Patent US4836982A successfully refreshed from Google Patents.
US4836982A
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Rapid solidification of metal-second phase composites
Assignee: Lockheed Martin Corp
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Filing: 1986-06-13
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Granted: 1989-06-06
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Expires: 2006-06-13
Abstract
Abstract This invention relates to a process for making in-situ precipitated second phase in a metal matrix which mixture is rapidly solidified to form a product. The invention also relates to a rapidly solidified product.
Inventors
- 👤 John M. Brupbacher
- 👤 Leontios Christodoulou
- 👤 Dennis C. Nagle
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-02 14:12
CPC Classifications
C; C22; C22C; C22C1/00; C22C1/04; C22C1/05; C22C1/051; B; B22; B22F; B22F3/00; B22F3/23; B22F9/00; B22F9/02; B22F9/14; B23; B23K; B23K35/00; B23K35/22; B23K35/24; B23K35/32; B23K35/327; B23K35/40; B82; B82Y; B82Y30/00; C22C1/10; C22C1/1005; C22C1/1015; C22C1/1036; C22C1/1047; C22C1/1052; C22C1/1068; C22C29/00; C22C32/00; C22C32/0047; C22C32/0078; C22C47/00; C22C47/02; C22C47/06; C22C47/08; C22C49/00; C22C49/14; Y; Y10; Y10T; Y10T428/00; Y10T428/12; Y10T428/12486
Claims Analysis
Total Claims: 75
Claim 1
Independent Claim
147 words
A method for the production of metalsecond phase composition materials containing a second phase, said method comprising precipitating at least one second phase material in a metal matrix by contacting reactive second phase forming constituents, in the presence of a substantially non-reactive solvent matrix metal in which the second phase forming constituents are more soluble that the second phase, at a temperature at which sufficient diffusion of said constituents into the solvent matrix metal occurs, to cause reaction of the reactive second phase forming constituents to increase the temperature to a temperature exceeding the melting temperature of the matrix metal, to precipitate the second phase in the solvent matrix metal, rapidly quenching the metal-second phase composite material at a rate in the range of approximately 10 4 ° C. per second to 10 8 ° C. per second and recovering a rapidly solidified metal-second phase composite material.
Claim 2
Independent Claim
147 words
A method for the production of metalsecond phase composition materials containing a second phase, said method comprising precipitating at least one second phase material in a metal matrix by contacting reactive second phase forming constituents, in the presence of a substantially non-reactive solvent matrix metal in which the second phase forming constituents are more soluble that the second phase, at a temperature at which sufficient diffusion of said constituents into the solvent matrix metal occurs, to cause reaction of the reactive second phase forming constituents to increase the temperature to a temperature exceeding the melting temperature of the matrix metal, to precipitate the second phase in the solvent matrix metal, rapidly quenching the metal-second phase composite material at a rate in the range of approximately 10 4 ° C. per second to 10 8 ° C. per second and recovering a rapidly solidified metal-second phase composite material.
Claim 3
Dependent Claim
23 words
The method of claim 1, wherein the rapid quenching is accomplished by depositing the metal-second phase material against a rapidly moving quench surface.
Claim 4
Dependent Claim
20 words
The method of claim 1, wherein the rapid quenching is accomplished by atomizing the metal-second phase material to form droplets.
Claim 5
Dependent Claim
14 words
The method of claim 3, wherein said droplets are subjected to a coolant shower.
Claim 6
Dependent Claim
14 words
The method of claim 3, wherein said droplets are deposited in a cooling bath.
Claim 7
Dependent Claim
11 words
The method of claim 1, wherein the reaction is substantially complete.
Claim 8
Dependent Claim
22 words
The method of claim 1, wherein the reactive second phase forming constituents and the solvent metal are each provided as individual elements.
Claim 9
Dependent Claim
22 words
The method as set forth in claim 1, wherein the second phase forming constituents and the solvent metal are provided as powders.
Claim 10
Dependent Claim
24 words
The method of claim 1, wherein the second phase forming constituents and the solvent metal are provided as powders that are premixed and compacted.
Claim 11
Dependent Claim
11 words
The method of claim 1, wherein the second phase is particulate.
