CN115846624A - Preparation method of ceramic/iron-based honeycomb-configuration composite material - Google Patents
Preparation method of ceramic/iron-based honeycomb-configuration composite material Download PDFInfo
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- CN115846624A CN115846624A CN202310173322.5A CN202310173322A CN115846624A CN 115846624 A CN115846624 A CN 115846624A CN 202310173322 A CN202310173322 A CN 202310173322A CN 115846624 A CN115846624 A CN 115846624A
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- titanium carbonitride
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 239000002131 composite material Substances 0.000 title claims abstract description 70
- 239000000919 ceramic Substances 0.000 title claims abstract description 49
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000010936 titanium Substances 0.000 claims abstract description 50
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 45
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 42
- 239000011812 mixed powder Substances 0.000 claims abstract description 33
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 28
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000001354 calcination Methods 0.000 claims abstract description 16
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000011230 binding agent Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 239000000161 steel melt Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000011049 filling Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000001257 hydrogen Substances 0.000 claims description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 230000009467 reduction Effects 0.000 claims description 13
- 150000002500 ions Chemical class 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 10
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 6
- 239000005038 ethylene vinyl acetate Substances 0.000 claims description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 229920002472 Starch Polymers 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 239000008107 starch Substances 0.000 claims description 4
- 235000019698 starch Nutrition 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 150000002431 hydrogen Chemical class 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 238000011946 reduction process Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 239000011159 matrix material Substances 0.000 abstract description 7
- 238000005299 abrasion Methods 0.000 abstract description 6
- 229910000831 Steel Inorganic materials 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 5
- 239000010959 steel Substances 0.000 abstract description 5
- 230000009471 action Effects 0.000 abstract description 2
- 239000004566 building material Substances 0.000 abstract description 2
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 229910001018 Cast iron Inorganic materials 0.000 description 13
- 229910052804 chromium Inorganic materials 0.000 description 12
- 239000011651 chromium Substances 0.000 description 12
- 230000002787 reinforcement Effects 0.000 description 10
- 239000010410 layer Substances 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 229910000851 Alloy steel Inorganic materials 0.000 description 7
- 229910000617 Mangalloy Inorganic materials 0.000 description 7
- 238000005266 casting Methods 0.000 description 7
- 238000005054 agglomeration Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 239000011324 bead Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 2
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 239000012692 Fe precursor Substances 0.000 description 1
- 241000251131 Sphyrna Species 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- UFGZSIPAQKLCGR-UHFFFAOYSA-N chromium carbide Chemical compound [Cr]#C[Cr]C#[Cr] UFGZSIPAQKLCGR-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000010114 lost-foam casting Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 229910003470 tongbaite Inorganic materials 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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Abstract
The invention discloses a preparation method of a ceramic/iron-based honeycomb-shaped composite material, and belongs to the technical field of metal-based composite materials. The method comprises the steps of uniformly mixing sol prepared from ferric nitrate nonahydrate, citric acid and the like and sol prepared from hydrated titanium dioxide, activated carbon and the like, drying, calcining at high temperature, roasting, reducing and the like to obtain mixed powder of titanium carbonitride ceramic and iron, uniformly stirring the mixed powder and a binder, filling the mixed powder into honeycomb walls of a honeycomb structure die to be solidified to form a prefabricated body, and pouring a steel melt to obtain the titanium carbonitride ceramic reinforced iron-based honeycomb configuration composite material. The titanium carbonitride ceramic is uniformly dispersed and distributed in the iron matrix of the composite region, the honeycomb wall of the composite material is composed of the composite region with higher hardness, the abrasion action on the honeycomb holes with softer hardness can be obviously reduced, the abrasion resistance is improved by more than 4 times compared with the traditional steel material, and the titanium carbonitride ceramic has wide application prospect in the fields of metallurgy, mines, building materials and the like.
Description
Technical Field
The invention relates to a preparation method of a ceramic/iron-based honeycomb-structure composite material, and belongs to the technical field of metal-based composite materials.
Background
In the fields of mines, metallurgy, building materials and the like, wear-resistant parts such as plate hammers, hammerheads, grinding rolls and the like need materials with higher mechanical and wear-resistant material wear properties. The ceramic/steel-based honeycomb-structure composite material has the advantages of high degree of designability, good wear resistance, lower cost and the like, and becomes an important development direction of wear-resistant materials for equipment manufacturing.
