CN117583596A - Preparation method of iron-based metal hollow sphere - Google Patents
Preparation method of iron-based metal hollow sphere Download PDFInfo
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- CN117583596A CN117583596A CN202311570522.0A CN202311570522A CN117583596A CN 117583596 A CN117583596 A CN 117583596A CN 202311570522 A CN202311570522 A CN 202311570522A CN 117583596 A CN117583596 A CN 117583596A
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- Prior art keywords
- hollow sphere
- iron
- based metal
- metal hollow
- crucible
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000002184 metal Substances 0.000 title claims abstract description 45
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 45
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 239000011246 composite particle Substances 0.000 claims abstract description 22
- 239000010935 stainless steel Substances 0.000 claims abstract description 17
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 239000011148 porous material Substances 0.000 claims abstract description 13
- 239000012798 spherical particle Substances 0.000 claims abstract description 12
- 239000011230 binding agent Substances 0.000 claims abstract description 4
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 16
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000007769 metal material Substances 0.000 abstract description 6
- 238000001035 drying Methods 0.000 description 16
- 239000010410 layer Substances 0.000 description 16
- 239000006260 foam Substances 0.000 description 14
- 239000002131 composite material Substances 0.000 description 10
- 229910000831 Steel Inorganic materials 0.000 description 7
- 239000010959 steel Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000010963 304 stainless steel Substances 0.000 description 6
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 6
- 238000004321 preservation Methods 0.000 description 6
- 239000002923 metal particle Substances 0.000 description 4
- 239000010965 430 stainless steel Substances 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 3
- 229910001628 calcium chloride Inorganic materials 0.000 description 3
- 239000001110 calcium chloride Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
Classifications
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
- B22F1/0655—Hollow particles
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/18—Non-metallic particles coated with metal
Landscapes
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a preparation method of an iron-based metal hollow sphere, and belongs to the technical field of porous metal materials. According to the invention, absolute ethyl alcohol is used as a binder, stainless steel powder is coated on the surfaces of anhydrous calcium chloride spherical particles in a mechanical mixing mode to obtain composite particles, and then the composite particles are sequentially dried, sintered and ultrasonically cleaned to obtain iron-based metal hollow spheres; the sintering comprises the following steps: firstly, preserving the heat of the dried composite particles at 750 ℃ for 60-120 min; then preserving heat for 30-120 min at 800 ℃; finally, the temperature is raised to 1100 ℃ to 1200 ℃ and the heat is preserved for 120min to 180min. The preparation method has the advantages of controllable process, high yield, low cost, mass production and the like. In addition, the pore size, the wall thickness and the particle size of the iron-based metal hollow sphere prepared by the method can be flexibly controlled, and the metal hollow sphere has high surface density, good sphericity and higher strength.
Description
Technical Field
The invention belongs to the technical field of porous metal materials, and particularly relates to a preparation method of an iron-based metal hollow sphere.
Background
Because the traditional foam metal and the light component thereof have defects of uneven pore distribution and macroscopic pores, the performance repeatability and the qualification rate of the sample are lower. The hollow sphere composite foam metal material is a novel multifunctional light composite material, and has the advantages of flexible and controllable pore distribution, excellent and stable mechanical properties, and becomes a research hot spot of the existing porous metal.
The metal hollow sphere plays an important role in the preparation of the hollow sphere composite foam metal, and the hollow sphere particles with uniform pore wall thickness and controllable particle size are key to the excellent performance of the composite foam metal material. The metal and pore uniform/gradient hollow sphere particles form the composite foam metal material through sintering/casting means, and the composite foam metal material has flexible and controllable pore, few defects, high specific strength/rigidity, impact resistance, heat insulation and other performances, and has wide application prospects in the fields of automobile industry, aerospace and military industry.
The existing preparation methods of the metal hollow spheres mainly comprise a melt atomization method, an additive manufacturing method, a mechanical stamping welding method and the like. The hollow sphere prepared by the melt atomization method has smaller size, the process is difficult to control, and the yield is low; the additive manufacturing method can obtain the metal hollow spheres with flexible and controllable pore and wall thickness, but has long production period, high cost and is not suitable for mass production; the mechanical stamping welding method mainly prepares large-size metal hollow spheres and has complex process. The method has limitations in the aspects of hollow sphere size control, yield, mass production and the like, cannot meet the industrial application requirements of the composite foam metal, and leads to less related researches and applications of the hollow sphere composite foam metal.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of an iron-based metal hollow sphere
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the iron-based metal hollow sphere comprises the steps of taking absolute ethyl alcohol as a binder, coating stainless steel powder on the surface of anhydrous calcium chloride in a mechanical mixing mode to obtain composite particles, and sequentially drying, sintering and carrying out ultrasonic treatment to obtain the iron-based metal hollow sphere; the sintering comprises the following steps: firstly, preserving heat at 750 ℃ for 60-120 min to ensure that metal particles are pre-combined and the hollow sphere has certain strength; then preserving heat for 30-120 min at 800 ℃ to enable the pore-forming template to flow out as much as possible; finally, the temperature is raised to 1100 ℃ to 1200 ℃ and the heat is preserved for 120min to 180min.