Claim 12
Dependent Claim
22 words
The method of claim 10, wherein the particulate second phase is titanium diboride, zirconium diboride, zirconium disilicide, titanium oxide, or titanium nitride.
Claim 13
Dependent Claim
13 words
The method of claim 11, wherein the second phase is submicron in size.
Claim 14
Dependent Claim
21 words
The method of claim 1, wherein the second phase forming constituents are each provided as an alloy of said solvent metal.
Claim 15
Dependent Claim
21 words
The method of claim 13, wherein the second phase forming constituents in the solvent matrix metal are contacted in stoichiometric proportions.
Claim 16
Dependent Claim
34 words
The method of claim 1, wherein at least one second phase forming constituent is provided as an alloy of the solvent metal, and the other second phase forming constituents are provided as individual elements.
Claim 17
Dependent Claim
23 words
The method of claim 1, wherein an additional alloying material is added to dioxidize the solvent metal matrix prior to the rapid quenching.
Claim 18
Dependent Claim
21 words
The method of claim 1, wherein additional alloying material is introduced to the solvent matrix metal prior to the rapid quenching.
Claim 19
Dependent Claim
23 words
The method of claim 17, wherein the concentration of the second phase is from about 0.1 to less than about 30 volume percent.
Claim 20
Dependent Claim
30 words
The method of claim 17, wherein the solvent metal matrix and the second phase forming constituents are added incrementally to the solvent matrix metal or alloy prior to rapid quenching.
Claim 21
Dependent Claim
27 words
The method of claim 17, wherein the solvent metal matrix with the second phase precipitated therein is added to a metal or alloy prior to rapid quenching.
Claim 22
Dependent Claim
27 words
The method of claim 1, wherein the solvent matrix metal with the second phase precipitated therein is added to a metal or alloy prior to rapid quenching.
Claim 23
Dependent Claim
21 words
The method of claim 21, wherein additional alloying material is introduced to the second phase containing material prior to rapid quenching.
Claim 24
Dependent Claim
30 words
The method of claim 1, wherein the solvent metal matrix and the second phase forming constituents are added incrementally to the solvent matrix metal or alloy prior to rapid quenching.
Claim 25
Dependent Claim
21 words
The method of claim 23, wherein additional alloying material is introduced to the second phase containing material prior to rapid quenching.
Claim 26
Dependent Claim
12 words
The method of claim 1, wherein the second phase is a ceramic.
Claim 27
Dependent Claim
12 words
The method of claim 1, wherein the second phase is an intermetallic.
Claim 28
Dependent Claim
15 words
The method of claim 1, wherein the composite contains additional particles precipitated during rapid quenching.
Claim 29
Dependent Claim
15 words
The method of claim 1, wherein the composite contains additional precipitate developed by scavenging interstitials.
Claim 30
Independent Claim
130 words
A method for precipitation of a second phase in a metallic matrix, the method comprising steps of: (a) preparing a mixture of reactive second phase forming constituents and a substantially nonreactive solvent matrix metal in which the second phase forming constituents are more soluble than the second phase; (b) heating the mixture to a reaction initiation temperature approximating the melting point of the solvent matrix metal to initiate an exothermic reaction; (c) permitting the exothermic reaction to further heat the mixture consuming the second phase forming constituents, and to form a uniform distribution of second phase particles; (d) rapidly quenching the mixture at a rate in the range of approximately 10 4 ° C. per second to 10 8 ° C. per second; and (e) recovering a rapidly solidified product.
Claim 31
Independent Claim
130 words
A method for precipitation of a second phase in a metallic matrix, the method comprising steps of: (a) preparing a mixture of reactive second phase forming constituents and a substantially nonreactive solvent matrix metal in which the second phase forming constituents are more soluble than the second phase; (b) heating the mixture to a reaction initiation temperature approximating the melting point of the solvent matrix metal to initiate an exothermic reaction; (c) permitting the exothermic reaction to further heat the mixture consuming the second phase forming constituents, and to form a uniform distribution of second phase particles; (d) rapidly quenching the mixture at a rate in the range of approximately 10 4 ° C. per second to 10 8 ° C. per second; and (e) recovering a rapidly solidified product.
