CN111763868A - High-entropy alloy powder for additive manufacturing and preparation method thereof - Google Patents
High-entropy alloy powder for additive manufacturing and preparation method thereof Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 84
- 239000000843 powder Substances 0.000 title claims abstract description 77
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 239000000654 additive Substances 0.000 title claims abstract description 16
- 230000000996 additive effect Effects 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 28
- 230000006698 induction Effects 0.000 claims abstract description 25
- 238000009689 gas atomisation Methods 0.000 claims abstract description 17
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 15
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 15
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 15
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 13
- 229910052742 iron Inorganic materials 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 10
- 238000003723 Smelting Methods 0.000 claims abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 6
- 239000001301 oxygen Substances 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- 239000012535 impurity Substances 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 238000012216 screening Methods 0.000 claims description 8
- 238000000889 atomisation Methods 0.000 claims description 6
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- 238000012360 testing method Methods 0.000 claims description 3
- 238000010146 3D printing Methods 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 5
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 238000004372 laser cladding Methods 0.000 abstract description 2
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- B22F1/0003—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0848—Melting process before atomisation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
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Abstract
The invention discloses high-entropy alloy powder for additive manufacturing and a preparation method thereof, wherein the high-entropy alloy powder comprises four or more elements of Fe, Al, Ni, Co, Cr, Mn and Mo, wherein the two elements of Fe and Al are required to exist in 1 or more, and the high-entropy alloy powder also comprises N element with the weight percentage of 0.1 at%, and the preparation method comprises the following steps: sequentially putting all pure metal raw materials into a vacuum induction smelting furnace according to the mass ratio of the elements for vacuum induction smelting, and then adopting a supersonic gas atomization rapid solidification technology to prepare the alloy. The high-entropy alloy powder prepared by the invention has ultrahigh purity, excellent fluidity, low hollow sphere rate and good sphericity, and can be used as a raw material of a 3D printing preparation technology to obtain a laser cladding layer with compact and uniform structure, less unmelted particles, low oxygen content, good mechanical property and corrosion resistance.
Description
Technical Field
The invention relates to the technical field of metal materials and 3D printing, in particular to high-entropy alloy powder for additive manufacturing and a preparation method thereof.
Background
To date, a total of 118 elements have been found, wherein 94 elements exist on the earth, the traditional alloy design uses a certain element as a base element, and on the basis of the base element, other alloy elements are added to obtain target performance, which has no doubt, so that the freedom of the alloy design is greatly limited, therefore, the alloy system to be developed is very limited, and only 30 kinds of high-entropy and multi-component alloy concepts are formally proposed in 2004 by professor samsung university of taiwan university leaf and Cantor of oxford university of britain, respectively, and the design concept of the high-entropy alloy is formally proposed in 2004 in journal of adv.eng.mater, so that the flail of the traditional alloy mainly using one element or two elements is broken through, and the paper singly refers more than 2400 times and causes huge reverberation in the field of metal materials.
With the rapid development of the 3D printing technology in recent years, the components of the alloy are more and more widely applied to the aspects of aerospace, high-speed rail ships, automobiles, military industry, medical implants and the like, and the 3D printing alloy components with the advantages are urgently needed aiming at the high-temperature resistance required by the components in harsh environments, the high wear resistance and high corrosion resistance required by ships and water conservancy, the high hardness required by the alloy components in high-speed rails and nuclear power, and the like.
The application of the additive manufacturing technology has more problems, one important technical bottleneck is the preparation of high-quality metal powder, at present, metal 3D printing powder at home and abroad is mostly prepared by adopting a traditional method, and the high-entropy alloy powder prepared by the methods has high impurity content and quality.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides high-entropy alloy powder for additive manufacturing and a preparation method thereof, and solves the problems that most of the existing domestic and foreign metal 3D printing powder is prepared by adopting the traditional method, and the high-entropy alloy powder prepared by the methods has high impurity content.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: the high-entropy alloy powder for additive manufacturing comprises high-entropy alloy powder which is composed of four or more elements of Fe, Al, Ni, Co, Cr, Mn and Mo in a near molar ratio or an equal molar ratio, wherein the two elements of Fe and Al are required to be present in 1 or more, and the high-entropy alloy powder also comprises 0.1 at% of N element in percentage by weight.
