CN111896595B - A method for system integration of high-throughput preparation and high-throughput electrochemical testing - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 52
- 238000012360 testing method Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 16
- 230000010354 integration Effects 0.000 title abstract description 5
- 239000000376 reactant Substances 0.000 claims abstract description 17
- 238000000840 electrochemical analysis Methods 0.000 claims abstract description 13
- 238000005286 illumination Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 17
- 238000012512 characterization method Methods 0.000 abstract description 4
- 238000010353 genetic engineering Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 19
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 15
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 15
- FBEIPJNQGITEBL-UHFFFAOYSA-J tetrachloroplatinum Chemical compound Cl[Pt](Cl)(Cl)Cl FBEIPJNQGITEBL-UHFFFAOYSA-J 0.000 description 8
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 6
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 5
- 229910000033 sodium borohydride Inorganic materials 0.000 description 5
- 239000012279 sodium borohydride Substances 0.000 description 5
- 229910000531 Co alloy Inorganic materials 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- LMHKOBXLQXJSOU-UHFFFAOYSA-N [Co].[Ni].[Pt] Chemical compound [Co].[Ni].[Pt] LMHKOBXLQXJSOU-UHFFFAOYSA-N 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 229910002058 ternary alloy Inorganic materials 0.000 description 2
- KPZGRMZPZLOPBS-UHFFFAOYSA-N 1,3-dichloro-2,2-bis(chloromethyl)propane Chemical compound ClCC(CCl)(CCl)CCl KPZGRMZPZLOPBS-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- -1 chlorine Cobalt chloride Chemical compound 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000001073 sample cooling Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
Description
技术领域technical field
本发明涉及材料基因工程技术领域，具体涉及一种系统集成高通量制备和高通量电化学测试的方法，尤其涉及一种快速生成多种条件缩短材料研发周期的系统集成高通量制备和高通量电化学测试的方法。The invention relates to the technical field of material genetic engineering, in particular to a method for system-integrated high-throughput preparation and high-throughput electrochemical testing, and in particular to a system-integrated high-throughput preparation and method for rapidly generating multiple conditions and shortening the material development cycle. A method for high-throughput electrochemical testing.
背景技术Background technique
材料基因工程中，为了缩短材料研发周期，试样的高通量制备与表征是必不可少的研究环节。高通量制备与表征是以大数据作为支撑,采用高通量设计、制备和表征技术,促使材料研究从传统的试错模式转向低成本、快速响应的新模式,从而加快新材料的研发速度,实现研发成本和周期“双减半”的目标。In material genetic engineering, in order to shorten the material development cycle, high-throughput preparation and characterization of samples is an essential research link. High-throughput preparation and characterization is supported by big data, and adopts high-throughput design, preparation and characterization technologies to promote material research from the traditional trial-and-error mode to a low-cost, fast-response new mode, thereby speeding up the development of new materials , to achieve the goal of "double halving" R&D costs and cycles.
公告号为CN107153025A的中国发明专利公开了一种材料的高通量制备方法，其是将材料试样进行加热后保温，然后将保温后的材料试样保持原位并自保温后的材料试样的一端进行冷却，试样沿着纵向方向主要以热传导方式散热，冷却速率慢，因此试样从底部到顶部的冷却速率逐渐减小，从而在一个试样上实现一系列连续不同的冷却速率；进而得到具有不同微观组织和性能的材料集合体。The Chinese invention patent with the notification number CN107153025A discloses a high-throughput preparation method of a material, which is to heat the material sample and keep it warm, then keep the heat-insulated material sample in place and self-insulate the material sample Cooling at one end of the sample, the sample is mainly dissipated by heat conduction along the longitudinal direction, and the cooling rate is slow, so the cooling rate of the sample decreases gradually from the bottom to the top, so that a series of continuously different cooling rates can be realized on one sample; Furthermore, material aggregates with different microstructures and properties are obtained.
但是上述材料基因工程高通量得到的一系列连续不同的冷却速率条件不够精确，无法控制，实用价值不高。However, the series of continuous and different cooling rate conditions obtained by the high-throughput genetic engineering of the above-mentioned materials are not precise enough, uncontrollable, and of low practical value.
发明内容Contents of the invention
针对现有技术的缺陷，本发明的目的在于提供一种系统集成高通量制备和高通量电化学测试的方法。Aiming at the defects of the prior art, the purpose of the present invention is to provide a method for systematically integrating high-throughput preparation and high-throughput electrochemical testing.