In the common ceramic phase of ceramic/iron-based composite materials, carbides such as titanium carbonitride (Ti (C, N)), titanium carbide (TiC), tungsten carbide (WC) and the like, and aluminum oxide (Al) 2 O 3 ) Oxides such as Zirconia Toughened Alumina (ZTA) and the like have better mechanical and abrasion resistance, and scholars at home and abroad carry out a great deal of research and application work on the composite materials, wherein titanium carbonitride (Ti (C, N)) ceramics have good toughness and low cost, and are widely applied to abrasion-resistant parts. But the wear-resistant part utilizes the extrusion effect to crush and grind materials in service, and the reinforced phase of the composite material is required not to be crushed and fall off under the action of strong pressure. The reduction of the size of the ceramic particles can obviously reduce the brittleness of the large-size particles, and the interface bonding strength of the authigenic ceramic particles and the iron matrix is higher, so that the research and development of the in-situ authigenic titanium carbonitride/iron-based composite material are paid attention by researchers at home and abroad, but the breakthrough progress is not obtained. In addition, the traditional ceramic reinforced iron-based surface layer composite material has insufficient ceramic infiltration depth of an iron matrix in the preparation process, the thickness of the composite layer is thin, and the composite layer is easy to peel off in the whole layer when in use due to large difference of thermophysical parameters of a composite region and a matrix region.
The invention only discloses a preparation method of an iron-based composite impeller cooperatively enhanced by titanium carbonitride and chromium carbide, which is disclosed by Chinese invention patent CN202210462248.4, namely reinforcing body particles and EPS beads are weighed according to volume fraction, an organic adhesive is mixed with the EPS beads, then the mixed reinforcing body is added and mixed, loose materials with the mixed reinforcing body bonded on the surface of the EPS beads are obtained, the loose materials are added into a material conveying pipe, and the impeller is prepared by adopting a V-EPC lost foam casting process. In the iron-based composite material prepared by the method, the ceramic phase is compounded in an additional form, the problem of intrinsic brittleness of the ceramic is not solved, and the ceramic reinforcement and the high polymer EPS beads are difficult to uniformly disperse and are easy to generate agglomeration segregation and other phenomena due to overlarge density difference.
Disclosure of Invention
In order to solve the problems of intrinsic brittleness of a large-size ceramic phase additionally added to a ceramic reinforced iron-based composite material, agglomeration and segregation of a ceramic reinforcement, easy peeling of the whole layer of a surface composite material composite region in a service process and insufficient wear resistance, the invention uniformly mixes an iron precursor and a titanium carbonitride precursor to obtain a novel method for preparing a honeycomb-shaped composite material with uniformly dispersed and distributed ceramic reinforcements in the composite region, and the method specifically comprises the following steps:
(1) Dissolving ferric nitrate nonahydrate in citric acid solution, controlling the proportion of ferric nitrate nonahydrate and citric acid in the solution, and then putting the mixed solution into a water bath kettle for constant-temperature heating to obtain sol (1).
(2) Adding nano activated carbon into the hydrated titanium dioxide solution, stirring at a high speed, and then placing the mixed solution into a water bath kettle for constant-temperature heating to obtain the sol (2).
(3) And (3) uniformly mixing the sol (1) obtained in the step (1) and the sol (2) obtained in the step (2) in proportion, and performing vacuum drying treatment to obtain mixed gel.
(4) Placing the mixed gel obtained in the step (3) in nitrogen for high-temperature calcination, performing roasting treatment to obtain mixed powder of titanium carbonitride and iron oxide, and then placing the mixed powder into a reduction furnace for reduction by reducing gas to obtain mixed powder of titanium carbonitride and iron;
(5) And (4) uniformly stirring the mixed powder obtained in the step (4) and a binder, then filling the mixture into the honeycomb wall of a honeycomb structure die to be solidified to form a prefabricated body, and pouring a steel melt to obtain the titanium carbonitride ceramic reinforced iron-based honeycomb-configuration composite material.
Preferably, the molar ratio of the ferric nitrate to the citric acid in the step (1) of the invention is 1 (0.6 to 1.2).
Preferably, the heating conditions of the water bath kettle in the step (1) of the invention are as follows: heating at 60-90 deg.C for 8-12h.