Preferably, the purity of Fe, Al, Ni, Co, Cr, Mn and Mo in the high-entropy alloy powder is more than or equal to 99.9%.
A preparation method of high-entropy alloy powder for additive manufacturing comprises the following steps:
step 1: weighing the raw materials according to the mass ratio of each element in the alloy powder, and entering the step 2;
step 2: smelting the weighed and taken raw materials by using a vacuum induction furnace, sequentially putting pure metal raw materials into a crucible in the furnace, sequentially putting Fe, Al, Ni, Co, Cr, Mn and Mo powder into the pure metal raw materials, and putting MN (M: Cr, Co, Ni and Mo) intermediate alloy according to the formula requirement; pressurizing the vacuum induction furnace in the working process, heating and refining the raw materials for three times by using a crucible, casting the raw materials into a mold to obtain a master alloy bar for gas atomization, and entering the step 3;
and step 3: A. opening a cabin door of electrode induction melting gas atomization equipment, polishing and removing impurities from the oxide skin on the surface of the master alloy bar obtained in the step (2), fixing the master alloy bar by a rotary electrode fixture, closing the cabin door, vacuumizing the electrode induction melting gas atomization equipment to less than or equal to 0.1Pa, heating to 1300 ℃, and introducing argon; B. and (4) continuously increasing the heating temperature of the electrode induction smelting gas atomization equipment, keeping the temperature for 1-3min until the temperature reaches 1550 ℃, finally atomizing by using argon, and entering the step 4.
And 4, step 4: and (3) collecting the atomized powder obtained in the step (3), and then screening the collected atomized powder by using cyclone separation equipment or a test screen to obtain the high-entropy alloy powder.
Preferably, the vacuum degree of the vacuum induction furnace after pressurization in the step 2 is not higher than 0.1 Pa.
Preferably, the atomization pressure of the argon in the step 3 is 8-10 MPa.
Preferably, the fluidity of the high-entropy alloy powder obtained after screening in the step 4 is less than or equal to 15s/50g, the oxygen content is less than or equal to 150ppm, the content of impurities such as S, P is less than or equal to 0.1%, and the particle size distribution is 5-180 μm.
(III) advantageous effects
The invention provides high-entropy alloy powder for additive manufacturing and a preparation method thereof. The method has the following beneficial effects:
(1) according to the high-entropy alloy powder provided by the invention, the mother alloy bar is subjected to secondary temperature progressive heating, and then argon gas with the pressure of 8-10MPa is used for atomization, so that compared with the high-entropy alloy powder prepared by a single heating method, the high-entropy alloy powder has higher purity and excellent fluidity, meanwhile, the oxygen content is not higher than 150ppm, the content of S, P and other impurities is not higher than 0.1%, compared with the high-entropy alloy powder prepared by a traditional method, the high-entropy alloy powder can be better applied to additive manufacturing, and the forming precision and the mechanical property of a product are favorably improved.
(2) The high-entropy alloy powder provided by the invention can be used as a raw material of a 3D printing preparation technology to obtain a laser cladding layer with compact and uniform structure, less unmelted particles, low oxygen content, good mechanical property and corrosion resistance, and can be widely applied to military fields such as aerospace aircraft engine cabins, nuclear combustion chamber repair protection and the like.
Drawings
FIG. 1 is an SEM photograph of the surface of the high-entropy alloy powder prepared by the invention;
FIG. 2 is a high-magnification SEM photograph of the surface of the high-entropy alloy powder prepared by the invention;
FIG. 3 is an SEM photograph of a cross section of the high-entropy alloy powder prepared by the invention;
FIG. 4 is an XRD diffraction pattern of the surface of the high-entropy alloy powder prepared by the invention.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention is further described in detail below with reference to the accompanying drawings.