本发明的目的是通过以下技术方案实现的：一种系统集成高通量制备和高通量电化学测试的方法，包括样品生成步骤、样品电化学测试步骤；The purpose of the present invention is achieved through the following technical solutions: a method for system integration of high-throughput preparation and high-throughput electrochemical testing, including a sample generation step and a sample electrochemical testing step;
所述样品生成步骤包括N级高通量制备步骤得到X组不同制备条件的样品，其中N大于或等于1，每级高通量制备步骤包括若干次平行的高通量制备操作；所述高通量制备操作具体包括：将若干反应物通过若干的条件发生器，生成若干组样品；所述条件发生器为生成某种条件梯度分布的仪器；The sample generation step includes N-level high-throughput preparation steps to obtain X groups of samples with different preparation conditions, wherein N is greater than or equal to 1, and each level of high-throughput preparation steps includes several parallel high-throughput preparation operations; The flux preparation operation specifically includes: passing several reactants through several condition generators to generate several groups of samples; the condition generator is an instrument that generates a certain condition gradient distribution;
所述样品电化学测试步骤包括对样品进行高通量电化学测试步骤。The sample electrochemical testing step includes a high-throughput electrochemical testing step for the sample.
优选地，所述高通量电化学测试步骤包括：对所述N级高通量制备步骤中得到的若干组不同制备条件的样品进行电化学测试，得到样品的电化学性能。Preferably, the high-throughput electrochemical testing step includes: performing electrochemical tests on several groups of samples obtained in the N-level high-throughput preparation step with different preparation conditions, to obtain the electrochemical performance of the samples.
优选地，当N大于1时，N-1级高通量制备步骤中高通量制备操作得到的样品为N级高通量制备步骤中高通量制备操作的反应物。Preferably, when N is greater than 1, the sample obtained from the high-throughput preparation operation in the N-1 level high-throughput preparation step is the reactant of the high-throughput preparation operation in the N-level high-throughput preparation step.
优选地，所述条件发生器包括浓度梯度发生器、温度梯度发生器、压强梯度发生器、电压梯度发生器、光照梯度发生器中的一种或多种。Preferably, the condition generator includes 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.
优选地，所述条件发生器数量大于或等于3个。Preferably, the number of condition generators is greater than or equal to three.
优选地，所述X大于或等于100。Preferably, said X is greater than or equal to 100.
优选地，所述N级高通量制备步骤得到X组不同制备条件的样品的周期小于或等于单个样品制备周期的X/5倍。Preferably, the period of obtaining X groups of samples with different preparation conditions in the N-level high-throughput preparation steps is less than or equal to X/5 times the preparation period of a single sample.
优选地，所述高通量电化学测试步骤同时对8个及以上样品进行电化学测试，得到电化学性能数据。比起重复X次单个样品的电化学测试，所述N级高通量电化学测试步骤得到X组样品的电化学测试数据周期具有时间成本上的优越性。Preferably, the high-throughput electrochemical testing step performs electrochemical testing on 8 or more samples at the same time to obtain electrochemical performance data. Compared with repeating the electrochemical test of a single sample for X times, the N-level high-throughput electrochemical test step to obtain the electrochemical test data cycle of the X group of samples has advantages in terms of time and cost.
综上所述，与现有技术相比，本发明具有如下的有益效果：In summary, compared with the prior art, the present invention has the following beneficial effects:
(1)快速完成大量样品的不同条件制备与性能测试，极大的缩短了材料研发周期；(1) Quickly complete the preparation and performance testing of a large number of samples under different conditions, which greatly shortens the material development cycle;
(2)能同时生成多种条件，支持复杂条件变化下的材料研发；(2) It can generate multiple conditions at the same time, supporting the research and development of materials under complex conditions;
(3)采用电化学测试的性能验证方法，数据直观易量化，方便对比；(3) The performance verification method of electrochemical test is adopted, the data is intuitive and easy to quantify, and it is convenient for comparison;
(4)制备出的样品几乎无损耗的进行后续测试，所得数据更为准确。(4) Subsequent tests are carried out on the prepared samples with almost no loss, and the obtained data are more accurate.
附图说明Description of drawings
通过阅读参照以下附图对非限制性实施例所作的详细描述，本发明的其它特征、目的和优点将会变得更明显：Other characteristics, objects and advantages of the present invention will become more apparent by reading the detailed description of non-limiting embodiments made with reference to the following drawings:
图1为本发明实施例2中一种系统集成高通量制备和高通量电化学测试的方法的流程图。Fig. 1 is a flow chart of a method for system integration of high-throughput preparation and high-throughput electrochemical testing in Example 2 of the present invention.