Preferably, the molar ratio of the hydrated titanium dioxide to the nano activated carbon in the step (2) of the invention is 1 (0.8 to 1.2), and the particle size of the nano activated carbon is 10-30nm.
Preferably, the heating conditions of the water bath kettle in the step (2) of the invention are as follows: heating at 40-70 deg.C for 4-8h.
Preferably, the molar ratio of Fe ions in the sol (1) to Ti ions in the sol (2) in the step (3) of the invention is 1 (0.02 to 0.4).
Preferably, the drying conditions in step (3) of the present invention are: drying in a vacuum drying oven at 100-150 deg.C for 14-20h.
Preferably, the calcining and calcining conditions in step (4) of the present invention are: calcining at 1400-1600 deg.C for 2-4 hr in nitrogen atmosphere, and calcining at 800-1000 deg.C for 3-5 hr in air atmosphere.
Preferably, the reducing gas used in the reduction process in the step (5) of the invention is hydrogen, the temperature of the reducing furnace is 600-800 ℃, and the hydrogen flow is 1.0-2.0m 3 The time is 4-6h.
Preferably, in step (5) of the present invention, the binder is any one of polyvinyl alcohol, ethylene-vinyl acetate copolymer, and starch paste.
Preferably, in the step (5) of the invention, the molar ratio of the binder to the titanium carbonitride and iron mixed powder is (0.02 to 0.04): 1.
Preferably, the curing conditions in step (5) of the present invention are: curing for 6-10h in a heat preservation box at 90-130 ℃.
The steel melt is conventional steel, and preferably any one of high-chromium cast iron, high-manganese steel and alloy steel.
Compared with the prior art, the invention has the beneficial effects that:
1) In the invention, the precursor sol of iron and the precursor sol of titanium carbonitride are uniformly mixed in a liquid state in the early stage of the preparation of the composite material, thereby avoiding the problem of reinforcement agglomeration or segregation caused by overlarge density difference when an additional ceramic reinforcement is mixed with iron or EPS; 2) In the method, the titanium carbonitride ceramic is in-situ self-generated, the size of the ceramic reinforcement is nano-scale, the intrinsic brittleness of the ceramic is obviously reduced, and the surface of the reinforcement is pollution-free and the compatibility between the matrix and the reinforcement is good because the ceramic reinforcement forms nuclei and grows in the iron matrix; 3) The honeycomb wall of the honeycomb-structure composite material is composed of a composite area composed of ceramic and iron with high hardness, and the honeycomb holes are composed of steel metal areas with low hardness, in the abrasion process, the composite area with high hardness can prevent the metal areas with low hardness from being abraded, the composite layer is not easy to peel off, the abrasion resistance is improved by more than 2 times compared with that of the traditional surface composite material, and is improved by more than 4 times compared with that of the traditional steel material.
Drawings
FIG. 1 is a photograph of a cured honeycomb-shaped preform prepared in accordance with the present invention;
FIG. 2 is a surface topography of the titanium carbonitride/iron based honeycomb configured composite material prepared in the present invention.
Detailed Description
The technical solutions in the present invention will be described clearly and completely with reference to the embodiments in the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by those skilled in the art without any creative work based on the embodiments in the present invention belong to the protection scope of the present invention.
Example 1
The embodiment relates to a preparation method of a ceramic/high-chromium cast iron based honeycomb-configuration composite material, which comprises the following specific steps:
(1) Dissolving ferric nitrate nonahydrate in citric acid solution, controlling the molar ratio of ferric nitrate nonahydrate to citric acid in the solution to be 1:1, then putting the mixed solution into a water bath, and heating at the constant temperature of 80 ℃ for 10h to obtain sol (1).
(2) Adding activated carbon with the particle size of 20nm into the hydrated titanium dioxide solution, wherein the molar ratio of the hydrated titanium dioxide to the nano activated carbon is 1:1, stirring at a high speed, putting the mixed solution into a water bath, and heating at the constant temperature of 60 ℃ for 5 hours to obtain the sol (2).
(3) Uniformly mixing the sol (1) obtained in the step (1) and the sol (2) obtained in the step (2) according to the molar ratio of Fe ions to Ti ions being 1.