The purity of the raw materials used in the embodiment of the invention is as follows: fe. The purity of Al, Ni, Co, Cr, Mn and Mo is more than or equal to 99.9 percent, and the purity of the intermediate alloy MN (M: Cr, Co, Ni and Mo) is more than or equal to 99.9 percent;
example 1
The preparation method of the high-entropy alloy powder comprises the following steps:
step 1: weighing the raw materials according to the mass ratio of each element in the alloy powder, and entering the step 2;
step 2: smelting the weighed and taken raw materials by using a vacuum induction furnace, sequentially putting pure metal raw materials into a crucible in the furnace, sequentially putting Fe, Al, Ni, Co, Cr, Mn and Mo powder into the pure metal raw materials, and putting MN (M: Cr, Co, Ni and Mo) intermediate alloy according to the formula requirement; pressurizing the vacuum induction furnace in the working process, heating and refining the raw materials for three times by using a crucible, casting the raw materials into a mold to obtain a master alloy bar for gas atomization, and entering the step 3, wherein the vacuum degree of the pressurized vacuum induction furnace is not higher than 0.1 Pa;
and step 3: A. opening a cabin door of the electrode induction melting gas atomization equipment, polishing and removing impurities from the oxide skin on the surface of the master alloy rod material obtained in the step (2), fixing the master alloy rod material by a rotary electrode fixture, closing the cabin door, vacuumizing the inside of the electrode induction melting gas atomization equipment to be more than or equal to 0.1Pa, heating to 1300 ℃, and introducing argon; B. continuing to increase the heating temperature of the electrode induction smelting gas atomization equipment until the temperature is 1550 ℃, preserving the heat for 1-3min, finally atomizing by using argon gas, wherein the atomization pressure of the argon gas is 8-10MPa, and entering the step 4;
and 4, step 4: and (3) collecting the atomized powder obtained in the step (3), and then screening the collected atomized powder by using cyclone separation equipment or a test sieve to obtain high-entropy alloy powder, wherein the fluidity of the high-entropy alloy powder obtained after screening is less than or equal to 15s/50g, the oxygen content is less than or equal to 150ppm, the content of S, P and other impurities is less than or equal to 0.1%, and the particle size distribution is 5-180 mu m.
The result of the detection
The SEM photograph of the high-entropy alloy powder prepared in the example 1 is shown in the attached drawing 1 of the specification, and the SEM photograph of the single powder in the attached drawing 2 of the specification shows that the powder has extremely high sphericity and only a small amount of satellite balls, the surface structure of the powder is uniform, the sphericity is good, no defects exist, the SEM photograph of the cross section of the powder in the attached drawing 3 of the specification shows that the powder is internally compact, the pores and the defects are extremely low, the fluidity of the powder measured by a Hall flowmeter of the high-entropy alloy powder prepared by the method is about 14s/50g, the filling effect is excellent, the high-entropy alloy powder is suitable for 3D printing, the attached drawing 4 of the specification shows that the XRD diffraction pattern of the FeCoNiMnCr high-entropy alloy powder after the trace N (0.1 at%) is added, and the sample is in a single FCC phase.
Example 2, a method of preparing a high entropy alloy powder for additive manufacturing is as follows:
step 1: weighing the raw materials according to the mass ratio of each element in the alloy powder, and entering the step 2;
step 2: smelting the weighed and taken raw materials by using a vacuum induction furnace, sequentially putting pure metal raw materials into a crucible in the furnace, sequentially putting Fe, Al, Ni, Co, Cr, Mn and Mo powder into the pure metal raw materials, and putting MN (M: Cr, Co, Ni and Mo) intermediate alloy according to the formula requirement; pressurizing the vacuum induction furnace in the working process, wherein the vacuum degree after pressurization is not higher than 0.1Pa, heating and refining the raw materials for three times by using a crucible, casting the raw materials into a mold to obtain a master alloy bar for gas atomization, and entering the step 3;
and step 3: A. opening a cabin door of electrode induction melting gas atomization equipment, polishing and removing impurities from oxide skin on the surface of the master alloy rod material obtained in the step (2), fixing the master alloy rod material by a rotary electrode fixture, closing the cabin door, vacuumizing the inside of the electrode induction melting gas atomization equipment to be more than or equal to 0.1Pa, heating to 1500 ℃, preserving the temperature for 1-3min, introducing argon, atomizing by using the argon, wherein the atomization pressure of the argon is 6-8MPa, and entering the step (4);
and 4, step 4: and (3) collecting the atomized powder obtained in the step (3), and then screening the collected atomized powder by using screening equipment to obtain the high-entropy alloy powder.