具体实施方式Detailed ways
以下实施例将有助于本领域的技术人员进一步理解本发明，但不以任何形式限制本发明。对本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变化和改进，这些都属于本发明的保护范围。在本文中所披露的范围的端点和任何值都不限于该精确的范围或值，这些范围或值应当理解为包含接近这些范围或值的值。对于数值范围来说，各个范围的端点值之间、各个范围的端点值和单独的点值之间，以及单独的点值之间可以彼此组合而得到一个或多个新的数值范围，这些数值范围应被视为在本文中具体公开，下面结合具体实施例对本发明进行详细说明：The following examples will help those skilled in the art to further understand the present invention, but do not limit the present invention in any form. Those of ordinary skill in the art can make several changes and improvements without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Neither the endpoints nor any values of the ranges disclosed herein are limited to such precise ranges or values, and these ranges or values are understood to include values approaching these ranges or values. For numerical ranges, between the endpoints of each range, between the endpoints of each range and individual point values, and between individual point values can be combined with each other to obtain one or more new numerical ranges, these values The scope should be regarded as specifically disclosed herein, and the present invention will be described in detail below in conjunction with specific examples:
实施例1Example 1
一种系统集成高通量制备和高通量电化学测试的方法，具体包括如下步骤：将50mL20％氯化镍溶液(反应物1)和50mL 20％氯化钴溶液(反应物2)加入条件发生器1中，本实施例中条件发生器1为一台浓度梯度发生器，它利用微流控原理将33mL 10％氯化镍溶液和33mL 10％氯化钴溶液分成20份5mL溶液，浓度分别为20％氯化镍、19％氯化镍1％氯化钴、18％氯化镍2％氯化钴……2％氯化镍18％氯化钴、1％氯化镍19％氯化钴、20％氯化钴。A method for system integration of high-throughput preparation and high-throughput electrochemical testing, specifically comprising the steps of: adding 50mL of 20% nickel chloride solution (reactant 1) and 50mL of 20% cobalt chloride solution (reactant 2) into the condition In generator 1, condition generator 1 is a concentration gradient generator in the present embodiment, and it utilizes microfluidic principle to divide 33mL 10% nickel chloride solution and 33mL 10% cobalt chloride solution into 20 parts of 5mL solution, concentration 20% nickel chloride, 19% nickel chloride, 1% cobalt chloride, 18% nickel chloride, 2% cobalt chloride... 2% nickel chloride, 18% cobalt chloride, 1% nickel chloride, 19% chlorine Cobalt chloride, 20% cobalt chloride.
将上述20份溶液加入条件发生器3中，本实施例中条件发生器3为一台温度梯度发生器，它能生成20℃、40℃、60℃、80℃、100℃五种温度梯度。条件发生器3将上述20份5mL溶液分为5组，每组20份1mL溶液，每组对应一个反应温度。Add the above 20 parts of the solution into the condition generator 3. The condition generator 3 in this embodiment is a temperature gradient generator, which can generate five temperature gradients of 20°C, 40°C, 60°C, 80°C, and 100°C. The condition generator 3 divides the above 20 parts of 5mL solution into 5 groups, each group has 20 parts of 1mL solution, and each group corresponds to a reaction temperature.
通过条件发生器1与条件发生器3对反应物1和反应物2的处理，获得了20种浓度梯度×5种温度梯度共100组不同的反应条件，将这些不同条件的反应物加入反应釜中利用5M硼氢化钠进行还原，可以获得100种不同反应条件下的100种不同的产物，在本实施例中即为100种不同成分形貌的镍钴合金。Through the treatment of reactant 1 and reactant 2 by condition generator 1 and condition generator 3, a total of 100 different reaction conditions of 20 concentration gradients × 5 temperature gradients were obtained, and these reactants with different conditions were added to the reactor 5M sodium borohydride is used for reduction, and 100 different products under 100 different reaction conditions can be obtained, which are 100 nickel-cobalt alloys with different composition and morphology in this embodiment.
对这100种镍钴合金进行电化学测试，即可得到100份电化学测试结果，再从中挑选出符合性能要求的镍钴合金，即得到满足该次性能要求的镍钴合金最佳反应条件。Perform electrochemical tests on these 100 kinds of nickel-cobalt alloys to obtain 100 electrochemical test results, and then select the nickel-cobalt alloys that meet the performance requirements, and then obtain the optimal reaction conditions for the nickel-cobalt alloys that meet the performance requirements.