Claim 32
Dependent Claim
27 words
The method of claim 29, wherein at least one second phase forming constituent is a transition metal of the third to sixth groups of the Periodic Table.
Claim 33
Dependent Claim
20 words
The method of claim 29, wherein the second phase is an oxide, nitride, boride, carbide, silicide, oxynitride, sulfide or oxysulfide.
Claim 34
Dependent Claim
52 words
The method of claim 29, wherein at least one second phase forming constituent is aluminum, titanium, silicon, boron, carbon, sulfur, tantalum, thorium, yttrium, cobalt, nickel, molybdenum, tungsten, vanadium, zirconium, niobium, hafnium, magnesium, scandium, lanthanum, chromium, oxygen, nitrogen, lithium, beryllium, iron, manganese, zinc, tin copper, silver, gold, platinum, or a rare earth element.
Claim 35
Dependent Claim
43 words
The method of claim 32, wherein said solvent metal is aluminum, nickel, titanium, copper, vanadium, chromium, manganese, cobalt, iron, silicon, molybdenum, beryllium, silver, gold, platinum, ruthenium, niobium, tantalum, hafnium, zirconium, magnesium, lead, zinc, tin, tungsten, antimony, bismuth, or an alloy of such metals.
Claim 36
Dependent Claim
20 words
The method of claim 29, wherein the second phase forming constituents and the solvent metal are provided as individual elements.
Claim 37
Dependent Claim
13 words
The method of claim 29, wherein said reaction takes place in liquid state.
Claim 38
Dependent Claim
43 words
The method of claim 35, wherein the solvent metal is aluminum, nickel, titanium, copper vanadium, chromium, manganese, cobalt, iron, silicon, molybdenum, beryllium, ruthenium, silver, gold platinum, niobium, tantalum, hafnium, zirconium, magnesium, lead, zinc, tin, tungsten, antimony, bismuth, or an alloy of such metals.
Claim 39
Dependent Claim
52 words
The method of claim 36, wherein at least one second phase forming constituent is aluminum, titanium, silicon, boron, carbon, sulfur, tantalum, thorium, yttrium, cobalt, nickel, molybdenum, tungsten, vanadium, zirconium, niobium, hafnium, magnesium, scandium, lanthanum, chromium, oxygen, nitrogen, lithium, beryllium, iron, manganese, zinc, tin, copper, silver, gold, platinum, or a rare earth element.
Claim 40
Dependent Claim
26 words
The method of claim 37, wherein at least one other second phase forming constituent is titanium diboride, zirconium diboride, zirconium disilicide, titanium oxide, or titanium nitride.
Claim 41
Dependent Claim
21 words
The method of claim 29, wherein the second phase forming constituents are each provided as an alloy of the solvent metal.
Claim 42
Dependent Claim
43 words
The method of claim 39, wherein said solvent metal is aluminum, nickel, titanium, copper, vanadium, chromium, manganese, cobalt, iron, silicon, molybdenum, beryllium, ruthenium, silver, gold platinum, niobium, tantalum, hafnium, zirconium, magnesium, lead, zinc, tin, tungsten, antimony, bismuth, or an alloy of such metals.
Claim 43
Dependent Claim
55 words
The method of claim 40, wherein said second phase forming constituents are selected from the group consisting of aluminum, titanium, silicon, boron, carbon, sulfur, tantalum, thorium, yttrium, cobalt, nickel, molybdenum, tungsten, vanadium, zirconium, niobium, hafnium, magnesium, scandium, lanthanum, chromium, oxygen, nitrogen, lithium, beryllium, iron, manganese, zinc, tin, copper, silver, gold, platinum and rare earth elements.
Claim 44
Dependent Claim
34 words
The method of claim 29, wherein at least one second phase forming constituent is provided as an individual element, and the other second phase forming constituents are provided as alloys of the solvent metal.
Claim 45
Dependent Claim
43 words
The method of claim 42, wherein said solvent metal is aluminum, nickel, titanium, copper, vanadium, chromium, manganese, cobalt, iron, silicon, molybdenum, beryllium, ruthenium, silver, gold, platinum, niobium, tantalum, hafnium, zirconium, magnesium, lead, zinc, tin, tungsten, ontimony, bismuth, or an alloy of such metals.
