# US 11,999,011 B1 · In situ alloying

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- Number: US 11,999,011 B1
- Document ID: US11999011B1
- Status: Granted
- Kind: B1
- Application number: 16/593,431
- Filed: 2019-10-04
- Granted: 2024-06-04
- Earliest claimed: 2019-10-04
- Assignees: Wisconsin Alumni Research Foundation
- Applicants: Wisconsin Alumni Research Foundation
- Inventors: Michael Joseph Moorehead; Adrien Couet; Dan J. Thoma
- Web page: https://patentgrep.com/patent/US11999011B1

## CPC

- B23K 26/342: Build-up welding
- B22F 1/09: {Mixtures of metallic powders}
- B22F 10/25: Direct deposition of metal particles, e.g. direct metal deposition [DMD] or laser engineered net shaping [LENS]
- B22F 12/53: Nozzles
- B22F 12/55: Two or more means for feeding material
- B22F 12/57: Metering means
- B22F 12/58: for changing the material composition, e.g. by mixing
- B23K 26/1464: {Supply to, or discharge from, nozzles of media, e.g. gas, powder, wire}
- B23K 26/147: {Features outside the nozzle for feeding the fluid stream towards the workpiece}
- B33Y 10/00: Processes of additive manufacturing
- B33Y 30/00: Apparatus for additive manufacturing; Details thereof or accessories therefor
- B33Y 50/02: for controlling or regulating additive manufacturing processes
- B33Y 70/00: Materials specially adapted for additive manufacturing
- C22C 1/04: by powder metallurgy (C22C1/08 takes precedence)
- B23K 2103/18: Dissimilar materials
- B23K: SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B22F: WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER (making alloys by powder metallurgy C22C); APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B33Y: ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- C22C: ALLOYS (treatment of alloys C21D, C22F)

## Abstract

As may be implemented in accordance with one or more approaches herein, a plurality of metal alloy samples are formed on a surface, in which each sample has a different metal alloy composition relative to the others. Elemental metal powders are provided from hoppers at respective delivery rates and mixed, such that the mixture for each sample is set via the respective delivery rates and is different than the mixture for the other samples. Multiple layers of each mixture are deposited by dispensing and melting the mixture to form the respective samples, and one or more layer of each of the samples is remelted

## Claims

### Claim 1

A method comprising:
dispensing metal-based material from a plurality of material sources, each source operable to dispense the metal-based material at a variable rate;
mixing the metal-based material dispensed by the plurality of material sources, and conveying the mixed metal-based material using a material conduit coupled to the plurality of material sources; and
using a deposition tool coupled to receive the mixed metal-based material via the material conduit, the deposition tool having control circuitry, a nozzle, and an energy source, to:
deposit layers of a first combination of the materials on a substrate surface by: supplying a mixture of the first combination of materials from the plurality of material sources, conveying the mixture to the deposition tool via the material conduit, dispensing the first combination of materials from the nozzle, and melting a first portion of the dispensed materials via the energy source, each layer having a second portion of the dispensed materials that remains unmelted,
remelt a top one of the deposited layers via the energy source, including melting the second portion of the dispensed materials in the top layer, and
deposit layers of a second combination of materials relative to the surface, the second combination being different than the first combination, by: adjusting the rate at which at least one of the material sources dispenses metal-based material, supplying a mixture of the second combination of materials from the plurality of material sources via the adjusted rate, conveying the mixture of the second combination of materials to the deposition tool via the material conduit, dispensing the second combination of materials from the nozzle, melting the dispensed materials via the energy source, and remelting a top one of the deposited layers.

### Claim 2 (depends on 1)

The method of claim 1, wherein:
depositing the layers of the first combination of materials includes depositing a set of layers including a first layer deposited directly on the surface and at least a second layer deposited on the first layer;
the top layer is deposited on the set of layers; and
using the set of layers to prevent interdiffusion of material from the substrate into the top layer.

### Claim 3 (depends on 2)

The method of claim 2, wherein depositing the set of layers includes using a single melting of the material deposited for each layer in the set of layers.

### Claim 4 (depends on 1)

The method of claim 1, wherein depositing the layers of the first combination of materials and depositing the layers of the second combination of materials includes forming a plurality of discrete structures on the surface, each structure having a different composition relative to the other structures, by setting, for each of the plurality of discrete structures, a different rate of material delivered by one or more of the plurality of delivery sources, relative to the rate of material delivered by the one or more of the plurality of delivery sources for forming the other structures.

### Claim 5 (depends on 1)

The method of claim 1, wherein depositing the layers of the first combination of materials and depositing the layers of the second combination of materials includes forming a structure having a different composition of materials at different regions within the structure, and includes adjusting the rate of material delivered by at least one of the plurality of delivery sources while depositing and melting the material delivered to the deposition tool.

### Claim 6 (depends on 1)

The method of claim 1, wherein dispensing the metal-based material includes dispensing, from each material source, powdered metal-based material from a hopper in which each hopper has a different type of powdered metal-based material, using a mechanical component to deliver the powdered metal-based material from the hopper at a variable rate in response to a control input received from the control circuitry and adjusted for the first and second combination of materials.

### Claim 7 (depends on 1)

The method of claim 1, further including forming a structure in which regions of the structure subjected to stress are provided with a greater material strength relative to other regions of the structure, by dynamically adjusting the rate of material delivered by at least one of the plurality of material sources while melting the mixture of materials to form the structure.

### Claim 8 (depends on 1)

The method of claim 1, wherein depositing the layers of the first combination of materials and depositing the layers of the second combination of materials includes moving the nozzle relative to the layers while dispensing and melting the first and second combinations of materials with a laser.

