preparation conditions obtained in the N-level high-flux preparation step to obtain the electrochemical performance of the samples; when N is larger than 1, the sample obtained by the high-flux preparation operation in the N-1 level high-flux preparation step is a reactant of the high-flux preparation operation in the N level high-flux preparation step;
x is greater than or equal to 100;
the cycle of the samples of X groups of different preparation conditions obtained by the N-level high-flux preparation step is less than or equal to 1/5 of the cycle of repeatedly preparing the samples of X times of single different preparation conditions;
and the high-flux electrochemical testing step is used for simultaneously carrying out electrochemical testing on 8 or more samples to obtain electrochemical performance data.
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| WO2018067802A1 (en) * | 2016-10-07 | 2018-04-12 | The Regents Of The University Of Michigan | Systems and methods for high throughput screening |
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