The result of the detection
(3) The embodiment 2 is basically the same as the embodiment 1, except that the master alloy bar is directly heated to 1550 ℃ by electrode induction melting gas atomization equipment, the argon atomization pressure is different, the obtained high-entropy alloy powder has poor sphericity, contains a large amount of satellite powder, has the fluidity of 18g/50s, and does not meet the index requirement of special powder for additive manufacturing, and the high-entropy alloy powder prepared in the embodiment 1 has extremely high sphericity, only has a small amount of satellite balls, has the fluidity of about 14s/50g, has higher purity and excellent fluidity, can be better applied to additive manufacturing, and is beneficial to improving the forming precision and the mechanical property of a product.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (6)
1. The high-entropy alloy powder for additive manufacturing is characterized by comprising high-entropy alloy powder which is composed of four or more elements of Fe, Al, Ni, Co, Cr, Mn and Mo in a near molar ratio or an equimolar ratio, wherein the two elements of Fe and Al are required to be present in 1 or more, and the high-entropy alloy powder also comprises 0.1 at% of N element in percentage by weight.
2. A high entropy alloy powder for additive manufacturing according to claim 1, wherein: the purity of Fe, Al, Ni, Co, Cr, Mn and Mo in the high-entropy alloy powder is more than or equal to 99.9 percent.
3. A method for producing a high-entropy alloy powder for additive manufacturing, according to any one of claims 1 to 2, comprising the steps of:
step 1: weighing the raw materials according to the mass ratio of each element in the alloy powder, and entering the step 2;
step 2: smelting the weighed and taken raw materials by using a vacuum induction furnace, sequentially putting pure metal raw materials into a crucible in the furnace, sequentially putting Fe, Al, Ni, Co, Cr, Mn and Mo powder into the pure metal raw materials, and putting MN (M: Cr, Co, Ni and Mo) intermediate alloy according to the formula requirement; pressurizing the vacuum induction furnace in the working process, heating and refining the raw materials for three times by using a crucible, casting the raw materials into a mold to obtain a master alloy bar for gas atomization, and entering the step 3;
and step 3: A. opening a cabin door of electrode induction melting gas atomization equipment, polishing and removing impurities from the oxide skin on the surface of the master alloy bar obtained in the step (2), fixing the master alloy bar by a rotary electrode fixture, closing the cabin door, vacuumizing the electrode induction melting gas atomization equipment to less than or equal to 0.1Pa, heating to 1300 ℃, and introducing argon; B. and (4) continuously increasing the heating temperature of the electrode induction smelting gas atomization equipment, keeping the temperature for 1-3min until the temperature reaches 1550 ℃, finally atomizing by using argon, and entering the step 4.
And 4, step 4: and (3) collecting the atomized powder obtained in the step (3), and then screening the collected atomized powder by using cyclone separation equipment or a test screen to obtain the high-entropy alloy powder.
4. A method for preparing high entropy alloy powder according to claim 3, characterized in that: and (3) in the step 2, the vacuum degree of the vacuum induction furnace after pressurization is not higher than 0.1 Pa.
5. A method for preparing high entropy alloy powder according to claim 3, characterized in that: in the step 3, the atomization pressure of the argon is 8-10 MPa.
6. A method for preparing high entropy alloy powder according to claim 3, characterized in that: the fluidity of the high-entropy alloy powder obtained after screening in the step 4 is less than or equal to 15s/50g, the oxygen content is less than or equal to 150ppm, the content of S, P and other impurities is less than or equal to 0.1%, and the particle size distribution is 5-180 mu.
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Cited By (5)
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| CN113976898A (en) * | 2021-10-29 | 2022-01-28 | 康硕(德阳)智能制造有限公司 | High-entropy alloy powder for 3D printing and preparation method thereof |
| CN114150330A (en) * | 2021-11-12 | 2022-03-08 | 东南大学 | FeCoNiMo high-entropy alloy powder oxygen evolution catalyst and preparation method thereof |
| CN114284422A (en) * | 2022-01-20 | 2022-04-05 | 济南大学 | Is suitable for CoSb3High-entropy electrode based on thermoelectric material and connection method of thermoelectric material and high-entropy electrode |
| CN114892058A (en) * | 2022-04-13 | 2022-08-12 | 哈尔滨工业大学 | Quaternary high-entropy alloy powder with body-centered cubic structure and preparation method thereof |
| CN114939654A (en) * | 2022-05-27 | 2022-08-26 | 中机新材料研究院(郑州)有限公司 | High-entropy alloy powder for laser additive manufacturing and preparation method and application thereof |
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