Method for producing material libraries by means of electrochemical deposition
View Patent ↗The invention relates to a method for combinatorially producing a library of materials by means of an electrochemical deposition in an array. The inventive library is made from an array of containers that consist of an electroconductive material, are open to the top and are electroconductively connected to a shared current supply device and is made from a corresponding array of auxiliary electrodes that are electroconductively connected to a shared current supply device and are arranged in such a way that an auxiliary electrode plunges into a container respectively or can be introduced therein without touching said container. The inventive method comprises the following steps: filling the containers with electrolytes having different compositions and containing electrolytically separable elements and applying an electric voltage between the current supply devices of the containers and auxiliary electrodes for obtaining an electrolytic deposition on the surfaces of the containers.
1. A process for combinatorial preparation of a material library by electrochemical deposition in an array which is formed of an array of open-top containers of electrically conducting material that are electrically connected to a shared power supply and a corresponding array of auxiliary electrodes which are electrically connected to a shared power supply and are disposed in such a manner that in each case one auxiliary electrode can be immersed in, or introduced into, a container without contacting it, comprising the following steps:
filling the containers with electrolytes of differing composition which contain electrolytically depositable elements and
applying an electric voltage between the power supplies of the containers and auxiliary electrodes in order to cause electrolytic deposition on the surfaces of the containers.
2. The process as claimed in claim 1 , characterized in that pulsed electrolysis is used.
3. The process as claimed in claim 2 , characterized in that the electrolytes of differing composition are prepared in an automated manner by mixing predetermined amounts of solutions of the electrolytically depositable elements in one or more mixing vessels operated in parallel and subsequently transferring them into the containers of the array.
4. The process as claimed in claim 2 , characterized in that the electrolytes of differing composition are prepared in an automated manner by preparing solutions of the electrolytically depositable elements in separate storage vessels and simultaneously or sequentially metering predetermined amounts of the predetermined solutions into the individual containers.
5. A process for the combinatorial testing of material libraries which are obtained according to a process as claimed in claim 2 , in which
(1) when containers are presented, these are transferred to tubes open at both ends and the tubes are introduced as catalysts into different channels of a body which has a multiplicity of continuous parallel channels,
(2) if appropriate activation of the catalysts in the body,
(3) heating/cooling the body to a desired reaction temperature,
(4) passing a fluid reactant or a fluid reaction mixture through channels of the body,
(5) discharge of the reacted fluids from individual or a plurality of combined channels of the body,
(6) analysis of the discharged reacted fluids,
(7) if appropriate comparative evaluation of the analytical results of a plurality of analyses.
6. The process as claimed in claim 1 , characterized in that the electrolytes of differing composition are prepared in an automated manner by mixing predetermined amounts of solutions of the electrolytically depositable elements in one or more mixing vessels operated in parallel and subsequently transferring them into the containers of the array.
7. A process for the combinatorial testing of material libraries which are obtained according to a process as claimed in claim 6 , in which
(1) when containers are presented, these are transferred to tubes open at both ends and the tubes are introduced as catalysts into different channels of a body which has a multiplicity of continuous parallel channels,
(2) if appropriate activation of the catalysts in the body,
(3) heating/cooling the body to a desired reaction temperature,
(4) passing a fluid reactant or a fluid reaction mixture through channels of the body,
(5) discharge of the reacted fluids from individual or a plurality of combined channels of the body,
(6) analysis of the discharged reacted fluids,
(7) if appropriate comparative evaluation of the analytical results of a plurality of analyses.
8. The process as claimed in claim 1 , characterized in that the electrolytes of differing composition are prepared in an automated manner by preparing solutions of the electrolytically depositable elements in separate storage vessels and simultaneously or sequentially metering predetermined amounts of the predetermined solutions into the individual containers.
9. A process for the combinatorial testing of material libraries which are obtained according to a process as claimed in claim 8 , in which
(1) when containers are presented, these are transferred to tubes open at both ends and the tubes are introduced as catalysts into different channels of a body which has a multiplicity of continuous parallel channels,
(2) if appropriate activation of the catalysts in the body,
(3) heating/cooling the body to a desired reaction temperature,
(4) passing a fluid reactant or a fluid reaction mixture through channels of the body,
(5) discharge of the reacted fluids from individual or a plurality of combined channels of the body,
(6) analysis of the discharged reacted fluids,
(7) if appropriate comparative evaluation of the analytical results of a plurality of analyses.
10. A process for the combinatorial testing of material libraries which are obtained according to a process as claimed in claim 1 , in which
(1) when containers are presented, these are transferred to tubes open at both ends and the tubes are introduced as catalysts into different channels of a body which has a multiplicity of continuous parallel channels,
(2) if appropriate activation of the catalysts in the body,
(3) heating/cooling the body to a desired reaction temperature,
(4) passing a fluid reactant or a fluid reaction mixture through channels of the body,
(5) discharge of the reacted fluids from individual or a plurality of combined channels of the body,
(6) analysis of the discharged reacted fluids,
(7) if appropriate comparative evaluation of the analytical results of a plurality of analyses.
11. The process as claimed in claim 10 , characterized in that, after heating/cooling the body to a first reaction temperature in step (3), the steps (4) to (7) are carried out successively for a plurality of different fluid reactants or fluid reaction mixtures, where in each case a purge step with a purge gas can be introduced, and then the body can be heated/cooled to a second reaction temperature and the preceding reactions can be repeated at this temperature.
12. A process for combinatorial preparation of a material library by electrochemical deposition in an array formed of an array of tubes made of electrically conducting material which are open at both ends and are electrically connected to a shared power supply, a corresponding array of auxiliary electrodes which are electrically connected to a shared power supply and are disposed in such a manner that in each case one auxiliary electrode can be immersed in or introduced into a tube without contacting it, and a corresponding array of auxiliary electrode containers made of electrically conducting material which are connected to a shared power supply and which each enclose one tube, in which case there is no contact between the tubes on the one hand and the auxiliary electrodes and auxiliary electrode containers on the other, which process comprises the following steps:
filling the auxiliary electrode containers with electrolytes of differing composition that contain electrolytically depositable elements,
applying an electric voltage between the power supply of the tubes on the one hand and the power supplies of the auxiliary electrodes and auxiliary electrode containers on the other in order to cause electrolytic deposition on the surfaces of the tubes.
13. The process as claimed in claim 12 , characterized in that pulsed electrolysis is used.
14. The process as claimed in claim 12 , characterized in that the electrolytes of differing composition are prepared in an automated manner by mixing predetermined amounts of solutions of the electrolytically depositable elements in one or more mixing vessels operated in parallel and subsequently transferring them into the containers of the array.
15. The process as claimed in claim 12 , characterized in that the electrolytes of differing composition are prepared in an automated manner by preparing solutions of the electrolytically depositable elements in separate storage vessels and simultaneously or sequentially metering predetermined amounts of the predetermined solutions into the individual containers.
16. A process for the combinatorial testing of material libraries which are obtained according to a process as claimed in claim 12 , in which
(1) when containers are presented, these are transferred to tubes open at both ends and the tubes are introduced as catalysts into different channels of a body which has a multiplicity of continuous parallel channels,
(2) if appropriate activation of the catalysts in the body,
(3) heating/cooling the body to a desired reaction temperature,
(4) passing a fluid reactant or a fluid reaction mixture through channels of the body,
(5) discharge of the reacted fluids from individual or a plurality of combined channels of the body,
(6) analysis of the discharged reacted fluids,
(7) if appropriate comparative evaluation of the analytical results of a plurality of analyses.