The anhydrous calcium chloride is easy to flow out of the metal shell after being melted at high temperature, has small influence on the matrix, and has excellent mechanical properties in the foam steel prepared by participation; in addition, the anhydrous calcium chloride is very soluble in water and insoluble in ethanol, so that the anhydrous ethanol can be used as a binder for coating the anhydrous calcium chloride with the metal powder, and favorable conditions are provided for preparing the iron-based metal hollow spheres with low cost and high performance.
As a preferred embodiment of the invention, the stainless steel powder and the anhydrous calcium chloride are mixed, then the anhydrous ethanol is added, and the composite particles of the stainless steel powder coated with the anhydrous calcium chloride are obtained by a mechanical mixing mode.
As a preferred embodiment of the present invention, the anhydrous calcium chloride is spherical particles with a melting point of 782 ℃.
As a preferred embodiment of the invention, the mass of the ethanol is 3-5% of the mass of the stainless steel powder.
As a preferred embodiment of the present invention, the composite particles of the stainless steel powder coated with anhydrous calcium chloride are dried at 40-80 ℃ for 60-120 min, and ethanol is removed.
As a preferred embodiment of the invention, the sintering is performed under argon at a rate of temperature rise of less than 5 ℃/min.
As a preferred embodiment of the present invention, the stainless steel powder is an aerosolized 200, 300, or 400 series stainless steel powder.
As a preferred embodiment of the invention, the volume fraction ratio of the stainless steel powder to the anhydrous calcium chloride is 5-3:5-7, and the wall thickness and the size of the hollow sphere are regulated by regulating the batching ratio of the stainless steel powder to the anhydrous calcium chloride and the size of the anhydrous calcium chloride.
As a preferred embodiment of the invention, the crucible used for sintering comprises a first layer of crucible, a second layer of crucible and a third layer of crucible which are sequentially stacked from bottom to top, and the arrangement of the multi-layer crucible can improve the yield; the pore plates are respectively placed in the three layers of crucibles, and the dried composite particles are uniformly laid on each layer of pore plate, so that the secondary pollution of the bonding between the high-temperature sintered particles and the outflow of anhydrous calcium chloride to the hollow spheres is avoided; the three layers of crucibles have the same size, and the inner diameter of the bottom of the upper crucible is matched with the outer diameter of the top of the lower crucible, so that the sealing performance of each crucible cavity is ensured, and the oxidation degree of particles is reduced. The three layers of crucibles have the same size and are stacked layer by layer, and each layer of crucible is provided with an independent cavity.
As a preferred embodiment of the invention, the outer diameter of the orifice plate conforms to the inner diameter of the crucible.
As a preferred embodiment of the invention, the crucible used for sintering further comprises a crucible cover which is stacked above the third layer of crucible and matched with the size of the third layer of crucible.
Compared with the prior art, the invention has the beneficial effects that: the preparation method has the advantages of controllable process, high yield, low cost, mass production and the like, provides preconditions for preparing the hollow sphere composite foam metal, and also provides technical support for development and industrial application of the composite foam metal. In addition, the pore size, the wall thickness and the particle size of the iron-based metal hollow sphere prepared by the method can be flexibly controlled, and the metal hollow sphere has high surface density, good sphericity and higher strength.
Drawings
FIG. 1 is a flow chart of the preparation of iron-based metal hollow spheres.
Fig. 2 is a diagram of the orifice plate.
Fig. 3 is a forward block diagram of the crucible.
Fig. 4 is a reverse structural view of the crucible.
FIG. 5 is a combination of a single layer crucible and an orifice plate.
Fig. 6 is an equipment structure diagram of crucible stacking, in which a is a first layer crucible, b is a second layer crucible, c is a third layer crucible, and d is a crucible cover.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples.