Claim 46
Dependent Claim
55 words
The method of claim 43, wherein said second phase forming constituents are selected from the group consisting of aluminum, titanium, silicon, boron, carbon, sulfur, tantalum, thorium, yttrium, cobalt, nickel, molybdenum, tungsten, vanadium, zirconium, niobium, hafnium, magnesium, scandium, lanthanum, chromium, oxygen, nitrogen, lithium, beryllium, iron manganese, zinc, tin, copper, silver, gold, platinum and rare earth elements.
Claim 47
Dependent Claim
19 words
The method of claim 29, wherein the second phase forming constituent is boron nitride, boron carbide, or boron oxide.
Claim 48
Dependent Claim
12 words
The method of claim 29, wherein the second phase is a ceramic.
Claim 49
Dependent Claim
12 words
The method of claim 29, wherein the second phase is an intermetallic.
Claim 50
Dependent Claim
27 words
The method of claim 29, wherein the solvent matrix metal with the second phase precipitated therein is added to a metal or alloy prior to rapid quenching.
Claim 51
Dependent Claim
29 words
The method of claim 29, wherein the solvent metal matrix and the second phase forming constituents are added to a solvent matrix metal or alloy prior to rapid quenching.
Claim 52
Dependent Claim
19 words
The method of claim 29, wherein the second phase forming constituents and the solvent metal are provided as powders.
Claim 53
Dependent Claim
24 words
The method of claim 29, wherein the second phase forming constituents and the solvent metal are provided as powders that are premixed and compacted.
Claim 54
Independent Claim
159 words
A method for dispersion of second phase dispersoids in a metal matrix, the method comprising forming a reaction mixture of reactive second phase forming constituents in the presence of at least two metals, at least one of which acts as a solvent metal, in which second phase forming constituents are more soluble than the second phase dispersoids, raising the temperature of the reaction mixture to a temperature at which sufficient diffusion of the second phase forming constituents into the lowest melting solvent metal occurs to initiate a reaction of the constituents, whereby the exothermic heat of reaction of the constituents causes the temperature of the reaction mixture to exceed the melting point of the higher melting point metal permitting dispersion of the second phase dispersoid in an alloy thereof, rapidly quenching the mixture at a rate in the range approximately 10 4 ° C. per second to 10 8 ° C. per second and recovering a rapidly solidified product.
Claim 55
Independent Claim
159 words
A method for dispersion of second phase dispersoids in a metal matrix, the method comprising forming a reaction mixture of reactive second phase forming constituents in the presence of at least two metals, at least one of which acts as a solvent metal, in which second phase forming constituents are more soluble than the second phase dispersoids, raising the temperature of the reaction mixture to a temperature at which sufficient diffusion of the second phase forming constituents into the lowest melting solvent metal occurs to initiate a reaction of the constituents, whereby the exothermic heat of reaction of the constituents causes the temperature of the reaction mixture to exceed the melting point of the higher melting point metal permitting dispersion of the second phase dispersoid in an alloy thereof, rapidly quenching the mixture at a rate in the range approximately 10 4 ° C. per second to 10 8 ° C. per second and recovering a rapidly solidified product.
Claim 56
Dependent Claim
22 words
The method of claim 52, wherein said higher melting solvent metal is cobalt, chromium, nickel, niobium, tantalum, titanium, vanadium, iron, or silicon.
Claim 57
Dependent Claim
19 words
The method of claim 53, wherein said lowest melting solvent metal is aluminum, copper, tin, zinc, lead or magnesium.
Claim 58
Dependent Claim
21 words
The method of claim 52, wherein additional alloying material is introduced to the solvent matrix metal prior to the rapid quenching.
Claim 59
Dependent Claim
12 words
The method of claim 52, wherein the second phase is a ceramic.
Claim 60
Dependent Claim
21 words
The method of claim 56, wherein additional alloying material is introduced to the solvent matrix metal prior to the rapid quenching.
