Autonomous inorganic material synthesis machine

Patent metadata

Field	Value
Publication number	US-2021350881-A1
Application number	US-202016868037-A
Country	US
Kind code	A1
Filing date	May 6, 2020
Priority date	May 6, 2020
Publication date	Nov 11, 2021
Grant date	—

Abstract

A synthesis machine for preparation of a targeted inorganic material for recommended synthesis by a computer program that determines optimal solid-state methods for synthesis of an inorganic material. The computational method involves inputting a target inorganic material, querying structural data and thermodynamic data for the target inorganic material, enumerating possible synthetic reactions to construct a synthetic reaction database with a viable subset of the possible synthetic methods. The routine generates a nucleation metric and competition metric that are combined to provide recommended synthetic methods. The output for each of the recommended syntheses are input into a robotic synthesis machine where the delivery of reactants, reaction conditions, and analysis of extent of reaction, and product quality is controlled by a processor.

First claim

What is claimed is:

1 . A synthesis machine for preparation of a target inorganic material, comprising:
a synthesis planner module coupled with a processor that outputs from a synthesis route recommendation computer program at least one solid-state synthetic method for the preparation of the target inorganic material, where the at least one solid-state synthetic method comprises a viable subset of a multiplicity of possible synthetic reactions; at least one reaction vessel for containment of at least one reactant for formation of the target inorganic material, wherein each reaction vessel is for the performance of a single solid-state synthetic method under a first stoichiometry and first set of conditions contained in the output of the computer program, or as an enumerated stoichiometry and enumerated set of conditions modified according to a result of a previous preparation of the target inorganic material by the synthesis machine, ultimately resulting from the first stoichiometry and first set of conditions; at least one delivery mechanism to provide a plurality of reactants to the reaction vessel, wherein a quantity of each of the plurality of reactants is provided at the first stoichiometry or in the enumerated stoichiometry; at least one controller configured for: controlling the first set of conditions or the enumerated set of conditions required for the solid-state synthetic method; monitoring the first set of conditions or the enumerated set of conditions during the solid-state synthetic method; and evaluating a progress of a reaction of the solid-state synthetic method.

2 . The synthesis machine according to claim 1 , wherein the recommended synthesis from the viable subset of the multiplicity of possible synthetic reactions is a synthesis with a calculated nucleation barrier metric and a competition metric that resides at or near an origin of a plot of the nucleation barrier metric vs. the competition metric or is on or near a pareto frontier of the plot for the target inorganic material input by a user, and wherein each recommended synthesis is separately input to the synthesis machine for syntheses.

3 . The synthesis machine according to claim 1 , wherein the computer program comprises at least one interface for the input of the target inorganic material by a user and/or by an inputting computer program.

4 . The synthesis machine according to claim 1 , wherein the delivery mechanism is computer controlled.

5 . The synthesis machine according to claim 1 , wherein the delivery mechanism comprises one or more of a powder dispensing technique, pipetting technique, ink-jet printing technique, spray pyrolysis technique, laser ablation technique, thermal evaporation technique; doping technique, chemical vapor deposition technique and gas flowing technique.

6 . The synthesis machine according to claim 1 , wherein the controller is coordinated with the synthesis planning module and imposes one or more reaction conditions according to the synthesis planner module with a signal imposed upon one or more of a heater, chiller, pressurizer, vacuum pump, and irradiators of laser, infrared, visible, or ultraviolet radiation.

7 . The synthesis machine according to claim 1 , wherein the controller coordinates monitoring of at least one in-situ probe of a thermistor, thermocouple, pressure gauge, balance, and an infrared camera attached to the reaction vessel, wherein a temperature, pressure, reaction mass, and visual depiction of a reaction mixture in the vessel are output to the processor.

8 . The synthesis machine according to claim 1 , wherein the controller coordinates monitoring one or more of temperature, pressure, mass, and ex-situ probes including diffractometers (such as an X-ray diffractometer), spectroscopic devices (such as an energy-dispersive spectroscopy device or X-ray fluorescence spectroscopy), calorimetric scanners (such as a differential scanning calorimetry), and optical or electron microscopes, results of which are output to synthesis planner's coupled processor.

9 . The synthesis machine according to claim 1 , further comprising a robotic sample transporter coupled to the controller for transporting a defined amount of the reaction mixture to one or more an ex-situ probe selected from a diffractometer, spectroscopic device, calorimetric scanner, optical microscope, or electron microscope.

10 . A method of synthesizing a target inorganic material, comprising:
a) receiving input for a recommended synthesis for a target inorganic material from a computer program for determining the recommended synthesis through an interface with a processor; b) transferring at least one reactant, and any desired diluent and catalyst, in a quantity prescribed by the computer program, to a reaction vessel; c) imposing, under computer control, a temperature, pressure, over gas, and/or radiation as prescribed by the computer program to the reaction vessel; d) monitoring, under computer control, at least one reaction condition; e) determining at least one condition and/or an extent of a reaction to a product inorganic material using at least one sensor with an output to the processor; f) determining a presence and a purity of the product inorganic material by at least one analytical technique controlled by the processor; and g) isolating, under computer control, the target inorganic material formed.

11 . The method according to claim 10 , wherein the input for the recommended synthesis for a target inorganic material is from a viable subset of a multiplicity of possible synthetic reactions having a calculated nucleation barrier metric and a competition metric that resides at or near an origin or on or near a pareto front of a plot of the nucleation barrier metric vs. the competition metric, as defined by a user for the target inorganic material, and wherein each of the recommended synthesis is separately input to a synthesis machine for syntheses.

12 . The method according to claim 10 , further comprising repeating steps a) through g) one or more times where the computer program provides a ranking of a viable subset of viable reactions where the input for the recommended synthesis for the target inorganic material are performed sequentially in the order of the ranking.

13 . The method according to claim 10 , wherein the transferring of the at least one reactant is performed by one or more of a powder dispensing technique, pipetting technique, ink-jet printing technique, spray pyrolysis technique, laser ablation technique, electron beam technique, thermal evaporation technique; doping technique; chemical vapor deposition technique and gas flowing technique.

14 . The method according to claim 10 , wherein the step of imposing the pressure comprises using an over gas, a press, or die and anvil.

15 . The method according to claim 10 , wherein the step of imposing the temperature comprises using a heater, radiant source of heating, and/or a chiller.

16 . The method according to claim 10 , wherein the step of monitoring at least one reaction condition comprises using any of thermal gauges, thermometers, thermocouples, pressure gauges, infrared cameras and probes for X-ray diffraction, energy-dispersive X-ray spectroscopy, X-ray fluorescence spectroscopy, differential scanning calorimetry, and optimal and electron microscopy.

17 . The method according to claim 10 , wherein the step of determining the extent of the reaction comprises measuring at least one of: X-ray diffraction spectra, energy-dispersive X-ray spectra, X-ray fluorescence spectra, differential

Assignees

• Toyota Res Inst Inc

Inventors

• Aykol Muratahan
• Suram Santosh K

Classifications

• B01J19/0013

  Controlling the temperature of the process · CPC title

• B01J2219/0022

  calculating difference · CPC title

• B01J19/0006

  Controlling or regulating processes (controlling or regulating in general G05) · CPC title

• B01J19/004

  Multifunctional apparatus for automatic manufacturing of various chemical products (sequential reactions B01J19/0046) · CPC title

• B01J2219/00243

  Mathematical modelling · CPC title