Example 1
The preparation method of the iron-based metal hollow sphere comprises the following steps:
(1) Mixing atomized 304 stainless steel powder with the average granularity of 400 meshes and anhydrous calcium chloride spherical particles with the granularity of 6-8 meshes according to the volume fraction ratio of 2:3, putting the mixture into a V-shaped mixer, uniformly mixing, adding absolute ethyl alcohol accounting for 4% of the total metal powder in the mixing process, and mixing for 60min to obtain composite particles with the steel powder uniformly coated with the anhydrous calcium chloride particles, wherein the melting point of the anhydrous calcium chloride spherical particles is 782 ℃.
(2) And (3) drying the composite particles in a drying oven to remove absolute ethyl alcohol, wherein the drying temperature is 60 ℃ and the drying time is 120min.
(3) Uniformly spreading the dried composite particles in a specially-made crucible (shown in fig. 5), and sintering in an argon atmosphere: in the sintering process, firstly, heat preservation is carried out for 120min at 750 ℃, so that metal particles are pre-combined, the hollow sphere is guaranteed to have certain strength, heat preservation is carried out for 60min at 800 ℃, anhydrous calcium chloride flows out from the particle shell as much as possible, the temperature is finally increased to 1100 ℃, sintering is carried out for 120min, and the temperature increasing rate in the sintering process is 4 ℃/min.
(4) Placing the spherical particles after sintering into an ultrasonic cleaner filled with deionized water for ultrasonic cleaning and multiple times of water bath heating cleaning to remove residual calcium chloride in the hollow spheres; and further drying to obtain 304 stainless steel hollow sphere particles.
The diameter of the 304 stainless steel hollow sphere prepared in example 1 is 2.6 mm-3.6 mm, the wall thickness is 0.22 mm-0.28 mm, and the density is 1.3g/cm 3 ～2.0g/cm 3 The foam steel block made of the hollow sphere has high compressive strength, which can reach 65MPa to 70MPa.
Example 2
The preparation method of the iron-based metal hollow sphere comprises the following steps:
(1) Mixing atomized 430 stainless steel powder with the average granularity of 400 meshes and anhydrous calcium chloride spherical particles with the granularity of 6-8 meshes according to the volume fraction ratio of 3:7, respectively putting the mixture into a V-shaped mixer for uniform mixing, adding absolute ethyl alcohol accounting for 4% of the total metal powder in the mixing process, and mixing for 60min to obtain composite particles with the steel powder uniformly coated with the anhydrous calcium chloride particles, wherein the melting point of the anhydrous calcium chloride spherical particles is 782 ℃.
(2) And (3) drying the composite particles in a drying oven to remove absolute ethyl alcohol, wherein the drying temperature is 40 ℃ and the drying time is 60min.
(3) The dried composite particles were uniformly tiled in a special crucible (as shown in fig. 5) and sealed with iron powder and sintered in an argon atmosphere: in the sintering process, firstly, heat preservation is carried out for 60min at 750 ℃ to ensure that metal particles are pre-combined, the hollow spheres are ensured to have certain strength, heat preservation is carried out for 30min at 800 ℃ to ensure that anhydrous calcium chloride flows out of the particle shells as much as possible, the temperature is finally increased to 1200 ℃, the sintering is carried out for 120min, and the temperature increasing rate in the sintering process is 4 ℃/min;
(4) Placing the spherical particles after sintering into an ultrasonic cleaner filled with deionized water for ultrasonic cleaning and multiple times of water bath heating cleaning to remove residual calcium chloride in the hollow spheres; and further drying to obtain 430 stainless steel hollow sphere particles.
The diameter of the 430 stainless steel hollow sphere prepared in example 2 is 2.4 mm-3.5 mm, the wall thickness is 0.16 mm-0.23 mm, and the density is 1.0g/cm 3 ～1.1g/cm 3 The foam steel block made of the hollow sphere has high compressive strength, which can reach 60MPa to 70MPa.
Example 3
The preparation method of the iron-based metal hollow sphere comprises the following steps:
(1) Mixing atomized 304 stainless steel powder with the average granularity of 400 meshes and anhydrous calcium chloride spherical particles with the granularity of 6-8 meshes according to the volume fraction ratio of 5:5, putting the mixture into a V-shaped mixer, uniformly mixing, adding absolute ethyl alcohol accounting for 5% of the total metal powder in the mixing process, and mixing for 60min to obtain composite particles with the steel powder uniformly coated with the anhydrous calcium chloride particles, wherein the melting point of the anhydrous calcium chloride spherical particles is 782 ℃.