(4) And (4) calcining the mixed gel obtained in the step (3) for 2.5h at 1500 ℃ in a nitrogen atmosphere, and then calcining for 4.5h at 900 ℃ in an air atmosphere to obtain the mixed powder of titanium carbonitride and ferric oxide.
(5) Putting the mixed powder into a hydrogen reduction furnace, wherein the temperature of the hydrogen reduction furnace is 750 ℃, and the hydrogen flow is 1.2m 3 And h, wherein the time is 5h, and the mixed powder of the titanium carbonitride and the iron is obtained.
(6) Uniformly mixing the mixed powder with a polyvinyl alcohol binder, wherein the molar ratio of polyvinyl alcohol to the mixed powder is 0.02 to 1, curing at 120 ℃ for 8 hours to form a honeycomb-shaped preform, and a macroscopic photograph of the preform is shown in fig. 1, and it can be seen from fig. 1 that titanium carbonitride and iron in the preform are uniformly mixed.
(7) The prefabricated body is placed into a casting cavity, then the smelted high-chromium cast iron melt is cast, and the titanium carbonitride ceramic/high-chromium cast iron based honeycomb-shaped composite material can be obtained after cooling, a macroscopic photo of the shaped composite material is shown in figure 2, as can be seen from figure 2, the composite material consists of a composite area and a metal area, the honeycomb structure is not collapsed, wherein titanium carbonitride reinforcements in the composite area are uniformly dispersed in a matrix, the agglomeration phenomenon is avoided, and no obvious defect exists in the composite area.
The titanium carbonitride reinforced high-chromium cast iron based honeycomb-shaped composite material prepared by the invention (the volume wear rate is 70.7 mm) 3 H) and the wear resistance is higher than that of the traditional high-chromium cast iron (the volume wear rate is 290 mm) 3 H) is improved by 4.1 times, and compared with the whole layer composite titanium carbonitride reinforced high chromium cast iron-based composite material (the volume wear rate is 155.5 mm) 3 The/h) is increased by 2.2 times.
Example 2
The embodiment relates to a preparation method of a ceramic/high manganese steel based honeycomb-structure composite material, which comprises the following specific steps:
(1) Dissolving ferric nitrate nonahydrate in a citric acid solution, controlling the molar ratio of the ferric nitrate nonahydrate to the citric acid in the solution to be 1.
(2) Adding activated carbon with the particle size of 10nm into a hydrated titanium dioxide solution, wherein the molar ratio of the hydrated titanium dioxide to the nano activated carbon is 1.2, stirring at a high speed, putting the mixed solution into a water bath, and heating at a constant temperature of 70 ℃ for 4 hours to obtain the sol (2).
(3) Uniformly mixing the sol (1) obtained in the step (1) and the sol (2) obtained in the step (2) according to the molar ratio of Fe ions to Ti ions being 1.
(4) And (4) calcining the mixed gel obtained in the step (3) for 4 hours at the temperature of 1400 ℃ in a nitrogen atmosphere, and then calcining for 3 hours at the temperature of 1000 ℃ in an air atmosphere to obtain the mixed powder of titanium carbonitride and ferric oxide.
(5) Putting the mixed powder into a hydrogen reduction furnace, wherein the temperature of the hydrogen reduction furnace is 600 ℃, and the hydrogen flow is 2.0m 3 And h, wherein the time is 4h, and the mixed powder of the titanium carbonitride and the iron is obtained.
(6) And uniformly mixing the mixed powder with an ethylene-vinyl acetate copolymer adhesive, wherein the molar ratio of the ethylene-vinyl acetate copolymer to the mixed powder is 0.04.
(7) And (3) placing the prefabricated body into a casting cavity, then casting the smelted high manganese steel melt, and cooling to obtain the titanium carbonitride ceramic/high manganese steel-based honeycomb-structure composite material.
The titanium carbonitride reinforced high manganese steel based honeycomb-shaped composite material prepared by the invention (the volume wear rate is 60.2 mm) 3 H) and the wear resistance is higher than that of the traditional high manganese steel (the volume wear rate is 240.6 mm) 3 The volume wear rate is 126.4mm, which is 4 times higher than that of the whole layer composite titanium carbonitride reinforced high manganese steel base composite material 3 The/h) is increased by 2.1 times.