### Claim 9

A method comprising:
forming a plurality of metal alloy samples on a surface, each sample having a metal alloy composition that is different than a metal alloy composition of the other samples, by, for each sample:
supplying elemental metal powders from a plurality of hoppers at respective delivery rates,
mixing the supplied elemental powders to create a mixture, the mixture for each sample being set via the respective delivery rates and being different than the mixture for the other samples, and
depositing multiple layers of the mixture by dispensing and melting the mixture; and
for each sample, remelting a top one of the multiple layers.

### Claim 10 (depends on 9)

The method of claim 9, wherein depositing the multiple layers of the mixture includes depositing a set of layers underlying the top layer and depositing the top layer on the set of layers, the set of layers having a thickness sufficient to prevent interdiffusion of material from the substrate into the top layer.

### Claim 11 (depends on 10)

The method of claim 10, wherein depositing the set of layers and the top layer includes depositing a first layer of the set of layers on the surface, and depositing successive layers of the set of layers and the top layer without remelting any of the layers in the set of layers.

### Claim 12 (depends on 9)

The method of claim 9, wherein remelting a top layer of each of the samples includes reducing an amount of unmelted powder mixture and reducing porosity in the top layer.

### Claim 13 (depends on 9)

The method of claim 9, wherein supplying the elemental metal powders from the plurality of hoppers at respective delivery rates includes:
determining mass flow rate coefficients based on measurements of the mass of powder dispensed over a fixed time measured for a series of rotational speeds of an auger that dispenses the powder;
deriving a retention rate by depositing layers of different metal alloy compositions using respective combinations of the elemental powders, and performing least-squares error minimization of a difference between a measured chemical composition the deposited layers and a predicted composition of the deposited layers as a sum of the respective mass flow rates, qualified for the different metal alloy compositions;
predicting an atomic fraction of each element in deposited layers based on the retention rate and mass flow rate coefficients; and
controlling augers to dispense the elemental powders from the plurality of hoppers based on the predicted atomic fraction.

### Claim 14

An apparatus comprising:
a plurality of material sources configured to dispense metal-based material at a variable rate;
a material conduit coupled to the plurality of material sources and configured to receive and mix the metal-based material dispensed by the plurality of material sources, and to convey the mixed metal-based material; and
a deposition tool coupled to receive the mixed metal-based material via the material conduit, the deposition tool having control circuitry, a nozzle, and an energy source, and programmed and configured with the plurality of material sources to:
deposit layers of a first combination of the materials on a substrate surface by: supplying a mixture of the first combination of materials from the plurality of material sources, conveying the mixture to the deposition tool via the material conduit, dispensing the first combination of materials from the nozzle, and melting a first portion of the dispensed materials via the energy source, each layer having a second portion of the dispensed materials that remains unmelted,
remelt a top one of the deposited layers via the energy source, including melting the second portion of the dispensed materials in the top layer, and
deposit layers of a second combination of materials relative to the surface, the second combination being different than the first combination, by: adjusting the rate at which at least one of the material sources dispenses metal-based material, supplying a mixture of the second combination of materials from the plurality of material sources via the adjusted rate, conveying the mixture of the second combination of materials to the deposition tool via the metal conduit, dispensing the second combination of materials from the nozzle, melting the dispensed materials via the energy source, and remelting a top one of the deposited layers.

### Claim 15 (depends on 14)

The apparatus of claim 14, wherein the deposition tool is programmed and configured with the plurality of material sources to deposit the layers of the first combination of materials by depositing a set of layers including a first layer deposited directly on the surface and at least a second layer deposited on the first layer, the top layer being deposited on the set of layers, the set of layers being sufficiently thick to prevent interdiffusion of material from the substrate into the top layer.

### Claim 16 (depends on 15)

The apparatus of claim 15, wherein the deposition tool is programmed and configured with the plurality of material sources to deposit the set of layers using a single melting of the material deposited for each layer in the set of layers.

### Claim 17 (depends on 14)

The apparatus of claim 14, wherein the deposition tool is configured and arranged with the material sources to form a plurality of discrete structures on the surface, each structure having a different composition relative to the other structures, by setting, for each of the plurality of discrete structures, a different rate of material delivered by one or more of the plurality of delivery sources, relative to the rate of material delivered by the one or more of the plurality of delivery sources for forming the other structures.

### Claim 18 (depends on 14)

The apparatus of claim 14, wherein each material source includes a hopper containing powdered metal-based material, each hopper having a different type of powdered metal-based material, each material source having a mechanical component configured to deliver the powdered metal-based material from the hopper at a variable rate in response to a control input received from the control circuitry and adjusted for the first and second combination of materials.

### Claim 19 (depends on 14)

The apparatus of claim 14, wherein the deposition tool is configured and arranged with the plurality of material sources to form a structure having a different composition of materials at different regions within the structure, by adjusting the rate of material delivered by at least one of the plurality of delivery sources while depositing and melting the material delivered to the deposition tool.

### Claim 20 (depends on 14)

The apparatus of claim 14, wherein the deposition tool is configured and arranged with the plurality of material sources to form a structure in which regions of the structure subjected to stress are provided with a greater material strength relative to other regions of the structure, by dynamically adjusting the rate of material delivered by at least one of the plurality of material sources while melting the mixture of materials to form the structure.

### Claim 21 (depends on 9)

The method of claim 9, wherein for each sample, depositing the multiple layers of the mixture includes depositing a set of layers underlying the top layer by, for each layer in the set of layers, melting a first portion of the layer while leaving a second portion of the layer unmelted, prior to remelting the top one of the multiple layers.