(2) And (3) drying the composite particles in a drying oven to remove absolute ethyl alcohol, wherein the drying temperature is 80 ℃ and the drying time is 120min.
(3) Uniformly spreading the dried composite particles in a specially-made crucible (shown in fig. 5), and sintering in an argon atmosphere: in the sintering process, firstly, heat preservation is carried out for 120min at 750 ℃ to ensure that metal particles are pre-combined, the hollow sphere is ensured to have certain strength, heat preservation is carried out for 120min at 800 ℃ to ensure that anhydrous calcium chloride flows out of the particle shell as much as possible, the temperature is finally increased to 1200 ℃, sintering is carried out for 180min, and the temperature increasing rate in the sintering process is 4 ℃/min.
(4) Placing the spherical particles after sintering into an ultrasonic cleaner filled with deionized water for ultrasonic cleaning and multiple times of water bath heating cleaning to remove residual calcium chloride in the hollow spheres; and further drying to obtain 304 stainless steel hollow sphere particles.
The diameter of the 304 stainless steel hollow sphere prepared in example 3 is 2.7 mm-3.8 mm, the wall thickness is 0.30 mm-0.37 mm, and the density is 2.3g/cm 3 ～3.1g/cm 3 The foam steel block made of the hollow sphere has high compressive strength which can reach 77MPa to 85MPa.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1. The preparation method of the iron-based metal hollow sphere is characterized in that absolute ethyl alcohol is used as a binder, stainless steel powder is coated on the surface of anhydrous calcium chloride in a mechanical mixing mode to obtain composite particles, and then the composite particles are sequentially dried, sintered and ultrasonically treated to obtain the iron-based metal hollow sphere; the sintering comprises the following steps: firstly, preserving the heat of the dried composite particles at 750 ℃ for 60-120 min; then preserving heat for 30-120 min at 800 ℃; finally, the temperature is raised to 1100 ℃ to 1200 ℃ and the heat is preserved for 120min to 180min.
2. The method for preparing the iron-based metal hollow sphere according to claim 1, wherein the stainless steel powder and the anhydrous calcium chloride are mixed, and then ethanol is added to obtain the composite particles of the stainless steel powder coated with the anhydrous calcium chloride.
3. The method for preparing the iron-based metal hollow sphere according to claim 1, wherein the anhydrous calcium chloride is spherical particles, and the melting point is 782 ℃.
4. The method for preparing the iron-based metal hollow sphere according to claim 1, wherein the mass of the ethanol is 3% -5% of the mass of the stainless steel powder.
5. The method for preparing the iron-based metal hollow sphere according to claim 1, wherein the composite particles are dried at 40 to 80 ℃ for 60 to 120 minutes.
6. The method for preparing the iron-based metal hollow sphere according to claim 1, wherein the temperature rising rate of sintering is less than 5 ℃/min, and the sintering is performed under argon.
7. The method for preparing the iron-based metal hollow sphere according to claim 1, wherein the stainless steel powder is an aerosolized 200, 300, or 400 series stainless steel powder.
8. The method for preparing the iron-based metal hollow sphere according to claim 1, wherein the volume fraction ratio of the stainless steel powder to the anhydrous calcium chloride is 5-3:5-7.
9. The method for preparing the iron-based metal hollow sphere according to claim 1, wherein the crucible used for sintering comprises a first layer of crucible, a second layer of crucible and a third layer of crucible which are sequentially stacked from bottom to top; respectively placing pore plates in the three layers of crucibles, and uniformly laying the dried composite particles on each layer of pore plates; the three layers of crucibles are the same in size, and each layer of crucible is provided with an independent cavity.
10. The method for preparing the iron-based metal hollow sphere according to claim 1, wherein the crucible used for sintering further comprises a crucible cover which is stacked above the third layer of crucible, and the crucible cover is matched with the third layer of crucible in size to realize crucible sealing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311570522.0A CN117583596A (en) | 2023-11-23 | 2023-11-23 | Preparation method of iron-based metal hollow sphere |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311570522.0A CN117583596A (en) | 2023-11-23 | 2023-11-23 | Preparation method of iron-based metal hollow sphere |
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| CN117583596A true CN117583596A (en) | 2024-02-23 |
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| CN202311570522.0A Pending CN117583596A (en) | 2023-11-23 | 2023-11-23 | Preparation method of iron-based metal hollow sphere |
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| Country | Link |
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- 2023-11-23 CN CN202311570522.0A patent/CN117583596A/en active Pending
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