Example 3
The embodiment relates to a preparation method of a ceramic/alloy steel-based honeycomb-shaped composite material, which comprises the following specific steps:
(1) Dissolving ferric nitrate nonahydrate in a citric acid solution, controlling the molar ratio of the ferric nitrate nonahydrate to the citric acid in the solution to be 1.2, then putting the mixed solution into a water bath kettle, and heating at a constant temperature of 90 ℃ for 8h to obtain the sol (1).
(2) Adding active carbon with the granularity of 30nm into the hydrated titanium dioxide solution, wherein the molar ratio of the hydrated titanium dioxide to the nano active carbon is 1:0.8, stirring at a high speed, putting the mixed solution into a water bath, and heating at a constant temperature of 40 ℃ for 8h to obtain the sol (2).
(3) Uniformly mixing the sol (1) obtained in the step (1) and the sol (2) obtained in the step (2) according to the molar ratio of Fe ions to Ti ions being 1.
(4) And (4) calcining the mixed gel obtained in the step (3) for 2 hours at 1600 ℃ in a nitrogen atmosphere, and then calcining for 5 hours at 800 ℃ in an air atmosphere to obtain the mixed powder of titanium carbonitride and ferric oxide.
(5) Putting the mixed powder into a hydrogen reduction furnace, wherein the temperature of the hydrogen reduction furnace is 800 ℃, and the hydrogen flow is 1.0m 3 And/h, the time is 6h, and the mixed powder of the titanium carbonitride and the iron is obtained.
(6) Uniformly mixing the mixed powder with an ethylene-vinyl acetate copolymer adhesive, wherein the molar ratio of the ethylene-vinyl acetate copolymer to the mixed powder is 0.03 to 1, and curing at 90 ℃ for 10 hours to form a honeycomb-shaped preform.
(7) And placing the prefabricated body into a casting cavity, then casting the smelted alloy steel melt, and cooling to obtain the titanium carbonitride ceramic/alloy steel-based honeycomb-shaped composite material.
The titanium carbonitride reinforced alloy steel-based honeycomb-configuration composite material prepared by the method (the volume wear rate is 86.4 mm) 3 H) and the wear resistance is higher than that of the traditional alloy steel (the volume wear rate is 362.7 mm) 3 The volume wear rate is 172.8mm, which is 4.2 times higher than that of the whole layer composite titanium carbonitride reinforced alloy steel base composite material 3 The/h) is increased by 2 times.
Example 4
The embodiment relates to a preparation method of a ceramic reinforced high-chromium cast iron-based honeycomb-configuration composite material, which comprises the following specific steps:
(1) Dissolving ferric nitrate nonahydrate in a citric acid solution, controlling the molar ratio of the ferric nitrate nonahydrate to the citric acid in the solution to be 1.
(2) Adding activated carbon with the particle size of 25nm into a hydrated titanium dioxide solution, wherein the molar ratio of the hydrated titanium dioxide to the nano activated carbon is 1.1, stirring at a high speed, putting the mixed solution into a water bath, and heating at the constant temperature of 55 ℃ for 6.5h to obtain sol (2).
(3) Uniformly mixing the sol (1) obtained in the step (1) and the sol (2) obtained in the step (2) according to the molar ratio of Fe ions to Ti ions being 1.
(4) And (4) calcining the mixed gel obtained in the step (3) for 3.5h at the temperature of 1450 ℃ in a nitrogen atmosphere, and then calcining for 2.5h at the temperature of 950 ℃ in an air atmosphere to obtain the mixed powder of titanium carbonitride and ferric oxide.
(5) Putting the mixed powder into a hydrogen reduction furnace, wherein the temperature of the hydrogen reduction furnace is 650 ℃, and the hydrogen flow is 1.4m 3 And h, the time is 5.5h, and the mixed powder of the titanium carbonitride and the iron is obtained.
(6) Uniformly mixing the mixed powder with a starch paste binder, wherein the molar ratio of the starch paste to the mixed powder is 0.025 to 1, and curing at 1150 ℃ for 7.5 hours to form a honeycomb-shaped preform.
(7) And placing the prefabricated body into a casting cavity, then casting the smelted high-chromium cast iron melt, and cooling to obtain the titanium carbonitride ceramic/high-chromium cast iron-based honeycomb-shaped composite material.