实施例2：Example 2:
如图1所示，一种系统集成高通量制备和高通量电化学测试的方法，具体包括如下步骤：一种系统集成高通量制备和高通量电化学测试的方法，具体包括如下步骤：将50mL20％氯化镍溶液(反应物1)和50mL 4mM四氯化铂溶液(反应物2)加入条件发生器1中，本实施例中条件发生器1为一台浓度梯度发生器，它利用微流控原理将20％氯化镍溶液和4mM四氯化铂溶液分成5份、每份20mL不同浓度的溶液，浓度分别为20％氯化镍、15％氯化镍1mM四氯化铂、10％氯化镍2mM四氯化铂、5％氯化镍3mM四氯化铂、4mM四氯化铂。As shown in Figure 1, a method for systematically integrating high-throughput preparation and high-throughput electrochemical testing specifically includes the following steps: a method for systematically integrating high-throughput preparation and high-throughput electrochemical testing specifically includes the following steps Step: 50mL20% nickel chloride solution (reactant 1) and 50mL 4mM platinum tetrachloride solution (reactant 2) are added in condition generator 1, and condition generator 1 is a concentration gradient generator in the present embodiment, It uses the principle of microfluidics to divide 20% nickel chloride solution and 4mM platinum tetrachloride solution into 5 parts, each 20mL solution with different concentrations, the concentrations are 20% nickel chloride, 15% nickel chloride and 1mM tetrachloride Platinum, 10% nickel chloride 2mM platinum tetrachloride, 5% nickel chloride 3mM platinum tetrachloride, 4mM platinum tetrachloride.
将2mL的5M硼氢化钠溶液(反应物3，硼氢化钠作为还原剂)加入条件发生器2中，本实施例中条件发生器2为一台浓度梯度发生器，它能够将5M四氯化铂溶液稀释为4种浓度，分别为1M、2M、3M、4M。将4种浓度的硼氢化钠溶液与5种浓度的氯化镍、四氯化铂混合溶液依次混合，得到20种不同浓度的硼氢化钠、氯化镍、四氯化铂混合溶液。2mL of 5M sodium borohydride solution (reactant 3, sodium borohydride as reducing agent) is added in condition generator 2, and condition generator 2 is a concentration gradient generator in the present embodiment, and it can 5M tetrachloride The platinum solution was diluted to 4 concentrations, namely 1M, 2M, 3M and 4M. Four concentrations of sodium borohydride solutions were mixed with five concentrations of nickel chloride and platinum tetrachloride mixed solutions in sequence to obtain 20 different concentrations of sodium borohydride, nickel chloride and platinum tetrachloride mixed solutions.
将上述20份溶液加入条件发生器3中，本实施例中条件发生器3为一台温度梯度发生器，它能生成20℃、40℃、60℃、80℃、100℃五种温度梯度。条件发生器3将上述20份溶液分为5组，每组对应一个反应温度。Add the above 20 parts of the solution into the condition generator 3. The condition generator 3 in this embodiment is a temperature gradient generator, which can generate five temperature gradients of 20°C, 40°C, 60°C, 80°C, and 100°C. The condition generator 3 divides the above 20 solutions into 5 groups, and each group corresponds to a reaction temperature.
通过条件发生器1、条件发生器2与条件发生器3对反应物1、反应物2和反应物3的处理，获得了5种浓度梯度×4种还原剂浓度×5种温度梯度共100组不同的反应条件，将这些不同条件的反应物加入反应釜中，可以获得100种不同反应条件下的100种不同的产物，在本实施例中即为100种不同成分形貌的铂钴镍三元合金。Through the treatment of reactant 1, reactant 2 and reactant 3 by condition generator 1, condition generator 2 and condition generator 3, a total of 100 groups of 5 concentration gradients × 4 reducing agent concentrations × 5 temperature gradients were obtained Different reaction conditions, adding these reactants under different conditions into the reactor, can obtain 100 different products under 100 different reaction conditions, in this embodiment, it is 100 kinds of platinum-cobalt-nickel-tri Yuan alloy.
对这100种铂钴镍三元合金进行电化学测试，即可得到100份电化学测试结果，再从中挑选出符合性能要求的铂钴镍三元合金，即得到满足该次性能要求的镍钴合三元金最佳反应条件。Perform electrochemical tests on these 100 platinum-cobalt-nickel ternary alloys to obtain 100 electrochemical test results, and then select the platinum-cobalt-nickel ternary alloys that meet the performance requirements, that is, obtain the nickel-cobalt that meets the performance requirements. The best reaction conditions for ternary gold.
以上对本发明的具体实施例进行了描述。需要理解的是，本发明并不局限于上述特定实施方式，本领域技术人员可以在权利要求的范围内做出各种变化或修改，这并不影响本发明的实质内容。在不冲突的情况下，本申请的实施例和实施例中的特征可以任意相互组合。Specific embodiments of the present invention have been described above. It should be understood that the present invention is not limited to the specific embodiments described above, and those skilled in the art may make various changes or modifications within the scope of the claims, which do not affect the essence of the present invention. In the case of no conflict, the embodiments of the present application and the features in the embodiments can be combined with each other arbitrarily.
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