Claim 61
Independent Claim
160 words
A method for dispersion of second phase dispersoids in a metal matrix, the method comprising forming a reaction mixture of reactive second phase forming constituents in the presence of at least two metals, at least one of which acts as a solvent metal, in which second phase forming constituents are more soluble than the second phase dispersoids, raising the temperature of the reaction mixture to a temperature at which sufficient diffusion of the second phase forming constituents into the lowest melting solvent metal occurs to initiate a reaction of the constituents, whereby the exothermic heat of reaction of the constituents causes the temperature of the reaction mixture to exceed the melting point of the lowest melting point metal permitting dispersion of the second phase dispersoid in a mixed metal matrix, rapidly quenching the mixture at a rate in the range approximately 10 4 ° C. per second to 10 8 ° C. per second and recovering a rapidly solidified product.
Claim 62
Independent Claim
160 words
A method for dispersion of second phase dispersoids in a metal matrix, the method comprising forming a reaction mixture of reactive second phase forming constituents in the presence of at least two metals, at least one of which acts as a solvent metal, in which second phase forming constituents are more soluble than the second phase dispersoids, raising the temperature of the reaction mixture to a temperature at which sufficient diffusion of the second phase forming constituents into the lowest melting solvent metal occurs to initiate a reaction of the constituents, whereby the exothermic heat of reaction of the constituents causes the temperature of the reaction mixture to exceed the melting point of the lowest melting point metal permitting dispersion of the second phase dispersoid in a mixed metal matrix, rapidly quenching the mixture at a rate in the range approximately 10 4 ° C. per second to 10 8 ° C. per second and recovering a rapidly solidified product.
Claim 63
Dependent Claim
21 words
The method of claim 58, wherein additional alloying material is introduced to the solvent matrix metal prior to the rapid quenching.
Claim 64
Dependent Claim
12 words
The method of claim 58, wherein the second phase is a ceramic.
Claim 65
Dependent Claim
12 words
The method of claim 58, wherein the second phase is an intermetallic.
Claim 66
Independent Claim
129 words
A method for the in-situ precipitation of at least one intermetallic material in a metallic matrix, comprising the steps of: (a) preparing a mixture of reactive intermetallic forming constituents and a nonreactive solvent matrix metal in which the intermetallic forming constituents are more soluble than the intermetallic material; (b) heating the mixture to a reaction initiation temperature approximating the melting point of the solvent matrix metal; (c) permitting the resultant exothermic reaction to raise the temperature of the mixture to a temperature exceeding the melting point of the matrix metal and to consume the intermetallic forming constituents; (d) rapidly quenching the mixture at a rate in the range approximately 10 4 ° C. per second to 10 8 ° C. per second; and (e) recovering a rapidly solidified product.
Claim 67
Independent Claim
129 words
A method for the in-situ precipitation of at least one intermetallic material in a metallic matrix, comprising the steps of: (a) preparing a mixture of reactive intermetallic forming constituents and a nonreactive solvent matrix metal in which the intermetallic forming constituents are more soluble than the intermetallic material; (b) heating the mixture to a reaction initiation temperature approximating the melting point of the solvent matrix metal; (c) permitting the resultant exothermic reaction to raise the temperature of the mixture to a temperature exceeding the melting point of the matrix metal and to consume the intermetallic forming constituents; (d) rapidly quenching the mixture at a rate in the range approximately 10 4 ° C. per second to 10 8 ° C. per second; and (e) recovering a rapidly solidified product.
Claim 68
Dependent Claim
42 words
The method of claim 62, wherein at least one intermetallic forming constituent ins aluminum, magnesium, chromium, manganese, iron, cobalt, copper, zinc, titanium, silicon, nickel, vanadium, molybdenum, niobium, beryllium, tin, silver, gold, hafnium, thorium, tungsten, zirconium, yttrium scandium, lanthanum, tantalum, platinum or lithium.
Claim 69
Dependent Claim
43 words
The method of claim 63, wherein said solvent metal is aluminum, nickel, titanium, copper, vanadium, chromium, manganese, cobalt, iron, silicon, molybdenum, beryllium, ruthenium, silver, gold, platinum, niobium, tantalum, hafnium, zirconium, magnesium, lead, zinc, tin, tungsten, antimony, bismuth, or an alloy of such metals.