The titanium carbonitride reinforced high-chromium cast iron based honeycomb-shaped composite material prepared by the invention (the volume wear rate is 72.5 mm) 3 H) and the wear resistance is higher than that of the traditional high-chromium cast iron (the volume wear rate is 290 mm) 3 Perh) is improved by 4 times, and is enhanced by the titanium carbonitride composite with the whole layerChromium cast iron-based composite material (volume wear rate 155.5 mm) 3 The/h) is increased by 2.1 times.
Claims (10)
1. The preparation method of the ceramic/iron-based honeycomb-structure composite material is characterized by comprising the following steps:
(1) Dissolving ferric nitrate nonahydrate in a citric acid solution, controlling the proportion of the ferric nitrate nonahydrate and the citric acid in the solution, and then putting the mixed solution into a water bath kettle for constant-temperature heating to obtain sol (1);
(2) Adding nano activated carbon into a hydrated titanium dioxide solution, stirring at a high speed, and then putting the mixed solution into a water bath kettle for constant-temperature heating to obtain sol (2);
(3) Uniformly mixing the sol (1) obtained in the step (1) and the sol (2) obtained in the step (2) in proportion, and performing vacuum drying treatment to obtain mixed gel;
(4) Placing the mixed gel obtained in the step (3) in nitrogen for high-temperature calcination, performing roasting treatment to obtain mixed powder of titanium carbonitride and iron oxide, and then placing the mixed powder into a reduction furnace for reduction by reducing gas to obtain mixed powder of titanium carbonitride and iron;
(5) And (4) uniformly stirring the mixed powder obtained in the step (4) and a binder, then filling the mixture into the honeycomb wall of a honeycomb structure die to be solidified to form a prefabricated body, and pouring a steel melt to obtain the titanium carbonitride ceramic reinforced iron-based honeycomb-configuration composite material.
2. The method for preparing the ceramic/iron-based honeycomb structure composite material according to claim 1, wherein the method comprises the following steps: the molar ratio of the ferric nitrate to the citric acid in the step (1) is 1 (0.6-1.2).
3. The method for preparing a ceramic/iron-based honeycomb-configuration composite material according to claim 1 or 2, wherein: the heating condition of the water bath kettle in the step (1) is as follows: heating at 60-90 deg.C for 8-12h.
4. The method for preparing a ceramic/iron-based honeycomb-structured composite material according to claim 1, wherein the method comprises the following steps: the molar ratio of the hydrated titanium dioxide to the nano activated carbon in the step (2) is 1 (0.8 to 1.2), and the granularity of the nano activated carbon is 10-30nm.
5. A method for preparing a ceramic/iron-based honeycomb configuration composite material according to claim 1 or 4, wherein: the heating condition of the water bath kettle in the step (2) is as follows: heating at 40-70 deg.C for 4-8h.
6. The method for preparing a ceramic/iron-based honeycomb-structured composite material according to claim 1, wherein the method comprises the following steps: the molar ratio of Fe ions in the sol (1) to Ti ions in the sol (2) in the step (3) is 1 (0.02 to 0.4).
7. The method for preparing a ceramic/iron-based honeycomb-structured composite material according to claim 1, wherein the method comprises the following steps: the drying conditions in the step (3) are as follows: drying in a vacuum drying oven at 100-150 deg.C for 14-20h.
8. The method for preparing a ceramic/iron-based honeycomb-structured composite material according to claim 1, wherein the method comprises the following steps: the calcining and roasting conditions in the step (4) are as follows: calcining at 1400-1600 deg.C for 2-4h in nitrogen atmosphere, and calcining at 800-1000 deg.C for 3-5h in air atmosphere.
9. The method for preparing a ceramic/iron-based honeycomb-structured composite material according to claim 1, wherein the method comprises the following steps: the reducing gas used in the reduction process in the step (4) is hydrogen, the temperature of the reducing furnace is 600-800 ℃, and the hydrogen flow is 1.0-2.0m 3 The time is 4-6h.
10. The method for preparing a ceramic/iron-based honeycomb-structured composite material according to claim 1, wherein the method comprises the following steps: the binder in the step (5) is any one of polyvinyl alcohol, ethylene-vinyl acetate copolymer and starch paste; the molar ratio of the binder to the titanium carbonitride and iron mixed powder is (0.02 to 0.04) to 1; the curing conditions were: curing for 6-10h in a heat preservation box at 90-130 ℃.
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