Claim 70
Independent Claim
129 words
A method for the in-situ precipitation of at least one ceramic material in a metallic matrix, comprising the steps of: (a) preparing a mixture of reactive ceramic forming constituents and a non-reactive solvent matrix metal in which the ceramic forming constituents are more soluble than the ceramic material; (b) heating the mixture to a reaction initiation temperature approximating the melting point of the solvent matrix metal; (c) permitting the resultant exothermic reaction to raise the temperature of the mixture to a temperature exceeding the melting point of the matrix metal and to consume the ceramic forming constituents; (d) rapidly quenching the mixture at a rate in the range approximately 10 4 ° C. per second to 10 8 ° C. per second; and (e) recovering a rapidly solidified product.
Claim 71
Independent Claim
129 words
A method for the in-situ precipitation of at least one ceramic material in a metallic matrix, comprising the steps of: (a) preparing a mixture of reactive ceramic forming constituents and a non-reactive solvent matrix metal in which the ceramic forming constituents are more soluble than the ceramic material; (b) heating the mixture to a reaction initiation temperature approximating the melting point of the solvent matrix metal; (c) permitting the resultant exothermic reaction to raise the temperature of the mixture to a temperature exceeding the melting point of the matrix metal and to consume the ceramic forming constituents; (d) rapidly quenching the mixture at a rate in the range approximately 10 4 ° C. per second to 10 8 ° C. per second; and (e) recovering a rapidly solidified product.
Claim 72
Independent Claim
152 words
A method for the in-situ precipitation of dispersoid particles of an intermetallic material and a ceramic material in a metal matrix, the method comprising the steps of: (a) preparing a mixture of reactive intermetallic and ceramic forming constituents and a substantially non-reactive solvent matrix metal in which the intermetallic forming constituents and the ceramic forming constituents are more soluble than the intermetallic or the ceramic material respectively; (b) heating the mixture to a reaction initiation temperature approximating the melting point of the solvent matrix metal; (c) initiating an exothermic reaction to raise the temperature of the mixture to a temperature exceeding the melting point of the matrix metal and to consume the intermetallic forming constituents and the ceramic forming constituents; (d) rapidly quenching the mix at a rate in the range approximately 10 4 ° C. per second to 10 8 ° C. per second; and (e) recovering a rapidly solidified product.
Claim 73
Independent Claim
152 words
A method for the in-situ precipitation of dispersoid particles of an intermetallic material and a ceramic material in a metal matrix, the method comprising the steps of: (a) preparing a mixture of reactive intermetallic and ceramic forming constituents and a substantially non-reactive solvent matrix metal in which the intermetallic forming constituents and the ceramic forming constituents are more soluble than the intermetallic or the ceramic material respectively; (b) heating the mixture to a reaction initiation temperature approximating the melting point of the solvent matrix metal; (c) initiating an exothermic reaction to raise the temperature of the mixture to a temperature exceeding the melting point of the matrix metal and to consume the intermetallic forming constituents and the ceramic forming constituents; (d) rapidly quenching the mix at a rate in the range approximately 10 4 ° C. per second to 10 8 ° C. per second; and (e) recovering a rapidly solidified product.
Claim 74
Dependent Claim
59 words
The method of claim 66, wherein the intermetallic forming constitutents and the ceramic forming constituents are selected from the group consisting of aluminum, titanium, silicon, boron, carbon, sulfur, tantalum, thorium, yttrium, cobalt, nickel, molybdenum, tungsten, vanadium, zirconium, niobium, hafnium, magnesium, scandium, lanthanum, chromium, oxygen, nitrogen, lithium, beryllium, iron, manganese, zinc, tin, copper, silver, golf, platinum, and rare earth elements.
Claim 75
Dependent Claim
42 words
The method of claim 67, wherein said solvent metal is aluminum, nickel, titanium, copper, vanadium, chromium, manganese, cobalt, iron, silicon, molybdenum, beryllium, silver, gold, platinum, niobium, tantalum, hafnium, zirconium, magnesium, lead, zinc, tin, tungsten, antimony, bismuth, or an alloy of such metals.
References Cited (Backward Citations)
US3194656A
Cited
US3726643A
Cited
US4007062A
Cited
US4025249A
Cited
US4343750A
Cited
US4161512A
Cited
US4268564A
Cited
US4240824A
Cited
US4431448A
Cited
US4402745A
Cited
US4444603A
Cited
US4540546A
Cited
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